Synthesis, characterization and swelling behavior of a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co- itaconic acid) hydrogels for adsorption and controlled release of ciprofloxacin

Synthesis, characterization and swelling behavior of a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co- itaconic acid) hydrogels for adsorption and controlled release of ciprofloxacin | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Synthesis, characterization and swelling behavior of a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co- itaconic acid) hydrogels for adsorption and controlled release of ciprofloxacin Wissam L Penyan, layth S Jassim This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3698789/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract In the current study, a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co-itaconic acid) hydrogel is synthesized by free radical copolymerization using acrylic acid and itaconic acid as monomers grafted on natural pectin. N, N′-Methylenebisacrylamide is used as a crosslinking agent, and potassium persulfate as an initiator. Various techniques, such as FTIR, SEM, XRD, and TGA, were used to characterize the synthesized bio-adsorbent hydrogel. The effect of several variables on the swelling behavior of the synthesized hydrogel was examined, like cross linker amount, pectin amount, initiator amount, and monomers amount. Furthermore, the swelling process was investigated at various pH levels. In order to establish suitable adsorption conditions, several adsorption parameters were examined, such as pH, equilibrium time, adsorbent amount, and temperature. The adsorption data were examined using the Langmuir, Freundlich, and Temkin models. The results showed that the adsorption is typically heterogeneous and of the multilayer type, as they were more consistent with the Freundlich model. The adsorption process is exothermic and spontaneous, according to thermodynamic parameters measured. In vitro drug release experiment results showed that after 30 hours, the CIP drug was released significantly higher in the simulated intestinal fluid (pH = 7.4) than in the simulated stomach fluid (pH = 1.2). The drug release of CIP from the hydrogel was measured at different temperatures: 30°Cand 40°C. These findings demonstrate that the hydrogel is highly efficient in ciprofloxacin adsorption and pH sensitive, making it appropriate for drug delivery in the small intestine. Hydrogel Swelling behavior Ciprofloxacin drug Adsorption controlled release Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Introduction Hydrogels are three-dimensional cross-linked polymeric network that swelling in aqueous solution and physiological fluid as a result the presence of hydrophilic groups such as hydroxyl(–OH), carboxylic(–COOH), amide (–CONH 2 ), sulfonic acid (–SO 3 H), and amino groups (–NH 2 ), which provide enough area for attract foreign materials that are adsorbed on the surface of hydrogels(Sharma et al. 2022 , Kumar et al. 2023 ) .Additionally, hydrogel is capable of absorbing water without losing its structural integrity, making it easier to separate and recycle the hydrogel adsorbents from treated wastewater(Mohamed and Mahmoud 2020 ). Hydrogels superior to conventional adsorption materials in terms of antibiotic residue removal rate, ease of preparation, compatibility with the environment, and efficiency(Song et al. 2023). Hydrogels have been shown to be useful in agriculture(Kaur et al. 2023 ) and biomedical applications such as controlled drug and protein delivery (Li et al. 2021 ),wound dressing (Martínez-Ibarra et al. 2019 ), and tissue engineering(Roshanbinfar et al. 2019 ). In general, hydrogels may be developed using synthetic or natural polymers; however, the use of natural polymers like alginate, pectin, starch, and others appears to be more likely due to their economical and biological advantages such as natural abundance, cheap costs, biodegradability, biocompatibility, and lower toxicity(Mota and Fajardo 2021 ). In recent years, there has been an increase in interest in polysaccharide modification via graft copolymerization(Weerasundara et al. 2021). Grafting synthetic hydrogels on natural polysaccharides helps to overcome some of the disadvantages of virgin polysaccharides, such as contamination from microbes, uncontrolled hydration, and age-related viscosity changes. As a result, synthetic hydrogels with a long life, excellent adsorption capacity, enhanced mechanical properties, and a high swelling nature exist(Thakur et al. 2018 , Maji and Maiti 2021 ). Pectin is a type of linear polysaccharide composed primarily of D-galacturonic acid (GalA) units linked in chains by α-(1–4)glycosidic bond with a number of carboxyl and hydroxyl groups distributed along the backbone(Sriamornsak 2011 , Nasrollahzadeh et al. 2020 ) .Plants are the primary source of pectin, such as the cell walls of citrus fruits(Kodoth et al. 2018 ). Pectin is used in a variety of applications due to its biocompatibility, biodegradability, and non-toxicity, including colon drug delivery, cosmetics, food, and other biological applications (Khotimchenko 2020 , Kedir et al. 2022 ). Acrylic acid (AA) is a synthetic pH-responsive monomer whose swelling index is primarily affected by the pH of the surrounding environment. Because AA carries a carboxylic acid (functional group) that is strongly associated with water molecules, the state of equilibrium swelling is significantly affected by the ionic strength and the pH level of the swolled solution (Suhail et al. 2022 ).Itaconic acid (IA) is an anionic, hydrophilic, unsaturated dicarboxylic acid that is used in the synthesis of co polymeric hydrogels. It has high pH sensitivity and good biocompatibility, which increases the swelling of hydrogels. Moreover, it copolymerizes easily to produce polymeric chains with -COOH side groups that can form hydrogen bonding with corresponding groups, increasing the mechanical properties of hydrogels(Kim et al. 2021 ). Fluoroquinolones (FQs) are a group of strong synthetic antibiotics that are frequently used in human prescription drugs and veterinary medications(Zhang et al. 2012 ). Ciprofloxacin (CIP) is a fluoroquinolone category drugs that is widely used as an antibiotic to treat infections caused by gram-negative as well as gram-positive bacteria(Ebrahimi and Salavaty 2018 , Ganesan et al. 2019 ). It was mainly employed to treat urinary, digestive, and respiratory illnesses(Prusty et al. 2021 ).CIP has very limited bioavailability within aqueous gastric intestinal fluid because of its short half-life and reduce rate of dissolution(Tanwar et al. 2021 ).In order to overcome these challenges, it would be extremely helpful to develop a controlled drug delivery system. Drug delivery systems are necessary for drugs that have a narrow therapeutic window of blood concentrations or that must be eliminated quickly or kept below levels where potentially harmful side effects become prevalent(Gulen and Demircivi 2020b ).Drug delivery systems have the benefits of increasing the length of stay of a drug within a patient, minimizing frequency of dosing and toxicity, as well as enhancing patient compliance, and thus effectiveness with most dosage requirements(Ameli and Alizadeh 2022 ).Furthermore, drug delivery systems provide protection the loaded drug from enzymatic degradation and low gastric pH, allowing for controlled release in the proximal colon(Anirudhan and Mohan 2014 ). Experimental Chemicals Without additional purification, all chemicals were used. Ciprofloxacin (CIP) (purity > 98%,C 17 H 18 FN 3 O 3 , MW = 331.4g/mol, λ max = 276 nm) was purchased from Macklin Biochemical Co., Ltd., China. Pectin was provided by Merck (Darmstadt, Germany). Acrylic acid (AA, 99% purity,) was provided from CDH Chemical Co., India. Itaconic acid(IA, 99%) was obtained from Macklin Biochemical Co., Ltd., China. N,N'-methylene bis-a acrylamide (MBA,99%) and the initiator potassium persulfate (KPS,99%) were purchased from Shanghai Macklin Biochemical Co., Ltd., China. Sodium chloride, calcium chloride, sodium hydroxide and hydrochloric acid were supplied from Fluka, Switzerland. Deionized water was used to make all solutions. Synthesis of Pectin–g–poly(AA–co–IA) hydrogel Firstly, 1g of pectin was dissolved in 30ml deionized water with continuous stirring at 40°C till the solution was homogeneous. After heating to 60°C at N 2 atmosphere, 0.07 g of initiator KPS (pre-dissolved in 2 mL of deionized water) was added to the solution under stirring to produce radicals. Then, in a separate beaker, 0.7 g of IA was dissolved in 5 mL deionized water and gently heated before being added to the above polymeric solution, and 5mL of AA was added to the mixture while continuously stirring. Following that, 0.05 g of MBA dissolved in 5 mL deionized water was added to the aforementioned polymeric solution. The resultant solution was carefully placed in test tubes after being stirred for 30 minutes at room temperature. It was then maintained in a water bath at 70°C for 2 hours to complete the formation of hydrogel. After the specified polymerization time, hydrogel rods were carefully removed from test tubes and cut into discs of specific dimensions using a sharp-edged blade. To get rid of any unreacted materials, discs were washed in deionized water for 30 minutes. Up until a constant pH value was reached, this washing procedure was repeated with periodic replacement of the washing solution. Discs were completely dried in an oven set at 60°C. The steps in the synthesis of a hydrogel are shown in Fig. 1 . Characterization UV-vis absorption measurements were carried out at room temperature using a UV 1800 spectrophotometer (Shimadzu, Japan). XRD (XRD-6000, Shimadzu, Japan) and CuK (0.15040 nm) were used to investigate the crystalline or amorphous structure of the pure drug, hydrogel before and after drug adsorption. The XRD pattern was captured in the 10°-80° range.The functional groups in pure drug, hydrogel before and after drug adsorption were identified using Fourier transform infrared (FTIR) spectroscopy (Shimadzu, Japan, 8400s with wave number 400–4000 cm − 1 ). SEM (Scanning Electron Microscope) (MIRA3, Tescan, Czech Republic, Iran) with a voltage of 25 kV was used to examine the surface morphology of the hydrogel before and after drug adsorption. The thermal behavior of the prepared hydrogel was evaluated by thermogravimetric analysis (TGA), a TGA-4000 Perkin Elmer thermoanalyzer was used. Swelling studies The pre-weighted hydrogel was dissolved in 100 mL of deionized water and allowed to stand at room temperature until the swelling equilibrium was reached. Before weighing, the hydrogel that had swelled up was removed, and extra water on its surface was wiped away with filter paper. The hydrogel that had swelled was weighed using an analytical weighing balance. Using the equation shown below, Eq. ( 1 ), the maximum swelling percentage was determined. $$\text{S}\text{w}\text{e}\text{l}\text{l}\text{i}\text{n}\text{g} \left(\text{%}\right)=\frac{{\text{W}}_{\text{S}}-{\text{W}}_{\text{d} }}{{\text{W}}_{\text{d}}}\text{x}100$$ 1 Where, \({\text{W}}_{\text{d} }\) is the weight of dry hydrogel and \({\text{W}}_{\text{S}}\) is the weight of swollen hydrogel. Point zero charge (pzc) determination Using a pH drift method, the pH of hydrogel with zero charge was investigated. A 150 mL conical flask containing 50 mL of deionized water was used for the measurement of pzc. Different pH solutions (pHi) in the varied of 2 to 11 were prepared using solutions of 0.1M NaOH and 0.1M HCl. After that, 0.05 g of hydrogel was added to each flask, which was then shaken at 130 rpm for 24 hours to reach the equilibrium point. The pH of the liquid was measured after 24 hours and is represented by (pH f ).The value of pzc for prepared hydrogel was determined by graphing the relationship between initial pH (pHi) against ΔpH, where ΔpH represents the difference between pHi and pHf values. The pHi at which ΔpH becomes zero was taken into account as pzc of hydrogel(Verma et al. 2020 ). Batch adsorption studies A UV-visible spectroscope was used to examine batch CIP adsorption on hydrogel adsorbent. To establish the ideal adsorption conditions, various adsorption factors like contact time, pH, adsorbent dose, temperature, and ionic strength were studied. At room temperature, 0.05g of the dried hydrogel was immersed in 10 mL of CIP solution (100 mg/L) with stirring at 130 rpm. After reaching equilibrium (about 120 minutes of contact time), the drug solutions were removed and centrifuged for 5 minutes (at 5000 rpm). A UV-vis spectrophotometer with a maximum wavelength of 276 nm was used to determine the remaining concentration of the drug solution. The CIP drug was quantified using an external calibration curve (y = 0.089x + 0.01354) with an R 2 value of 0.9982. According to Eq. ( 2 ), the changes in drug concentration before and after adsorption were used to calculate the equilibrium adsorption capacity, \({\text{q}}_{\text{e}}(\text{m}\text{g}/\text{g})\) (Majid et al. 2019 ). $${q}_{e }=\frac{{C}_{o}-{C}_{e }*V}{m}$$ 2 The drug removal efficiency (% Removal) is calculated using Eq. ( 3 ). $$\text{R}\text{e}\text{m}\text{o}\text{v}\text{a}\text{l}\left(\text{%}\right)=\frac{{\text{C}}_{\text{o}}-{\text{C}}_{\text{e} }}{{\text{C}}_{\text{o}}} \text{x}100$$ 3 Where, \({\text{C}}_{0}\) and \({\text{C}}_{\text{e}}\) indicates the initial and equilibrium drug concentrations in (mg/L), respectively, m is the adsorbent dose in (g), and V is the volume of drug solution in (L). In vitro drug release study After optimizing the variables controlling the CIP drug loading as previously described, to investigate the CIP drug release. The drug in vitro release study from the hydrogel was performed in a shaking incubator at 37°C and 50 rpm. The CIP drug-loaded hydrogel (0.1 g) was submerged in a predetermined volume of gastric and intestinal liquids with pH values of 1.2 and 7.4, respectively. 2 mL of the medium was removed for absorbance tests at the proper intervals. To maintain the bath volume constant, fresh 2 mL buffer solution was added every time. Employing a calibration curve of the CIP drug at various concentrations, the UV–vis spectrophotometer was used to determine the concentration of CIP drug releasing at 276 nm. Using Eq. ( 4 ), the release percentage was determined(Hanna and Saad 2019 ). $$\left(\text{%}\right)\text{o}\text{f} \text{d}\text{r}\text{u}\text{g} \text{r}\text{e}\text{l}\text{e}\text{a}\text{s}\text{e}=\frac{\text{A}\text{m}\text{o}\text{u}\text{n}\text{t} \text{o}\text{f} \text{C}\text{I}\text{P} \text{d}\text{r}\text{u}\text{g} \text{r}\text{e}\text{l}\text{e}\text{a}\text{s}\text{e}\text{d}}{\text{A}\text{m}\text{o}\text{u}\text{n}\text{t} \text{o}\text{f} \text{C}\text{I}\text{P} \text{d}\text{r}\text{u}\text{g} \text{a}\text{d}\text{s}\text{o}\text{r}\text{b}\text{e}\text{d} \text{w}\text{i}\text{t}\text{h}\text{i}\text{n} \text{t}\text{h}\text{e} \text{h}\text{y}\text{d}\text{r}\text{o}\text{g}\text{e}\text{l} } \text{x}100$$ 4 Results and Discussion Hydrogel Formation Mechanism In this study, Fig. 2 illustrates a potential mechanism for the grafting of acrylic acid and itaconic acid monomers onto the Pectin backbone via the free radical polymerization method. In the first step, the initiator KPS was broken down into sulfate anion-radicals while being heated at 70°C. These radicals then produced alkoxy radicals by removing hydrogen atoms from the hydroxyl groups of the Pectin chains. Following the addition of the monomer molecules (acrylic and itaconic acids), the active radical sites on the Pectin chains would start the vinyl groups of the monomers to create chains propagation. During chain propagation, MBA with double vinyl groups operated as cross-link points via covalent bonding at both ends of the linear polymer chains, resulting in the formation of a Pectin-g-poly(AA-co-IA) hydrogel network(Mohammadzadeh Pakdel et al. 2022 ). FTIR Analysis The changes in structure throughout grafting copolymerization and drug adsorption were investigated using an FTIR spectrum comparison, as shown in Fig. 5 . According to the literature, Pectin exhibits a peak of -OH groups at 3402 cm − 1 , C-H group at 2928 cm − 1 , and -C = O group at 1749 cm − 1 resulting from the presence of COOCH 3 group, -CH 2 scissoring and -OH bending vibrations at 1441 cm − 1 and 1342 cm − 1 respectively, and -CH-OH group vibrations at 1150 cm − 1 (Kowalski et al. 2019 ). Acrylic acid is reported to have peaks of -OH groups at 3380 cm − 1 , -CH 2 groups at 2973 cm − 1 , -C = O groups at 1707 cm − 1 , -C-C groups at 1709 cm − 1 , -C = C groups at 1626 cm − 1 , and -C-O-C groups at 1173 cm − 1 (Feng et al. 2018 ). Itaconic acid is reported to shows broad peaks at 3085 cm − 1 that correlate with -OH stretching, 2750 cm − 1 associated to -CH 2 asymmetric stretching mode, and 1427 cm − 1 related to C-C bending vibration. The C = O stretching vibration was assigned a peak at 1695 cm − 1 , 1620 cm − 1 may be attributed to C = C stretching vibrations, and the C-O-C stretching vibration was ascribed a peak at 1203 cm − 1 (Olvera-Sosa et al. 2020 ).Crosslinking agent (MBA) is reported to shows peak at 3302 cm − 1 is correlated with N–H stretching vibrations. The peak at 1655 cm − 1 is associated with C = O group, while the peak at 1538 cm − 1 indicates existence of C = C groups on MBA(Ayu Laksanawati and Novarita Trisanti 2019). On observing FTIR spectra of prepared hydrogels as shown in Fig. 3 a, It is notable that significant differences can be observed between the prepared hydrogel and the monomers due to crosslinking of the chains of polymeric to develop Pectin–g–poly(AA–co–IA) network. The overlapping of the O-H stretching vibrations and N-H stretching vibrations (amide group) of the crosslinking agent( MBA) was observed by a broad peak in the range of 3000–3564 cm − 1 (Hu et al. 2015 ). The absorption band of C = O groups in Pectin (1749 cm − 1 ), acrylic acid (1707 cm − 1 ), itaconic acid (1695 cm − 1 ) and MBA(1615 cm − 1 ) are shifted towards wave number (1712 cm − 1 ) because of carbonyl groups depletion in the synthesis of cross-linked network structure(Ajaz et al. 2020 ). The peak at 1164 cm − 1 could be attributed to stretching vibration of C–N in MBA(Dai et al. 2019 ). The absorption band of a C = C stretching vibration that typically appears at 1626 cm − 1 in acrylic acid and1620 cm − 1 in itaconic acid was not observed in prepared hydrogel, which suggests that polymerization reaction has occurred to the monomers (Sun et al. 2013 ).All these changes in peaks indicate that acrylic acid and itaconic acid grafting on backbone of pectin to form Pectin–g–poly(AA–co–IA) hydrogel. The FTIR spectrum of pure ciprofloxacin displays numerous absorption bands, as shown in Fig. 3 b. The O-H stretching in COOH at 3379 cm − 1 has the most distinctive bands. The band at 3525 cm − 1 could be ascribed to N-H group stretching vibrations. Another band at 2923cm − 1 represented alkenes and aromatic C–H stretching vibrations. The peaks at 1704 cm − 1 and 1620 cm − 1 due to the C = O stretching in COOH and 4-quinolone, respectively. The C = C stretching in aromatic ring at 1465 cm − 1 and the C–O stretching in COOH at 1265 cm − 1 . In addition, a band at 933 cm − 1 was assigned to C-F group(Kowalczuk 2020 ). FTIR spectrum of drug loaded with hydrogel demonstrates in Fig. 3 c, it can be seen that the intensity and position of peaks assigned to characteristic functional groups were either disappeared or slightly shifted after drug adsorption, indicating that H–bonding and electrostatic interactions are present between the hydrogel and the drug. SEM Analysis SEM was employed to study the surface appearance of hydrogel because it provides a magnified view of the material for easy visualization and analysis. Figure 4 shows SEM micrographs of hydrogel prior to adsorption and hydrogel adsorbed with CIP. The SEM analysis of the hydrogel prior to CIP adsorption, as shown in Fig. 4 a, revealed a smooth surface with some cracks distributed throughout the Pectin-g-poly(AA-co-IA) surface. Following CIP adsorption, the hydrogel surface changed significantly, becoming coarse and containing a bulky intense layer, as shown in Fig. 4 b. These changes could be attributed to CIP drug adsorption on the hydrogel surface. TGA Analysis TGA is widely regarded as an extremely important technique for determining the thermal stability of polymeric materials. It measures the amount of weight loss in a sample as a function of temperature. Figure 5 depicts the TGA curve of the prepared hydrogel at temperatures ranging from 40 to 800°C, with weight loss occurring in three stages during the thermal decomposition process. The first stage occurred at 30 to 140°C and is due to the loss of water content from the hydrogel, resulting in approximately 9.48% weight loss. The second stage began at temperatures ranging from 140 to 280°C, and during this stage, the hydrogel lost 26.83% of its total weight. The third stage had a weight loss of 99.482% and was situated between 350 and 800°C. The second and third stages were connected to a number of intricate processes, such as the dehydration of saccharide rings, the breaking down of C-O-C bonds in the Pectin chain, the breakdown of branches and side chain groups in the graft copolymer, the splitting of the PAA/IA chains, and the dissolution of the cross-linked network structure(Ilgin et al. 2020 ). XRD Analysis The crystalline, semi-crystalline, and amorphous nature of the materials can be quickly determined using the fundamental analytical technique known as XRD. Figure 6 a, depicts the XRD pattern of the pure CIP drug. It is obvious that the pure drug displayed numerous sharp peaks at positions 2θ = 10˚ to 45˚, indicating the drug crystalline nature(Khan et al. 2020 ). Figure 6 b, shows the prepared hydrogel XRD pattern. It is evident that the hydrogel is amorphous because there are no distinct diffraction peaks other than a broad band between 2θ = 15° and 45°. The characteristic peaks of the crystalline CIP drug were not observed in the X-ray diffractograms, as shown in the XRD pattern of CIP adsorption onto hydrogel in Fig. 6 c, suggesting loss of crystallinity of CIP in addition to successful adsorption of CIP into a developed superabsorbent hydrogel. Optimization of Pectin–g–poly(AA–co–IA)hydrogel swelling Effect of Cross Linker Content The presence of cross-linkers is an important factor in determining the swelling capacity of a superabsorbent hydrogel because cross-linkers make the hydrogel insoluble in aqueous environments(Hasija et al. 2018 ). To investigate the effect of cross-linker content on swelling percentage, swelling was examined at five different cross-linking amounts varying from 0.001 to 0.1g. As illustrated in Fig. 7a. The swelling percentage increased as the cross-linking agent content increased from 0.001 to 0.05 g, with the maximum swelling attained when the amount of crosslinking agent was 0.05g. When the cross-linker amount raised and exceeded 0.05 g, more cross-linking points were created through polymerization, resulting in a grater cross-linking density and less hydrodynamic free volume available to accommodate water molecules, which reduced swelling(Sharika and Mohanan 2021 ). Effect of Pectin Content Using deionized water at constant other influencing conditions, Fig .7b illustrates the impact of varying the pectin content (0.3–2g) on the level of swelling of the developed hydrogel. The results showed that increasing the amount of pectin in the hydrogel matrix from 0.3 to 1g significantly enhanced the swelling degree from 1600 to 2350%. This is because pectin naturally contains a variety of OH and COOH groups that contribute to the hydrophilic properties of the hydrogel network. As a result, the hydrogel network swells more due to the greater attraction of water molecules for diffusion into the gel matrix. whereas, the swelling ratio decreased to 1207% with additional Pectin content up to 2g because of increasing the density of the hydrogel network, and thus, the rate of water molecule diffusion reduces, resulting in a decrease in the swelling level value. Additionally, with increased Pectin content, the viscosity of the reaction medium will obviously increase, which inhibited the free movement and uniform distribution of other reactants in the reaction system(Wang et al. 2017, Omer et al. 2023 ). Effect of Acrylic Acid Content To examine the impact of acrylic acid monomer on hydrogel swelling ratio, monomer volume was varied between (1.0–10 mL), and the results are displayed in Fig. 7c. The swelling percentage increased significantly as the AA monomer content increased from 1 to 5 mL, and the swelling percentage increased from 1100 to 2530%, respectively. This could be attributed to the increased amount of AA providing more hydrophilic groups such as –COO– and -COOH grafted onto the Pectin, which could enhance the hydrogel swelling ability. Nonetheless, after 5 mL, the swelling level of hydrogel with increased AA content declines significantly and reaches 1400% at 10 mL. This is most likely explained by an increase in reaction medium viscosity and restricted free radical movement, in addition to preferred photopolymerization over graft copolymerization and a reduction in osmotic pressure difference, leading to hydrogel network shrinkage(Tanan et al. 2019 ). Effect of Itaconic Acid Content The relationship between IA content and hydrogel swelling percentage was investigated over a range of 0.3 to 1.5 g, with the highest swelling percentage found at a content of 0.7 g as shown in Fig. 7d. Due to a higher hydrogel swelling percentage, raising the IA content from 0.3 g to 0.7 g leads to more IA molecules available for the chain propagation sites on the graft copolymer network. IA content greater than 0.7 g accelerated the photopolymerization reaction and reduced the hydrogel swelling percentage(Thakur et al. 2022 ). Effect of Initiator Content The effect of the initiator content on the hydrogel swelling percentage is shown in Fig. 7e. KPS initiator had a range of 0.01 to 0.1g of content. When the KPS content was increased from 0.01 to 0.07g, it was observed that the swelling percentage improved from 1350 to 2488%. This is because there were sufficient active free radicals on the pectin backbone and monomers, which is what caused the swelling(He et al. 2017 ). However, increasing the initiator content above 0.07g caused the swelling percentage to decrease. This, in turn, led to an increase in the terminating step reaction through bimolecular collision, which in turn increased crosslinking density. Another factor contributing to swelling-loss at higher KPS concentrations is the oxidative damage from free radicals(Bagheri Marandi et al. 2011 ). Effect of pH The influence of pH on the swelling behaviors of hydrogel was studied using different pH solutions that varied from 2 to 10, as displayed in Fig. 7f,g. It can be observed that the swelling of the hydrogel increases linearly as the pH of the solution increases. The maximum swelling capacity of hydrogel is at pH = 7.4. When the pH rises above 7.4, the water absorbency gradually decreases. Most carboxylate anions –COO – are protonated and converted to COOH groups under strongly acidic environments (pH ≤ 4). The electrostatic repulsion between carboxylate anions –COO – groups was reduced, and as a result, swelling ratio were reduced(Sharma et al. 2014 ). Additionally, protonation results in the strengthening of H-bonds among COOH, which raises the level of physical crosslinking in the skeleton network and reduces the hydrogel tendency to swell. With pH levels rising, some COOH groups are converted to –COO – , weakening the H-bonding interactions and the adverse impact of H + on electrostatic repulsion between carboxylate groups –COO – . As a result of the strong anion-anion repulsion, the degree of physical crosslinking is reduced. As a result, the swelling percentage increases noticeably and reaches its maximum (2602%) at pH = 7.4. On the other hand, at pH > 7.4, the swelling of hydrogel is significantly reduced as the pH rises. This behavior could be explained by the "charge shielding effect" of excessive Na + in the swelling media, which protects the carboxylate anions –COO – and inhibits effective anion-anion repulsion, resulting in a lower swelling percentage(Li et al. 2015 ). Point zero charge of synthesis hydrogel The electrostatic attraction between the functional groups of the drug molecule and the hydrogel surface functionality determines how well the CIP drug will bind to the surface. The initial pH of the water has an impact on the surface charge of the hydrogel. The hydrogel functional groups experience deprotonation as pHi rises. In more specific terms, the hydrogel surface is going to be positively charged if pHi pHpzc. In our study, the pHpzc for hydrogel is 4.2, as shown in Fig. 8 , indicating that for pH values below 4.2, the active regions on hydrogel have a positive charge. At pH level exceeds 4.2, the hydrogel surface becomes negatively charged Effects of the adsorption parameters Effect of Solution pH pH represents one of the most key factors in drug adsorption because it influences drug speciation, adsorbent capacity, and surface charge, all of which influence drug interactions. To better understand the impact of pH, batch experiments were conducted under controlled conditions with pH ranging from 2 to 11, while maintaining the other process parameters constant at their ideal levels (initial concentration = 100 mg/L, adsorbent dosage 0.05g, contact time = 120 min, and temperature = 15 ◦ C). Since CIP is an antibiotic, the protonation of the amine group causes it to exist in a cationic form (CIP+) at pH 5.9. The ionization of the carboxylic acid causes the CIP to exist in an anionic form (CIP−) when the pH is higher than 8.9. Additionally, the CIP can exist in the pH range of 5.9 to 8.9 in a zwitterionic form (CIP ±)(Gulen and Demircivi 2020 a, Igwegbe et al. 2021 ). As shown in Fig. 9 a, the CIP adsorption capacity gradually increased from 2 to 6, then gradually declined from 6 to 11, with a particularly rapid decline at pH 7. This is clarified by the electrostatic attraction that occurs between the hydrogel surface charge and the charge of the CIP. The hydrogel surface becomes negatively charged at pH 6 (greater than point zero charge), and CIP molecules are positively charged, resulting in strong electrostatic attraction between the cationic (CIP+) and the negatively charged of the hydrogel surface. The rapid decrease after pH 7 could be attributed to electrostatic repulsion between the anionic (CIP) and negatively charged hydrogel surface(Tran et al. 2022). At pH > 7 (with anionic CIP as the dominant species), a significant reduction in CIP removal was observed, which is attributed to electrostatic repulsion between the anionic drug (CIP−) and the negatively charged adsorbent. Additionally, as can be seen in Fig. 9 a, adsorption was reduced when the solution pH was below 4 because the hydrogel surface has a positive charge at pH < 4.2 (pH < pHpzc), which causes electrostatic repulsion between the cationic species (CIP+) and the positively charged hydrogel surface(Yadav et al. 2021 ). Consequently, in this study, a pH of 6 was purposefully chosen as the optimum adsorption condition for the CIP drug . Effect of Adsorbent Dosage Adsorbent dosage is a significant factor that influences the effectiveness of adsorption. In general, it is preferable for economic adsorption to use a small amount of adsorbent that can achieve a high adsorption percentage. The effectiveness of CIP removal was examined using experimental conditions, and the effects are depicted in Fig. 9 b, for a hydrogel adsorbent dosage range of 0.005 g to 0.1 g, while the other process variables remained constant and at their ideal levels (initial concentration = 100 mg/L, pH = 6, contact time = 120 min, and temperature = 15 ◦ C). It was discovered that increasing the adsorbent dosage from 0.005 to 0.1g caused the removal efficiency of CIP to rise from 86.55–94.75%.The increased adsorbent dosage resulted in a greater number of functional groups and more available sites for adsorption, which contributed to the improvement in removal efficiency. Nevertheless, when the adsorption process attained saturation, the impact of introduced more adsorbent was not significant. Consequently, it is important to optimize the adsorbent dosage with respect to both efficiency and cost-effectiveness(Lu et al. 2020 ). The adsorbent dosage of 0.05 g was selected for further experiments in this study. The Effect of Contact Time The influence of contact time on CIP removal efficiency was examined over a time ranging from 1-250 min at an initial concentration of 100 mg/L while maintaining a constant pH, adsorbent dosage, and temperature of 6, 0.05g, and 15 ◦ C, respectively. As displayed in Fig. 9 c, the removal efficiency raised rapidly as time increased at first, then attained a constant value. Due to the adsorption sites on the adsorbent surface are vacant at first, the adsorption is rapid(Avcı et al. 2020 ). Furthermore, the hydrogel three-dimensional polymeric network and porous structure likely reduce mass transfer resistance and enhance CIP diffusion into the interior of the adsorbents. Then it gradually slows until it reaches a constant value of 120min. At the start of the adsorption process, the active sites rapidly adsorb a large number of CIP till the outer surface is completely saturated. CIP enters the adsorbent pores after the outer surface is saturated and is adsorbed into the interior surface of the hydrogel(Mohammadinezhad et al. 2018 ). As a result, adsorption equilibrium might be reached in 120 minutes. Effect of Temperature Temperature can have a significant impact on the affinity of the adsorbent to the CIP molecules. As a result, the effect of solution temperature on the level of CIP removal was investigated at temperatures ranging from 15°C to 35°C, while concentration, pH, adsorbent dosage, and contact time were kept constant at 100 mg/L, 6, 0.05g, and 150 min, respectively. The results of the temperature impacts are shown in Fig. 9 d, where decreasing the temperature is clearly preferable for CIP removal onto hydrogel (94.07%), whereas CIP removal reduces as solution temperature increases up to 35°C. This indicates the exothermic nature of the adsorption process. In most exothermic adsorption processes, increasing the temperature causes desorption of the target contaminants to the liquid phase at equilibrium(Cheng et al. 2019 ). In another way, as temperature increases, the diffusive transfer of mass and solubility of CIP in water increase, weakening the adsorptive forces between adsorbent sites. As consequently, physical adsorption would be reduced and removal efficiency would be reduced (Saber et al. 2021 ). Therefore, 15°C was selected for the subsequent experiments. Adsorption Isotherm Studies Adsorption Isotherm studies were carried out to investigate a single layer or multiple-layer adsorption. For the isotherm experiments, 10 mL of CIP solution was placed in a 50 mL conical flask with 0.05 g of adsorbent at various concentrations (10–300 mg/L). These solutions were then shaken for 120 minutes in a thermostat shaker set to 15°C (130 rpm). The remaining CIP concentration was determined using a UV-vis spectrophotometer. Various isotherm models, including Langmuir, Freundlich, and Temkin, were used to analyze the data Langmuir model Assumes that adsorption takes place homogeneous adsorption where the sorption process is monolayer adsorption and each adsorbate molecule onto the surface has equal sorption activation energy(Balarak and McKay 2021 ). The following Eq. ( 4 ) illustrates the Langmuir isotherm equation. $$\frac{{\mathbf{C}}_{\mathbf{e}}}{{\mathbf{q}}_{\mathbf{e}}}=\frac{1}{{\mathbf{q}}_{\mathbf{m} }.{\mathbf{K}}_{\mathbf{L}}}+\left(\frac{1}{{\mathbf{q}}_{\mathbf{m}}}\right).{\mathbf{C}}_{\mathbf{e}}$$ 4 The equilibrium adsorbate solution concentration is \({\text{C}}_{\text{e}}\) (mg/L), the equilibrium adsorption capacity is \({\text{q}}_{\text{e}}(\text{m}\text{g}/\text{g})\) , the maximum adsorption capacity is \({\text{q}}_{\text{m} }(\text{m}\text{g}/\text{g})\) , and the equilibrium Langmuir's constant is \({\text{K}}_{\text{L}}(\text{L}/\text{m}\text{g})\) . By analyzing the slope and intercept of the plot of \({\text{C}}_{\text{e}}\) / \({\text{q}}_{\text{e}}\) against \({\text{C}}_{\text{e}}\) , the values of \({\text{q}}_{\text{m} }\) and \({\text{K}}_{\text{L}}\) were calculated. Freundlich Isotherm In the case of multilayer adsorption systems, the Freundlich isotherm is applied to a heterogeneous surface. Every site has undergone the adsorption process(Ayouch et al. 2021 ). The Freundlich isotherm equation is shown in the following Eq. ( 5 ). $$\text{l}\text{o}\text{g}{\text{q}}_{\text{e}}=\text{l}\text{o}\text{g}{\text{K}}_{\text{f}}+\frac{ 1 }{\text{n}}\text{l}\text{o}\text{g}{\text{C}}_{\text{e}}$$ 5 where, the adsorption intensity is indicated by the exponent \(1/\text{n}\) and \({\text{K}}_{\text{f}}\) is the constant associated with the adsorption capacity. The favorability and capacity of the adsorption system are indicated by the value of 1/n. Eq. ( 5 ) states that the Freundlich constant \({\text{K}}_{\text{f}}\) is the intercept and that the slope of a plot of \(\text{l}\text{o}\text{g}{q}_{e}\) versus \(\text{l}\text{o}\text{g} {\text{C}}_{\text{e}}\) is equal to \(1/\text{n}\) . Temkin Isotherm is predicated on the idea that adsorption heat decreases inversely with the amount of adsorbent surface covered, and that an even distribution of binding energies exists up to the maximum binding energy(Peng et al. 2016 ). In Eq. ( 6 ), the Temkin isotherm is displayed. $${\text{q}}_{\text{e}}=\text{B}\text{l}\text{n}{\text{K}}_{\text{T}}+\text{B}\text{l}\text{n}{\text{C}}_{\text{e}}$$ 6 Where KT (L /mg), R(8.314 J/mol.K), and T(K) are the Temkin parameters associated with the absolute temperature, the gas constant, and the equilibrium binding constant, respectively. \(\text{b}\) is heat of adsorption, \(\text{B}=\text{R}\text{T}/\text{b}\) . By plotting of \({\text{q}}_{\text{e}}\) against \(\left(\text{l}\text{n}{\text{C}}_{\text{e}}\right)\) ,Slope is \(\text{B}\) and intercept is \(\text{B}\text{l}\text{n}{\text{K}}_{\text{T}}\) . Table 1 The correlation coefficients and constants of Langmuir, Freundlich and Temkin models for the adsorption of CIP Langmuir Freundlich Timken R 2 0.7299 R 2 0.9986 R 2 0.7866 q max 192.307 n 1.115 B 13.626 K L 0.020 K F 4.031 K T 1.414 The Freundlich isotherm model was used to fit the adsorption isotherm data. Table 1 summarizes the obtained parameters. As shown in Fig. 10 b, the Freundlich model established the adsorption of CIP drug from aqueous solutions using Pectin-g-poly (AA-co-IA). Under the Freundlich model, the value of (n) in (Table 1 ) demonstrates the strength of adsorption and classifies the type of adsorption as favorable (1 n), or irreversible (n = 1). The heterogeneity condition was confirmed in the current context since the value of (n) was greater than one (n > 1). In addition, the Freundlich model R 2 correlation value is significantly greater than those of the Langmuir and Temkin models. Hence, the Freundlich isotherm more closely matches the adsorption data, suggesting that the bulk solution of drug molecules are adsorbed onto a heterogeneity multiple-layer(Chen et al. 2019 , Wu et al. 2019 ). Adsorption Thermodynamics Studies To investigate the spontaneity of the adsorption process, thermodynamic parameters were established. The change in enthalpy ( \(\varDelta {\text{H}}^{0}\) ), free energy ( \(\varDelta {\text{G}}^{0}\) ) and entropy ( \(\varDelta {\text{S}}^{0}\) ) were investigated to determine the thermodynamic characteristics of CIP adsorption onto the Pectin-g-poly(AA-co-IA)sorbent. The parameters related to thermodynamics were calculated using the following equations: $${\text{K}}_{\text{d}}=\frac{{\text{C}}_{0}-{\text{C}}_{\text{e}}}{{\text{C}}_{\text{e}}}$$ 7 $$\varDelta {\text{G}}^{0}=-\text{R}\text{T}\text{l}\text{n}{\text{K}}_{\text{d}}$$ 8 $$\varDelta {\text{G}}^{0}=\varDelta {\text{H}}^{0}-\text{T}\varDelta {\text{S}}^{0}$$ 9 $$\text{l}\text{n}{\text{K}}_{\text{d}}=\frac{\varDelta {\text{S}}^{0}}{\text{R}}- \frac{\varDelta {\text{H}}^{0}}{\text{R}\text{T}}$$ 10 Where \({\text{C}}_{0}\) and \({\text{C}}_{\text{e}}\) are the initial and equilibrium concentrations of CIP in (mg/L), R is the gas constant ( \(8.314 \text{J}/\text{m}\text{o}\text{l}.\text{K}\) ) and T is the temperature (K). \({\text{K}}_{\text{d} }\) is the equilibrium constant. Figure 11 displays Van't Hoff plots of \({\text{l}\text{n}\text{K}}_{\text{d}}\) against 1/T. The slope ( \(-\varDelta {\text{H}}^{0}/\text{R}\) ) and intercept ( \(\varDelta {\text{S}}^{0}/\text{R}\) ) were used to calculate the \(\varDelta {\text{H}}^{0}\) and \(\varDelta {\text{S}}^{0}\) , respectively. Table 2 contains the obtained thermodynamic parameters. With an increase in temperature, the free energy change \(\varDelta {\text{G}}^{0}\) becomes less negative, which is consistent with a decrease in removal efficiency, and CIP adsorption was a spontaneous process. While the negative \(\varDelta {\text{S}}^{0}\) value for adsorption indicated decreased randomness at the solid/liquid interface in the adsorption process, the negative \(\varDelta {\text{H}}^{0}\) value for adsorption proved that the CIP adsorption process was exothermic(Chafyq et al. 2021, Seera et al. 2021). Table 2 The obtained thermodynamics parameters of CIP adsorption on hydrogel at different temperatures T(K) ∆H o (kJ/mol) ∆S o (J/mol.K) ∆G o (kJ/mol) 288 –18.194 – 40.075 – 6.610 298 – 6.310 303 – 6.116 308 – 5.768 In vitro release of CIP drug The drug release profiles from hydrogels (Fig. 12 ) show that the CIP drug release at pH 7.4 has been demonstrated to be greater than that observed at pH 1.2, which is consistent with their swelling data. The CIP drug cumulative release ratio is 36% after 2 hours, 50% after 5 hours, 71% after 12 hours, and reaches a high of 85.15% after 30 hours at simulated intestinal fluid (pH = 7.4).CIP is not highly soluble in neutral pH ranges. As a result, the drug release results show that the swelling amount of the drug-loaded hydrogel in media has a greater influence on drug release than CIP solubility. At pH = 7.4, the high swelling ratio of hydrogel results in the formation of larger pore sizes within the hydrogel network, which promotes drug diffusion from larger pore sizes in hydrogel. Furthermore, at pH = 7.4, CIP includes both anionic carboxylate and cationic amine groups, while the hydrogel just has anionic carboxylate. In truth, anionic groups on hydrogel and protonated amine on CIP drug lead to electrostatic attraction among drug and carrier, resulting in sustained CIP drug release(Sabzi et al. 2020 , Alinavaz et al. 2021 ). The results obtained demonstrated that this protecting system proved an excellent method for passing CIP into the intestine and increasing the therapeutic effectiveness of the medicine, which is sensitive to pH level in the stomach. Effect of temperature on CIP release The release of CIP drug from hydrogel was investigated at two different temperatures (37 and 39°C) at pH = 7.4. As shown in Fig. 13 , there is significant variation in CIP release rate at 37°C and 39°C. The lowest amount of drug release (71%) was recorded at 27°C, and the highest amount of drug release (99%) was noticed at 37°C. Because the ratio of swelling rises with temperature due to the adaptable nature of the hydrogel network, water rapidly penetrates the network and swells. Hence, increased the rate of drug release. Additionally, as the temperature rose, the drug molecules in the hydrogel moved faster, accelerating the rate of release(Hajikarimi and Sadeghi 2020 , Thippeswamy et al. 2021 ). Conclusion The grafting copolymerization method was employed to develop a novel bio-adsorbent of pectin grafted poly (acrylic acid -co- itaconic acid) hydrogel for CIP drug adsorption and controlled release. In deionized water, the bio-adsorbent hydrogel shown best swelling levels at reaction conditions (MBA = 0.05 g, pectin = 1g, AA = 5mL, IA = 0.7 g, KPS = 0.07 g) and demonstrated the highest swelling capacity of 2602% at pH = 7.4. At optimized conditions (pH = 6, contact time = 120 min, temperature = 15 o C, adsorbent dosage = 0.05g), the maximum % adsorption of CIP drug onto hydrogel (94.05%) was recorded. CIP adsorption fit better with the Freundlich isotherm (R 2 = 0.9986), indicating that the adsorption process of CIP drug was multilayer. According to the thermodynamic parameters, adsorption is a spontaneous and exothermic process. The low enthalpy value associated with the adsorption suggests that the interaction among the drug and the hydrogel is physisorption in nature. According to the results of the in vitro release experiment, the cumulative release of the CIP drug after 30 hours was higher in simulated intestinal fluid (85.15%) than in simulated stomach fluid (41. 31%). Also, the influence of temperature upon drug release revealed that drug release raised with temperature. Consequently, drug loading into a hydrogel might be able to prevent the negative effects of drug on the stomach. The oral route of CIP drug loading on hydrogel can effectively extend the action time of CIP drug as well as improve its bioavailability. As a result, this hydrogel can be used in future studies as a sustained-release drugs carrier. Declarations Acknowledgements Authors would like to thanks University of Al-Qadisiyah, Iraq for providing necessary support and facilities for completion of project . Author contributions All authors contributed to the design and conduct of the study. Materials preparation , experiments, data collection, analysis and written were performed by Wissam L Penyan and Laith S.Jassim. all authors commented on previous versions of the manuscript. Finally, all authors read and approved the final manuscript. 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Sci Total Environ 650:671-678 Yadav S, Asthana A, Singh AK, Chakraborty R, Sree Vidya S, Singh A, Carabineiro SA (2021) Methionine-functionalized graphene oxide/sodium alginate bio-polymer nanocomposite hydrogel beads: synthesis, isotherm and kinetic studies for an adsorptive removal of fluoroquinolone antibiotics. Nanomaterials 11(3):568 Zhang X, Gao X, Huo P, Yan Y (2012) Selective adsorption of micro ciprofloxacin by molecularly imprinted functionalized polymers appended onto ZnS. Environ Technol 33(17):2019-2025 Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-3698789","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":264682022,"identity":"06b174bf-7df7-4672-928f-6c298844500d","order_by":0,"name":"Wissam L Penyan","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA9UlEQVRIiWNgGAWjYDACZmTOByBmYydFC+MMkBZmXEqxaufBsBcLMDjO/vjDz5w7cuYSyc8e2/zaJs/HzMD44WMOHi2Hecwke7c9M7ackWZunNt327CNmYFZcuY23FrMDvOwMfBuO5y44UaCmXRuz21GoBY2Zl68Wtgff/y77XD9hhvp36Qte27bE6GFwUAaaEuCwY0cM2mGH7cTCWqxB/pFWnbbM8MNZ96USfY23E5uY2ZsxusXyf7jjz++3XZH3uB4+jaJH39u285vbz744SMeLVBwgIFBIAEYl20gDmMDQfUQLfxAzPCHGMWjYBSMglEw0gAAQQtTumEYiWoAAAAASUVORK5CYII=","orcid":"https://orcid.org/0009-0004-1485-539X","institution":"University of Al-Qadisiyah","correspondingAuthor":true,"prefix":"","firstName":"Wissam","middleName":"L","lastName":"Penyan","suffix":""},{"id":264682023,"identity":"744b69bd-8be1-45f0-8e37-47670f115458","order_by":1,"name":"layth S Jassim","email":"","orcid":"","institution":"University of Al-Qadisiyah","correspondingAuthor":false,"prefix":"","firstName":"layth","middleName":"S","lastName":"Jassim","suffix":""}],"badges":[],"createdAt":"2023-12-02 21:04:07","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3698789/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3698789/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":49111876,"identity":"ae1f832f-5b8d-4b77-af8d-120b06b8ef6f","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":144172,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic diagram showing the synthesis of the Pectin–g–poly(AA–co–IA) hydrogel\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/aae7197d791f885909f7ace7.png"},{"id":49111884,"identity":"82fd10d7-1474-4f12-aa8b-f5d00d0c29e2","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":34488,"visible":true,"origin":"","legend":"\u003cp\u003eProposed reaction mechanism for synthesizing Pectin–g–poly(AA–co–IA) hydrogel\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/e251ca6990e24750d22bacdc.png"},{"id":49111874,"identity":"36369c1c-2d68-4322-973a-f0cd8d67c1f7","added_by":"auto","created_at":"2024-01-03 09:11:33","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":71730,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR spectra of \u003cstrong\u003e(a)\u003c/strong\u003eblank hydrogel, \u003cstrong\u003e(b)\u003c/strong\u003e pure drug and (\u003cstrong\u003ec)\u003c/strong\u003e hydrogel after CIP adsorption\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/7ff5969db9c6b5da74423a81.png"},{"id":49112737,"identity":"c3f00f81-7a92-4ef8-a8f5-d6955e6e392b","added_by":"auto","created_at":"2024-01-03 09:27:34","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":387930,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of \u003cstrong\u003e(a)\u003c/strong\u003e hydrogel before adsorption, and \u003cstrong\u003e(b)\u003c/strong\u003e hydrogel after CIP adsorption\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/12b12aba2e68615442705dbb.png"},{"id":49111875,"identity":"0e0c55f7-cec5-4ae0-8f67-e0be95705c05","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":56900,"visible":true,"origin":"","legend":"\u003cp\u003eTGA thermogram of Pectin–g–poly(AA–co–IA)hydrogel\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/b99d587ba6f508715cb04185.png"},{"id":49112344,"identity":"2f2db48d-46ed-471c-80d2-056e5e4873b5","added_by":"auto","created_at":"2024-01-03 09:19:34","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":49793,"visible":true,"origin":"","legend":"\u003cp\u003eXRD pattern of the \u003cstrong\u003e(a\u003c/strong\u003e) pure drug, \u003cstrong\u003e(b)\u003c/strong\u003e hydrogel before adsorption, and \u003cstrong\u003e(c)\u003c/strong\u003e hydrogel after CIP adsorption\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/7074136ec6e46d392ffeb5b2.png"},{"id":49111881,"identity":"cb4ef0f4-2fea-4338-aa99-5514632cda90","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":258888,"visible":true,"origin":"","legend":"\u003cp\u003evariation\u003cstrong\u003e \u003c/strong\u003ein hydrogel swelling percentage as a function of (\u003cstrong\u003ea\u003c/strong\u003e) MBA content, (\u003cstrong\u003eb\u003c/strong\u003e) Pectin content, (\u003cstrong\u003ec\u003c/strong\u003e) AA content, (\u003cstrong\u003ed\u003c/strong\u003e) IA content, (\u003cstrong\u003ee\u003c/strong\u003e) KPS content, (\u003cstrong\u003ef\u003c/strong\u003e) effect of pH, and (\u003cstrong\u003eg\u003c/strong\u003e) laboratory images for the swelling forms of hydrogel at different pH\u003c/p\u003e","description":"","filename":"7.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/b173386b96455974fd978cd6.png"},{"id":49112345,"identity":"b56836d5-ae9e-477c-a06f-d0ecb3282ce1","added_by":"auto","created_at":"2024-01-03 09:19:34","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":29613,"visible":true,"origin":"","legend":"\u003cp\u003eThe point zero charge graph for Pectin–g–poly(AA–co–IA)hydrogel.\u003c/p\u003e","description":"","filename":"8.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/07567d0031022ab9b0bdcb36.png"},{"id":49111883,"identity":"e4223043-ff8b-41f9-9894-9c4e17f27273","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":106006,"visible":true,"origin":"","legend":"\u003cp\u003eEffect of (\u003cstrong\u003ea\u003c/strong\u003e) pH, (\u003cstrong\u003eb\u003c/strong\u003e) adsorbent dosage, (\u003cstrong\u003ec\u003c/strong\u003e) contact time, and (\u003cstrong\u003ed\u003c/strong\u003e) temperature on the adsorption of CIP drug onto hydrogel\u003c/p\u003e","description":"","filename":"9.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/fba29c5370118ea973282e28.png"},{"id":49111885,"identity":"7df35233-75ca-4751-a250-0bdf4b188b82","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":56436,"visible":true,"origin":"","legend":"\u003cp\u003eThe models isotherm adsorption for CIP drug adsorption onto hydrogel: (\u003cstrong\u003ea\u003c/strong\u003e) Langmuir isotherm, (\u003cstrong\u003eb\u003c/strong\u003e) Freundlich isotherm, and (\u003cstrong\u003ec\u003c/strong\u003e) Temkin model\u003c/p\u003e","description":"","filename":"10.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/933026b1b57e1ed392d03647.png"},{"id":49112346,"identity":"a9552c06-5afb-4041-98cf-82b9d0776031","added_by":"auto","created_at":"2024-01-03 09:19:34","extension":"png","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":19344,"visible":true,"origin":"","legend":"\u003cp\u003eVan't Hoff plot for CIP adsorption onto hydrogel (conditions : pH = 6, concentration =100 mg/ L, volume = 10 mL, contact time =120 min,adsorbent dose = 0.05g)\u003c/p\u003e","description":"","filename":"11.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/ca7902fc3378b7d572b6ec19.png"},{"id":49111878,"identity":"bb39b079-ca8b-47d6-bf4e-992aa8c011ae","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":40329,"visible":true,"origin":"","legend":"\u003cp\u003eThe cumulative release curves of CIP drug from hydrogel at different pH values at 37 °C\u003c/p\u003e","description":"","filename":"12.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/74a69baa8e7b63dc63fd613b.png"},{"id":49111882,"identity":"a1e23112-cc88-42ae-ac8f-e919e406b3a4","added_by":"auto","created_at":"2024-01-03 09:11:34","extension":"png","order_by":13,"title":"Figure 13","display":"","copyAsset":false,"role":"figure","size":43640,"visible":true,"origin":"","legend":"\u003cp\u003eTemperature effect on CIP drug releasing at pH = 7.4\u003c/p\u003e","description":"","filename":"13.png","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/13414ce3f1507ae5ca97b02e.png"},{"id":55022061,"identity":"df00b2a7-d66c-4732-98f6-ad8efc16879a","added_by":"auto","created_at":"2024-04-20 07:54:08","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1698038,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3698789/v1/456bb301-2299-4c46-b324-873524a68a98.pdf"}],"financialInterests":"","formattedTitle":"Synthesis, characterization and swelling behavior of a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co- itaconic acid) hydrogels for adsorption and controlled release of ciprofloxacin","fulltext":[{"header":"Introduction","content":"\u003cp\u003eHydrogels are three-dimensional cross-linked polymeric network that swelling in aqueous solution and physiological fluid as a result the presence of hydrophilic groups such as hydroxyl(\u0026ndash;OH), carboxylic(\u0026ndash;COOH), amide (\u0026ndash;CONH\u003csub\u003e2\u003c/sub\u003e), sulfonic acid (\u0026ndash;SO\u003csub\u003e3\u003c/sub\u003eH), and amino groups (\u0026ndash;NH\u003csub\u003e2\u003c/sub\u003e), which provide enough area for attract foreign materials that are adsorbed on the surface of hydrogels(Sharma et al. \u003cspan citationid=\"CR56\" class=\"CitationRef\"\u003e2022\u003c/span\u003e, Kumar et al. \u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e2023\u003c/span\u003e) .Additionally, hydrogel is capable of absorbing water without losing its structural integrity, making it easier to separate and recycle the hydrogel adsorbents from treated wastewater(Mohamed and Mahmoud \u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Hydrogels superior to conventional adsorption materials in terms of antibiotic residue removal rate, ease of preparation, compatibility with the environment, and efficiency(Song et al. 2023). Hydrogels have been shown to be useful in agriculture(Kaur et al. \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e2023\u003c/span\u003e) and biomedical applications such as controlled drug and protein delivery (Li et al. \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e2021\u003c/span\u003e),wound dressing (Mart\u0026iacute;nez-Ibarra et al. \u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e2019\u003c/span\u003e), and tissue engineering(Roshanbinfar et al. \u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). In general, hydrogels may be developed using synthetic or natural polymers; however, the use of natural polymers like alginate, pectin, starch, and others appears to be more likely due to their economical and biological advantages such as natural abundance, cheap costs, biodegradability, biocompatibility, and lower toxicity(Mota and Fajardo \u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). In recent years, there has been an increase in interest in polysaccharide modification via graft copolymerization(Weerasundara et al. 2021). Grafting synthetic hydrogels on natural polysaccharides helps to overcome some of the disadvantages of virgin polysaccharides, such as contamination from microbes, uncontrolled hydration, and age-related viscosity changes. As a result, synthetic hydrogels with a long life, excellent adsorption capacity, enhanced mechanical properties, and a high swelling nature exist(Thakur et al. \u003cspan citationid=\"CR64\" class=\"CitationRef\"\u003e2018\u003c/span\u003e, Maji and Maiti \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Pectin is a type of linear polysaccharide composed primarily of D-galacturonic acid (GalA) units linked in chains by α-(1\u0026ndash;4)glycosidic bond with a number of carboxyl and hydroxyl groups distributed along the backbone(Sriamornsak \u003cspan citationid=\"CR58\" class=\"CitationRef\"\u003e2011\u003c/span\u003e, Nasrollahzadeh et al. \u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e2020\u003c/span\u003e) .Plants are the primary source of pectin, such as the cell walls of citrus fruits(Kodoth et al. \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Pectin is used in a variety of applications due to its biocompatibility, biodegradability, and non-toxicity, including colon drug delivery, cosmetics, food, and other biological applications (Khotimchenko \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2020\u003c/span\u003e, Kedir et al. \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). Acrylic acid (AA) is a synthetic pH-responsive monomer whose swelling index is primarily affected by the pH of the surrounding environment. Because AA carries a carboxylic acid (functional group) that is strongly associated with water molecules, the state of equilibrium swelling is significantly affected by the ionic strength and the pH level of the swolled solution (Suhail et al. \u003cspan citationid=\"CR59\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).Itaconic acid (IA) is an anionic, hydrophilic, unsaturated dicarboxylic acid that is used in the synthesis of co polymeric hydrogels. It has high pH sensitivity and good biocompatibility, which increases the swelling of hydrogels. Moreover, it copolymerizes easily to produce polymeric chains with -COOH side groups that can form hydrogen bonding with corresponding groups, increasing the mechanical properties of hydrogels(Kim et al. \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Fluoroquinolones (FQs) are a group of strong synthetic antibiotics that are frequently used in human prescription drugs and veterinary medications(Zhang et al. \u003cspan citationid=\"CR72\" class=\"CitationRef\"\u003e2012\u003c/span\u003e). Ciprofloxacin (CIP) is a fluoroquinolone category drugs that is widely used as an antibiotic to treat infections caused by gram-negative as well as gram-positive bacteria(Ebrahimi and Salavaty \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2018\u003c/span\u003e, Ganesan et al. \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). It was mainly employed to treat urinary, digestive, and respiratory illnesses(Prusty et al. \u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e2021\u003c/span\u003e).CIP has very limited bioavailability within aqueous gastric intestinal fluid because of its short half-life and reduce rate of dissolution(Tanwar et al. \u003cspan citationid=\"CR62\" class=\"CitationRef\"\u003e2021\u003c/span\u003e).In order to overcome these challenges, it would be extremely helpful to develop a controlled drug delivery system. Drug delivery systems are necessary for drugs that have a narrow therapeutic window of blood concentrations or that must be eliminated quickly or kept below levels where potentially harmful side effects become prevalent(Gulen and Demircivi \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2020b\u003c/span\u003e).Drug delivery systems have the benefits of increasing the length of stay of a drug within a patient, minimizing frequency of dosing and toxicity, as well as enhancing patient compliance, and thus effectiveness with most dosage requirements(Ameli and Alizadeh \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).Furthermore, drug delivery systems provide protection the loaded drug from enzymatic degradation and low gastric pH, allowing for controlled release in the proximal colon(Anirudhan and Mohan \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2014\u003c/span\u003e).\u003c/p\u003e"},{"header":"Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eChemicals\u003c/h2\u003e \u003cp\u003eWithout additional purification, all chemicals were used. Ciprofloxacin (CIP) (purity\u0026thinsp;\u0026gt;\u0026thinsp;98%,C\u003csub\u003e17\u003c/sub\u003eH\u003csub\u003e18\u003c/sub\u003eFN\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, MW\u0026thinsp;=\u0026thinsp;331.4g/mol, λ\u003csub\u003emax\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;276 nm) was purchased from Macklin Biochemical Co., Ltd., China. Pectin was provided by Merck (Darmstadt, Germany). Acrylic acid (AA, 99% purity,) was provided from CDH Chemical Co., India. Itaconic acid(IA, 99%) was obtained from Macklin Biochemical Co., Ltd., China. N,N'-methylene bis-a acrylamide (MBA,99%) and the initiator potassium persulfate (KPS,99%) were purchased from Shanghai Macklin Biochemical Co., Ltd., China. Sodium chloride, calcium chloride, sodium hydroxide and hydrochloric acid were supplied from Fluka, Switzerland. Deionized water was used to make all solutions.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003eSynthesis of Pectin\u0026ndash;g\u0026ndash;poly(AA\u0026ndash;co\u0026ndash;IA) hydrogel\u003c/h2\u003e \u003cp\u003eFirstly, 1g of pectin was dissolved in 30ml deionized water with continuous stirring at 40\u0026deg;C till the solution was homogeneous. After heating to 60\u0026deg;C at N\u003csub\u003e2\u003c/sub\u003e atmosphere, 0.07 g of initiator KPS (pre-dissolved in 2 mL of deionized water) was added to the solution under stirring to produce radicals. Then, in a separate beaker, 0.7 g of IA was dissolved in 5 mL deionized water and gently heated before being added to the above polymeric solution, and 5mL of AA was added to the mixture while continuously stirring. Following that, 0.05 g of MBA dissolved in 5 mL deionized water was added to the aforementioned polymeric solution. The resultant solution was carefully placed in test tubes after being stirred for 30 minutes at room temperature. It was then maintained in a water bath at 70\u0026deg;C for 2 hours to complete the formation of hydrogel. After the specified polymerization time, hydrogel rods were carefully removed from test tubes and cut into discs of specific dimensions using a sharp-edged blade. To get rid of any unreacted materials, discs were washed in deionized water for 30 minutes. Up until a constant pH value was reached, this washing procedure was repeated with periodic replacement of the washing solution. Discs were completely dried in an oven set at 60\u0026deg;C. The steps in the synthesis of a hydrogel are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003eCharacterization\u003c/h2\u003e \u003cp\u003eUV-vis absorption measurements were carried out at room temperature using a UV 1800 spectrophotometer (Shimadzu, Japan). XRD (XRD-6000, Shimadzu, Japan) and CuK (0.15040 nm) were used to investigate the crystalline or amorphous structure of the pure drug, hydrogel before and after drug adsorption. The XRD pattern was captured in the 10\u0026deg;-80\u0026deg; range.The functional groups in pure drug, hydrogel before and after drug adsorption were identified using Fourier transform infrared (FTIR) spectroscopy (Shimadzu, Japan, 8400s with wave number 400\u0026ndash;4000 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e). SEM (Scanning Electron Microscope) (MIRA3, Tescan, Czech Republic, Iran) with a voltage of 25 kV was used to examine the surface morphology of the hydrogel before and after drug adsorption.\u003c/p\u003e \u003cp\u003eThe thermal behavior of the prepared hydrogel was evaluated by thermogravimetric analysis (TGA), a TGA-4000 Perkin Elmer thermoanalyzer was used.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003eSwelling studies\u003c/h2\u003e \u003cp\u003eThe pre-weighted hydrogel was dissolved in 100 mL of deionized water and allowed to stand at room temperature until the swelling equilibrium was reached. Before weighing, the hydrogel that had swelled up was removed, and extra water on its surface was wiped away with filter paper. The hydrogel that had swelled was weighed using an analytical weighing balance. Using the equation shown below, Eq.\u0026nbsp;(\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), the maximum swelling percentage was determined.\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$\\text{S}\\text{w}\\text{e}\\text{l}\\text{l}\\text{i}\\text{n}\\text{g} \\left(\\text{%}\\right)=\\frac{{\\text{W}}_{\\text{S}}-{\\text{W}}_{\\text{d} }}{{\\text{W}}_{\\text{d}}}\\text{x}100$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eWhere, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{W}}_{\\text{d} }\\)\u003c/span\u003e\u003c/span\u003eis the weight of dry hydrogel and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{W}}_{\\text{S}}\\)\u003c/span\u003e\u003c/span\u003e is the weight of swollen hydrogel.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003ePoint zero charge (pzc) determination\u003c/h2\u003e \u003cp\u003eUsing a pH drift method, the pH of hydrogel with zero charge was investigated. A 150 mL conical flask containing 50 mL of deionized water was used for the measurement of pzc. Different pH solutions (pHi) in the varied of 2 to 11 were prepared using solutions of 0.1M NaOH and 0.1M HCl. After that, 0.05 g of hydrogel was added to each flask, which was then shaken at 130 rpm for 24 hours to reach the equilibrium point. The pH of the liquid was measured after 24 hours and is represented by (pH\u003csub\u003ef\u003c/sub\u003e).The value of pzc for prepared hydrogel was determined by graphing the relationship between initial pH (pHi) against ΔpH, where ΔpH represents the difference between pHi and pHf values. The pHi at which ΔpH becomes zero was taken into account as pzc of hydrogel(Verma et al. \u003cspan citationid=\"CR67\" class=\"CitationRef\"\u003e2020\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eBatch adsorption studies\u003c/h2\u003e \u003cp\u003eA UV-visible spectroscope was used to examine batch CIP adsorption on hydrogel adsorbent. To establish the ideal adsorption conditions, various adsorption factors like contact time, pH, adsorbent dose, temperature, and ionic strength were studied. At room temperature, 0.05g of the dried hydrogel was immersed in 10 mL of CIP solution (100 mg/L) with stirring at 130 rpm. After reaching equilibrium (about 120 minutes of contact time), the drug solutions were removed and centrifuged for 5 minutes (at 5000 rpm). A UV-vis spectrophotometer with a maximum wavelength of 276 nm was used to determine the remaining concentration of the drug solution. The CIP drug was quantified using an external calibration curve (y\u0026thinsp;=\u0026thinsp;0.089x\u0026thinsp;+\u0026thinsp;0.01354) with an R\u003csup\u003e2\u003c/sup\u003e value of 0.9982. According to Eq.\u0026nbsp;(\u003cspan refid=\"Equ2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), the changes in drug concentration before and after adsorption were used to calculate the equilibrium adsorption capacity, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{e}}(\\text{m}\\text{g}/\\text{g})\\)\u003c/span\u003e\u003c/span\u003e (Majid et al. \u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$${q}_{e }=\\frac{{C}_{o}-{C}_{e }*V}{m}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe drug removal efficiency (% Removal) is calculated using Eq.\u0026nbsp;(\u003cspan refid=\"Equ3\" class=\"InternalRef\"\u003e3\u003c/span\u003e).\u003cdiv id=\"Equ3\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ3\" name=\"EquationSource\"\u003e\n$$\\text{R}\\text{e}\\text{m}\\text{o}\\text{v}\\text{a}\\text{l}\\left(\\text{%}\\right)=\\frac{{\\text{C}}_{\\text{o}}-{\\text{C}}_{\\text{e} }}{{\\text{C}}_{\\text{o}}} \\text{x}100$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e3\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eWhere, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{0}\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e indicates the initial and equilibrium drug concentrations in (mg/L), respectively, m is the adsorbent dose in (g), and V is the volume of drug solution in (L).\u003c/p\u003e \u003cdiv id=\"Sec9\" class=\"Section3\"\u003e \u003ch2\u003eIn vitro drug release study\u003c/h2\u003e \u003cp\u003eAfter optimizing the variables controlling the CIP drug loading as previously described, to investigate the CIP drug release. The drug in vitro release study from the hydrogel was performed in a shaking incubator at 37\u0026deg;C and 50 rpm. The CIP drug-loaded hydrogel (0.1 g) was submerged in a predetermined volume of gastric and intestinal liquids with pH values of 1.2 and 7.4, respectively. 2 mL of the medium was removed for absorbance tests at the proper intervals. To maintain the bath volume constant, fresh 2 mL buffer solution was added every time. Employing a calibration curve of the CIP drug at various concentrations, the UV\u0026ndash;vis spectrophotometer was used to determine the concentration of CIP drug releasing at 276 nm. Using Eq.\u0026nbsp;(\u003cspan refid=\"Equ5\" class=\"InternalRef\"\u003e4\u003c/span\u003e), the release percentage was determined(Hanna and Saad \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003cdiv id=\"Equ4\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ4\" name=\"EquationSource\"\u003e\n$$\\left(\\text{%}\\right)\\text{o}\\text{f} \\text{d}\\text{r}\\text{u}\\text{g} \\text{r}\\text{e}\\text{l}\\text{e}\\text{a}\\text{s}\\text{e}=\\frac{\\text{A}\\text{m}\\text{o}\\text{u}\\text{n}\\text{t} \\text{o}\\text{f} \\text{C}\\text{I}\\text{P} \\text{d}\\text{r}\\text{u}\\text{g} \\text{r}\\text{e}\\text{l}\\text{e}\\text{a}\\text{s}\\text{e}\\text{d}}{\\text{A}\\text{m}\\text{o}\\text{u}\\text{n}\\text{t} \\text{o}\\text{f} \\text{C}\\text{I}\\text{P} \\text{d}\\text{r}\\text{u}\\text{g} \\text{a}\\text{d}\\text{s}\\text{o}\\text{r}\\text{b}\\text{e}\\text{d} \\text{w}\\text{i}\\text{t}\\text{h}\\text{i}\\text{n} \\text{t}\\text{h}\\text{e} \\text{h}\\text{y}\\text{d}\\text{r}\\text{o}\\text{g}\\text{e}\\text{l} } \\text{x}100$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e4\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e"},{"header":"Results and Discussion","content":"\u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003eHydrogel Formation Mechanism\u003c/h2\u003e \u003cp\u003eIn this study, Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e illustrates a potential mechanism for the grafting of acrylic acid and itaconic acid monomers onto the Pectin backbone via the free radical polymerization method. In the first step, the initiator KPS was broken down into sulfate anion-radicals while being heated at 70\u0026deg;C. These radicals then produced alkoxy radicals by removing hydrogen atoms from the hydroxyl groups of the Pectin chains. Following the addition of the monomer molecules (acrylic and itaconic acids), the active radical sites on the Pectin chains would start the vinyl groups of the monomers to create chains propagation. During chain propagation, MBA with double vinyl groups operated as cross-link points via covalent bonding at both ends of the linear polymer chains, resulting in the formation of a Pectin-g-poly(AA-co-IA) hydrogel network(Mohammadzadeh Pakdel et al. \u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).\u003c/p\u003e\u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003eFTIR Analysis\u003c/h2\u003e \u003cp\u003eThe changes in structure throughout grafting copolymerization and drug adsorption were investigated using an FTIR spectrum comparison, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. According to the literature, Pectin exhibits a peak of -OH groups at 3402 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, C-H group at 2928 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, and -C\u0026thinsp;=\u0026thinsp;O group at 1749 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e resulting from the presence of COOCH\u003csub\u003e3\u003c/sub\u003e group, -CH\u003csub\u003e2\u003c/sub\u003e scissoring and -OH bending vibrations at 1441 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 1342 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e respectively, and -CH-OH group vibrations at 1150 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e(Kowalski et al. \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). Acrylic acid is reported to have peaks of -OH groups at 3380 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, -CH\u003csub\u003e2\u003c/sub\u003e groups at 2973 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, -C\u0026thinsp;=\u0026thinsp;O groups at 1707 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, -C-C groups at 1709 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, -C\u0026thinsp;=\u0026thinsp;C groups at 1626 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, and -C-O-C groups at 1173 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e (Feng et al. \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Itaconic acid is reported to shows broad peaks at 3085 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e that correlate with -OH stretching, 2750 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e associated to -CH\u003csub\u003e2\u003c/sub\u003e asymmetric stretching mode, and 1427 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e related to C-C bending vibration. The C\u0026thinsp;=\u0026thinsp;O stretching vibration was assigned a peak at 1695 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, 1620 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e may be attributed to C\u0026thinsp;=\u0026thinsp;C stretching vibrations, and the C-O-C stretching vibration was ascribed a peak at 1203 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e(Olvera-Sosa et al. \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e2020\u003c/span\u003e).Crosslinking agent (MBA) is reported to shows peak at 3302 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e is correlated with N\u0026ndash;H stretching vibrations. The peak at 1655 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e is associated with C\u0026thinsp;=\u0026thinsp;O group, while the peak at 1538 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e indicates existence of C\u0026thinsp;=\u0026thinsp;C groups on MBA(Ayu Laksanawati and Novarita Trisanti 2019). On observing FTIR spectra of prepared hydrogels as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea, It is notable that significant differences can be observed between the prepared hydrogel and the monomers due to crosslinking of the chains of polymeric to develop Pectin\u0026ndash;g\u0026ndash;poly(AA\u0026ndash;co\u0026ndash;IA) network. The overlapping of the O-H stretching vibrations and N-H stretching vibrations (amide group) of the crosslinking agent( MBA) was observed by a broad peak in the range of 3000\u0026ndash;3564 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e (Hu et al. \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). The absorption band of C\u0026thinsp;=\u0026thinsp;O groups in Pectin (1749 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), acrylic acid (1707 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), itaconic acid (1695 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and MBA(1615 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) are shifted towards wave number (1712 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) because of carbonyl groups depletion in the synthesis of cross-linked network structure(Ajaz et al. \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The peak at 1164 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e could be attributed to stretching vibration of C\u0026ndash;N in MBA(Dai et al. \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). The absorption band of a C\u0026thinsp;=\u0026thinsp;C stretching vibration that typically appears at 1626 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in acrylic acid and1620 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in itaconic acid was not observed in prepared hydrogel, which suggests that polymerization reaction has occurred to the monomers (Sun et al. \u003cspan citationid=\"CR60\" class=\"CitationRef\"\u003e2013\u003c/span\u003e).All these changes in peaks indicate that acrylic acid and itaconic acid grafting on backbone of pectin to form Pectin\u0026ndash;g\u0026ndash;poly(AA\u0026ndash;co\u0026ndash;IA) hydrogel. The FTIR spectrum of pure ciprofloxacin displays numerous absorption bands, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb. The O-H stretching in COOH at 3379 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e has the most distinctive bands. The band at 3525 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e could be ascribed to N-H group stretching vibrations. Another band at 2923cm\u003csup\u003e\u003cem\u003e\u0026minus;\u003c/em\u003e\u0026thinsp;1\u003c/sup\u003e represented alkenes and aromatic C\u0026ndash;H stretching vibrations. The peaks at 1704 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 1620 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e due to the C\u0026thinsp;=\u0026thinsp;O stretching in COOH and 4-quinolone, respectively. The C\u0026thinsp;=\u0026thinsp;C stretching in aromatic ring at 1465 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and the C\u0026ndash;O stretching in COOH at 1265 cm\u003csup\u003e\u003cem\u003e\u0026minus;\u003c/em\u003e\u0026thinsp;1\u003c/sup\u003e. In addition, a band at 933 cm\u003csup\u003e\u003cem\u003e\u0026minus;\u003c/em\u003e\u0026thinsp;1\u003c/sup\u003e was assigned to C-F group(Kowalczuk \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). FTIR spectrum of drug loaded with hydrogel demonstrates in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ec, it can be seen that the intensity and position of peaks assigned to characteristic functional groups were either disappeared or slightly shifted after drug adsorption, indicating that H\u0026ndash;bonding and electrostatic interactions are present between the hydrogel and the drug.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec13\" class=\"Section2\"\u003e \u003ch2\u003eSEM Analysis\u003c/h2\u003e \u003cp\u003eSEM was employed to study the surface appearance of hydrogel because it provides a magnified view of the material for easy visualization and analysis. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e shows SEM micrographs of hydrogel prior to adsorption and hydrogel adsorbed with CIP. The SEM analysis of the hydrogel prior to CIP adsorption, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea, revealed a smooth surface with some cracks distributed throughout the Pectin-g-poly(AA-co-IA) surface. Following CIP adsorption, the hydrogel surface changed significantly, becoming coarse and containing a bulky intense layer, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb. These changes could be attributed to CIP drug adsorption on the hydrogel surface.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section2\"\u003e \u003ch2\u003eTGA Analysis\u003c/h2\u003e \u003cp\u003eTGA is widely regarded as an extremely important technique for determining the thermal stability of polymeric materials. It measures the amount of weight loss in a sample as a function of temperature. Figure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e depicts the TGA curve of the prepared hydrogel at temperatures ranging from 40 to 800\u0026deg;C, with weight loss occurring in three stages during the thermal decomposition process. The first stage occurred at 30 to 140\u0026deg;C and is due to the loss of water content from the hydrogel, resulting in approximately 9.48% weight loss. The second stage began at temperatures ranging from 140 to 280\u0026deg;C, and during this stage, the hydrogel lost 26.83% of its total weight. The third stage had a weight loss of 99.482% and was situated between 350 and 800\u0026deg;C. The second and third stages were connected to a number of intricate processes, such as the dehydration of saccharide rings, the breaking down of C-O-C bonds in the Pectin chain, the breakdown of branches and side chain groups in the graft copolymer, the splitting of the PAA/IA chains, and the dissolution of the cross-linked network structure(Ilgin et al. \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2020\u003c/span\u003e).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec15\" class=\"Section2\"\u003e \u003ch2\u003eXRD Analysis\u003c/h2\u003e \u003cp\u003eThe crystalline, semi-crystalline, and amorphous nature of the materials can be quickly determined using the fundamental analytical technique known as XRD. Figure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ea, depicts the XRD pattern of the pure CIP drug. It is obvious that the pure drug displayed numerous sharp peaks at positions 2θ\u0026thinsp;=\u0026thinsp;10˚ to 45˚, indicating the drug crystalline nature(Khan et al. \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Figure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003eb, shows the prepared hydrogel XRD pattern. It is evident that the hydrogel is amorphous because there are no distinct diffraction peaks other than a broad band between 2θ\u0026thinsp;=\u0026thinsp;15\u0026deg; and 45\u0026deg;. The characteristic peaks of the crystalline CIP drug were not observed in the X-ray diffractograms, as shown in the XRD pattern of CIP adsorption onto hydrogel in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ec, suggesting loss of crystallinity of CIP in addition to successful adsorption of CIP into a developed superabsorbent hydrogel.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec16\" class=\"Section2\"\u003e \u003ch2\u003eOptimization of Pectin\u0026ndash;g\u0026ndash;poly(AA\u0026ndash;co\u0026ndash;IA)hydrogel swelling\u003c/h2\u003e \u003cdiv id=\"Sec17\" class=\"Section3\"\u003e \u003ch2\u003eEffect of Cross Linker Content\u003c/h2\u003e \u003cp\u003eThe presence of cross-linkers is an important factor in determining the swelling capacity of a superabsorbent hydrogel because cross-linkers make the hydrogel insoluble in aqueous environments(Hasija et al. \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). To investigate the effect of cross-linker content on swelling percentage, swelling was examined at five different cross-linking amounts varying from 0.001 to 0.1g. As illustrated in Fig.\u0026nbsp;7a. The swelling percentage increased as the cross-linking agent content increased from 0.001 to 0.05 g, with the maximum swelling attained when the amount of crosslinking agent was 0.05g. When the cross-linker amount raised and exceeded 0.05 g, more cross-linking points were created through polymerization, resulting in a grater cross-linking density and less hydrodynamic free volume available to accommodate water molecules, which reduced swelling(Sharika and Mohanan \u003cspan citationid=\"CR54\" class=\"CitationRef\"\u003e2021\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec18\" class=\"Section2\"\u003e \u003ch2\u003eEffect of Pectin Content\u003c/h2\u003e \u003cp\u003eUsing deionized water at constant other influencing conditions, Fig .7b illustrates the impact of varying the pectin content (0.3\u0026ndash;2g) on the level of swelling of the developed hydrogel. The results showed that increasing the amount of pectin in the hydrogel matrix from 0.3 to 1g significantly enhanced the swelling degree from 1600 to 2350%. This is because pectin naturally contains a variety of OH and COOH groups that contribute to the hydrophilic properties of the hydrogel network. As a result, the hydrogel network swells more due to the greater attraction of water molecules for diffusion into the gel matrix. whereas, the swelling ratio decreased to 1207% with additional Pectin content up to 2g because of increasing the density of the hydrogel network, and thus, the rate of water molecule diffusion reduces, resulting in a decrease in the swelling level value. Additionally, with increased Pectin content, the viscosity of the reaction medium will obviously increase, which inhibited the free movement and uniform distribution of other reactants in the reaction system(Wang et al. 2017, Omer et al. \u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e2023\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec19\" class=\"Section2\"\u003e \u003ch2\u003eEffect of Acrylic Acid Content\u003c/h2\u003e \u003cp\u003eTo examine the impact of acrylic acid monomer on hydrogel swelling ratio, monomer volume was varied between (1.0\u0026ndash;10 mL), and the results are displayed in Fig.\u0026nbsp;7c. The swelling percentage increased significantly as the AA monomer content increased from 1 to 5 mL, and the swelling percentage increased from 1100 to 2530%, respectively. This could be attributed to the increased amount of AA providing more hydrophilic groups such as \u0026ndash;COO\u0026ndash; and -COOH grafted onto the Pectin, which could enhance the hydrogel swelling ability. Nonetheless, after 5 mL, the swelling level of hydrogel with increased AA content declines significantly and reaches 1400% at 10 mL. This is most likely explained by an increase in reaction medium viscosity and restricted free radical movement, in addition to preferred photopolymerization over graft copolymerization and a reduction in osmotic pressure difference, leading to hydrogel network shrinkage(Tanan et al. \u003cspan citationid=\"CR61\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec20\" class=\"Section2\"\u003e \u003ch2\u003eEffect of Itaconic Acid Content\u003c/h2\u003e \u003cp\u003eThe relationship between IA content and hydrogel swelling percentage was investigated over a range of 0.3 to 1.5 g, with the highest swelling percentage found at a content of 0.7 g as shown in Fig.\u0026nbsp;7d. Due to a higher hydrogel swelling percentage, raising the IA content from 0.3 g to 0.7 g leads to more IA molecules available for the chain propagation sites on the graft copolymer network. IA content greater than 0.7 g accelerated the photopolymerization reaction and reduced the hydrogel swelling percentage(Thakur et al. \u003cspan citationid=\"CR63\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec21\" class=\"Section2\"\u003e \u003ch2\u003eEffect of Initiator Content\u003c/h2\u003e \u003cp\u003eThe effect of the initiator content on the hydrogel swelling percentage is shown in Fig.\u0026nbsp;7e. KPS initiator had a range of 0.01 to 0.1g of content. When the KPS content was increased from 0.01 to 0.07g, it was observed that the swelling percentage improved from 1350 to 2488%. This is because there were sufficient active free radicals on the pectin backbone and monomers, which is what caused the swelling(He et al. \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). However, increasing the initiator content above 0.07g caused the swelling percentage to decrease. This, in turn, led to an increase in the terminating step reaction through bimolecular collision, which in turn increased crosslinking density. Another factor contributing to swelling-loss at higher KPS concentrations is the oxidative damage from free radicals(Bagheri Marandi et al. \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2011\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec22\" class=\"Section2\"\u003e \u003ch2\u003eEffect of pH\u003c/h2\u003e \u003cp\u003eThe influence of pH on the swelling behaviors of hydrogel was studied using different pH solutions that varied from 2 to 10, as displayed in Fig.\u0026nbsp;7f,g. It can be observed that the swelling of the hydrogel increases linearly as the pH of the solution increases. The maximum swelling capacity of hydrogel is at pH\u0026thinsp;=\u0026thinsp;7.4. When the pH rises above 7.4, the water absorbency gradually decreases. Most carboxylate anions \u0026ndash;COO \u003csup\u003e\u0026ndash;\u003c/sup\u003e are protonated and converted to COOH groups under strongly acidic environments (pH\u0026thinsp;\u0026le;\u0026thinsp;4). The electrostatic repulsion between carboxylate anions \u0026ndash;COO\u003csup\u003e\u0026ndash;\u003c/sup\u003e groups was reduced, and as a result, swelling ratio were reduced(Sharma et al. \u003cspan citationid=\"CR55\" class=\"CitationRef\"\u003e2014\u003c/span\u003e). Additionally, protonation results in the strengthening of H-bonds among COOH, which raises the level of physical crosslinking in the skeleton network and reduces the hydrogel tendency to swell. With pH levels rising, some COOH groups are converted to \u0026ndash;COO\u003csup\u003e\u0026ndash;\u003c/sup\u003e, weakening the H-bonding interactions and the adverse impact of H\u003csup\u003e+\u003c/sup\u003e on electrostatic repulsion between carboxylate groups \u0026ndash;COO\u003csup\u003e\u0026ndash;\u003c/sup\u003e. As a result of the strong anion-anion repulsion, the degree of physical crosslinking is reduced. As a result, the swelling percentage increases noticeably and reaches its maximum (2602%) at pH\u0026thinsp;=\u0026thinsp;7.4. On the other hand, at pH\u0026thinsp;\u0026gt;\u0026thinsp;7.4, the swelling of hydrogel is significantly reduced as the pH rises. This behavior could be explained by the \"charge shielding effect\" of excessive Na\u003csup\u003e+\u003c/sup\u003e in the swelling media, which protects the carboxylate anions \u0026ndash;COO\u003csup\u003e\u0026ndash;\u003c/sup\u003eand inhibits effective anion-anion repulsion, resulting in a lower swelling percentage(Li et al. \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2015\u003c/span\u003e).\u003c/p\u003e \u003cdiv id=\"Sec23\" class=\"Section3\"\u003e \u003ch2\u003ePoint zero charge of synthesis hydrogel\u003c/h2\u003e \u003cp\u003eThe electrostatic attraction between the functional groups of the drug molecule and the hydrogel surface functionality determines how well the CIP drug will bind to the surface. The initial pH of the water has an impact on the surface charge of the hydrogel. The hydrogel functional groups experience deprotonation as pHi rises. In more specific terms, the hydrogel surface is going to be positively charged if pHi\u0026thinsp;\u0026lt;\u0026thinsp;pHpzc and negatively charged when pHi\u0026thinsp;\u0026gt;\u0026thinsp;pHpzc. In our study, the pHpzc for hydrogel is 4.2, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e8\u003c/span\u003e, indicating that for pH values below 4.2, the active regions on hydrogel have a positive charge. At pH level exceeds 4.2, the hydrogel surface becomes negatively charged\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec24\" class=\"Section2\"\u003e \u003ch2\u003eEffects of the adsorption parameters\u003c/h2\u003e \u003cdiv id=\"Sec25\" class=\"Section3\"\u003e \u003ch2\u003eEffect of Solution pH\u003c/h2\u003e \u003cp\u003epH represents one of the most key factors in drug adsorption because it influences drug speciation, adsorbent capacity, and surface charge, all of which influence drug interactions. To better understand the impact of pH, batch experiments were conducted under controlled conditions with pH ranging from 2 to 11, while maintaining the other process parameters constant at their ideal levels (initial concentration\u0026thinsp;=\u0026thinsp;100 mg/L, adsorbent dosage 0.05g, contact time\u0026thinsp;=\u0026thinsp;120 min, and temperature\u0026thinsp;=\u0026thinsp;15\u003csup\u003e◦\u003c/sup\u003eC). Since CIP is an antibiotic, the protonation of the amine group causes it to exist in a cationic form (CIP+) at pH 5.9. The ionization of the carboxylic acid causes the CIP to exist in an anionic form (CIP\u0026minus;) when the pH is higher than 8.9. Additionally, the CIP can exist in the pH range of 5.9 to 8.9 in a zwitterionic form (CIP \u0026plusmn;)(Gulen and Demircivi \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2020\u003c/span\u003ea, Igwegbe et al. \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e9\u003c/span\u003ea, the CIP adsorption capacity gradually increased from 2 to 6, then gradually declined from 6 to 11, with a particularly rapid decline at pH 7. This is clarified by the electrostatic attraction that occurs between the hydrogel surface charge and the charge of the CIP. The hydrogel surface becomes negatively charged at pH 6 (greater than point zero charge), and CIP molecules are positively charged, resulting in strong electrostatic attraction between the cationic (CIP+) and the negatively charged of the hydrogel surface. The rapid decrease after pH 7 could be attributed to electrostatic repulsion between the anionic (CIP) and negatively charged hydrogel surface(Tran et al. 2022). At pH\u0026thinsp;\u0026gt;\u0026thinsp;7 (with anionic CIP as the dominant species), a significant reduction in CIP removal was observed, which is attributed to electrostatic repulsion between the anionic drug (CIP\u0026minus;) and the negatively charged adsorbent. Additionally, as can be seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e9\u003c/span\u003ea, adsorption was reduced when the solution pH was below 4 because the hydrogel surface has a positive charge at pH\u0026thinsp;\u0026lt;\u0026thinsp;4.2 (pH\u0026thinsp;\u0026lt;\u0026thinsp;pHpzc), which causes electrostatic repulsion between the cationic species (CIP+) and the positively charged hydrogel surface(Yadav et al. \u003cspan citationid=\"CR71\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Consequently, in this study, a pH of 6 was purposefully chosen as the optimum adsorption condition for the CIP drug .\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec26\" class=\"Section3\"\u003e \u003ch2\u003eEffect of Adsorbent Dosage\u003c/h2\u003e \u003cp\u003eAdsorbent dosage is a significant factor that influences the effectiveness of adsorption. In general, it is preferable for economic adsorption to use a small amount of adsorbent that can achieve a high adsorption percentage. The effectiveness of CIP removal was examined using experimental conditions, and the effects are depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e9\u003c/span\u003eb, for a hydrogel adsorbent dosage range of 0.005 g to 0.1 g, while the other process variables remained constant and at their ideal levels (initial concentration\u0026thinsp;=\u0026thinsp;100 mg/L, pH\u0026thinsp;=\u0026thinsp;6, contact time\u0026thinsp;=\u0026thinsp;120 min, and temperature\u0026thinsp;=\u0026thinsp;15\u003csup\u003e◦\u003c/sup\u003eC). It was discovered that increasing the adsorbent dosage from 0.005 to 0.1g caused the removal efficiency of CIP to rise from 86.55\u0026ndash;94.75%.The increased adsorbent dosage resulted in a greater number of functional groups and more available sites for adsorption, which contributed to the improvement in removal efficiency. Nevertheless, when the adsorption process attained saturation, the impact of introduced more adsorbent was not significant. Consequently, it is important to optimize the adsorbent dosage with respect to both efficiency and cost-effectiveness(Lu et al. \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The adsorbent dosage of 0.05 g was selected for further experiments in this study.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec27\" class=\"Section3\"\u003e \u003ch2\u003eThe Effect of Contact Time\u003c/h2\u003e \u003cp\u003eThe influence of contact time on CIP removal efficiency was examined over a time ranging from 1-250 min at an initial concentration of 100 mg/L while maintaining a constant pH, adsorbent dosage, and temperature of 6, 0.05g, and 15\u003csup\u003e◦\u003c/sup\u003eC, respectively. As displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e9\u003c/span\u003ec, the removal efficiency raised rapidly as time increased at first, then attained a constant value. Due to the adsorption sites on the adsorbent surface are vacant at first, the adsorption is rapid(Avcı et al. \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Furthermore, the hydrogel three-dimensional polymeric network and porous structure likely reduce mass transfer resistance and enhance CIP diffusion into the interior of the adsorbents. Then it gradually slows until it reaches a constant value of 120min. At the start of the adsorption process, the active sites rapidly adsorb a large number of CIP till the outer surface is completely saturated. CIP enters the adsorbent pores after the outer surface is saturated and is adsorbed into the interior surface of the hydrogel(Mohammadinezhad et al. \u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). As a result, adsorption equilibrium might be reached in 120 minutes.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec28\" class=\"Section2\"\u003e \u003ch2\u003eEffect of Temperature\u003c/h2\u003e \u003cp\u003eTemperature can have a significant impact on the affinity of the adsorbent to the CIP molecules. As a result, the effect of solution temperature on the level of CIP removal was investigated at temperatures ranging from 15\u0026deg;C to 35\u0026deg;C, while concentration, pH, adsorbent dosage, and contact time were kept constant at 100 mg/L, 6, 0.05g, and 150 min, respectively. The results of the temperature impacts are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e9\u003c/span\u003ed, where decreasing the temperature is clearly preferable for CIP removal onto hydrogel (94.07%), whereas CIP removal reduces as solution temperature increases up to 35\u0026deg;C. This indicates the exothermic nature of the adsorption process. In most exothermic adsorption processes, increasing the temperature causes desorption of the target contaminants to the liquid phase at equilibrium(Cheng et al. \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). In another way, as temperature increases, the diffusive transfer of mass and solubility of CIP in water increase, weakening the adsorptive forces between adsorbent sites. As consequently, physical adsorption would be reduced and removal efficiency would be reduced (Saber et al. \u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Therefore, 15\u0026deg;C was selected for the subsequent experiments.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec29\" class=\"Section2\"\u003e \u003ch2\u003eAdsorption Isotherm Studies\u003c/h2\u003e \u003cp\u003eAdsorption Isotherm studies were carried out to investigate a single layer or multiple-layer adsorption. For the isotherm experiments, 10 mL of CIP solution was placed in a 50 mL conical flask with 0.05 g of adsorbent at various concentrations (10\u0026ndash;300 mg/L). These solutions were then shaken for 120 minutes in a thermostat shaker set to 15\u0026deg;C (130 rpm). The remaining CIP concentration was determined using a UV-vis spectrophotometer. Various isotherm models, including Langmuir, Freundlich, and Temkin, were used to analyze the data\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eLangmuir model\u003c/h3\u003e\n\u003cp\u003eAssumes that adsorption takes place homogeneous adsorption where the sorption process is monolayer adsorption and each adsorbate molecule onto the surface has equal sorption activation energy(Balarak and McKay \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The following Eq.\u0026nbsp;(\u003cspan refid=\"Equ5\" class=\"InternalRef\"\u003e4\u003c/span\u003e) illustrates the Langmuir isotherm equation.\u003cdiv id=\"Equ5\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ5\" name=\"EquationSource\"\u003e\n$$\\frac{{\\mathbf{C}}_{\\mathbf{e}}}{{\\mathbf{q}}_{\\mathbf{e}}}=\\frac{1}{{\\mathbf{q}}_{\\mathbf{m} }.{\\mathbf{K}}_{\\mathbf{L}}}+\\left(\\frac{1}{{\\mathbf{q}}_{\\mathbf{m}}}\\right).{\\mathbf{C}}_{\\mathbf{e}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e4\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe equilibrium adsorbate solution concentration is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e(mg/L), the equilibrium adsorption capacity is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{e}}(\\text{m}\\text{g}/\\text{g})\\)\u003c/span\u003e\u003c/span\u003e, the maximum adsorption capacity is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{m} }(\\text{m}\\text{g}/\\text{g})\\)\u003c/span\u003e\u003c/span\u003e, and the equilibrium Langmuir's constant is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{K}}_{\\text{L}}(\\text{L}/\\text{m}\\text{g})\\)\u003c/span\u003e\u003c/span\u003e. By analyzing the slope and intercept of the plot of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e/\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003eagainst \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e, the values of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{m} }\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{K}}_{\\text{L}}\\)\u003c/span\u003e\u003c/span\u003e were calculated.\u003c/p\u003e \u003cdiv id=\"Sec31\" class=\"Section2\"\u003e \u003ch2\u003eFreundlich Isotherm\u003c/h2\u003e \u003cp\u003eIn the case of multilayer adsorption systems, the Freundlich isotherm is applied to a heterogeneous surface. Every site has undergone the adsorption process(Ayouch et al. \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The Freundlich isotherm equation is shown in the following Eq.\u0026nbsp;(\u003cspan refid=\"Equ6\" class=\"InternalRef\"\u003e5\u003c/span\u003e).\u003cdiv id=\"Equ6\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ6\" name=\"EquationSource\"\u003e\n$$\\text{l}\\text{o}\\text{g}{\\text{q}}_{\\text{e}}=\\text{l}\\text{o}\\text{g}{\\text{K}}_{\\text{f}}+\\frac{ 1 }{\\text{n}}\\text{l}\\text{o}\\text{g}{\\text{C}}_{\\text{e}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e5\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere, the adsorption intensity is indicated by the exponent \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(1/\\text{n}\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{K}}_{\\text{f}}\\)\u003c/span\u003e\u003c/span\u003e is the constant associated with the adsorption capacity. The favorability and capacity of the adsorption system are indicated by the value of 1/n. Eq.\u0026nbsp;(\u003cspan refid=\"Equ6\" class=\"InternalRef\"\u003e5\u003c/span\u003e) states that the Freundlich constant \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{K}}_{\\text{f}}\\)\u003c/span\u003e\u003c/span\u003e is the intercept and that the slope of a plot of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{l}\\text{o}\\text{g}{q}_{e}\\)\u003c/span\u003e\u003c/span\u003e versus \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{l}\\text{o}\\text{g} {\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e is equal to \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(1/\\text{n}\\)\u003c/span\u003e\u003c/span\u003e.\u003c/p\u003e \u003cdiv id=\"Sec32\" class=\"Section3\"\u003e \u003ch2\u003eTemkin Isotherm\u003c/h2\u003e \u003cp\u003eis predicated on the idea that adsorption heat decreases inversely with the amount of adsorbent surface covered, and that an even distribution of binding energies exists up to the maximum binding energy(Peng et al. \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). In Eq.\u0026nbsp;(\u003cspan refid=\"Equ7\" class=\"InternalRef\"\u003e6\u003c/span\u003e), the Temkin isotherm is displayed.\u003cdiv id=\"Equ7\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ7\" name=\"EquationSource\"\u003e\n$${\\text{q}}_{\\text{e}}=\\text{B}\\text{l}\\text{n}{\\text{K}}_{\\text{T}}+\\text{B}\\text{l}\\text{n}{\\text{C}}_{\\text{e}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e6\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eWhere KT (L /mg), R(8.314 J/mol.K), and T(K) are the Temkin parameters associated with the absolute temperature, the gas constant, and the equilibrium binding constant, respectively. \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{b}\\)\u003c/span\u003e\u003c/span\u003e is heat of adsorption,\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{B}=\\text{R}\\text{T}/\\text{b}\\)\u003c/span\u003e\u003c/span\u003e. By plotting of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{q}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e against \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\left(\\text{l}\\text{n}{\\text{C}}_{\\text{e}}\\right)\\)\u003c/span\u003e\u003c/span\u003e,Slope is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{B}\\)\u003c/span\u003e\u003c/span\u003e and intercept is \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\text{B}\\text{l}\\text{n}{\\text{K}}_{\\text{T}}\\)\u003c/span\u003e\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eThe correlation coefficients and constants of Langmuir, Freundlich and Temkin models for the adsorption of CIP\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"3\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eLangmuir\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eFreundlich\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eTimken\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eR\u003csup\u003e2\u003c/sup\u003e 0.7299\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eR\u003csup\u003e2\u003c/sup\u003e 0.9986\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eR\u003csup\u003e2\u003c/sup\u003e 0.7866\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eq\u003csub\u003emax\u003c/sub\u003e 192.307\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003en 1.115\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eB 13.626\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eK\u003csub\u003eL\u003c/sub\u003e 0.020\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eK\u003csub\u003eF\u003c/sub\u003e 4.031\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eK\u003csub\u003eT\u003c/sub\u003e 1.414\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe Freundlich isotherm model was used to fit the adsorption isotherm data. Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e summarizes the obtained parameters. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e10\u003c/span\u003eb, the Freundlich model established the adsorption of CIP drug from aqueous solutions using Pectin-g-poly (AA-co-IA). Under the Freundlich model, the value of (n) in (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e) demonstrates the strength of adsorption and classifies the type of adsorption as favorable (1\u0026thinsp;\u0026lt;\u0026thinsp;n), unfavorable (1\u0026thinsp;\u0026gt;\u0026thinsp;n), or irreversible (n\u0026thinsp;=\u0026thinsp;1). The heterogeneity condition was confirmed in the current context since the value of (n) was greater than one (n\u0026thinsp;\u0026gt;\u0026thinsp;1). In addition, the Freundlich model R\u003csup\u003e2\u003c/sup\u003e correlation value is significantly greater than those of the Langmuir and Temkin models. Hence, the Freundlich isotherm more closely matches the adsorption data, suggesting that the bulk solution of drug molecules are adsorbed onto a heterogeneity multiple-layer(Chen et al. \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2019\u003c/span\u003e, Wu et al. \u003cspan citationid=\"CR70\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec33\" class=\"Section3\"\u003e \u003ch2\u003eAdsorption Thermodynamics Studies\u003c/h2\u003e \u003cp\u003eTo investigate the spontaneity of the adsorption process, thermodynamic parameters were established. The change in enthalpy (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{H}}^{0}\\)\u003c/span\u003e\u003c/span\u003e), free energy (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{G}}^{0}\\)\u003c/span\u003e\u003c/span\u003e) and entropy (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{S}}^{0}\\)\u003c/span\u003e\u003c/span\u003e) were investigated to determine the thermodynamic characteristics of CIP adsorption onto the Pectin-g-poly(AA-co-IA)sorbent. The parameters related to thermodynamics were calculated using the following equations:\u003cdiv id=\"Equ8\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ8\" name=\"EquationSource\"\u003e\n$${\\text{K}}_{\\text{d}}=\\frac{{\\text{C}}_{0}-{\\text{C}}_{\\text{e}}}{{\\text{C}}_{\\text{e}}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e7\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ9\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ9\" name=\"EquationSource\"\u003e\n$$\\varDelta {\\text{G}}^{0}=-\\text{R}\\text{T}\\text{l}\\text{n}{\\text{K}}_{\\text{d}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e8\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ10\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ10\" name=\"EquationSource\"\u003e\n$$\\varDelta {\\text{G}}^{0}=\\varDelta {\\text{H}}^{0}-\\text{T}\\varDelta {\\text{S}}^{0}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e9\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ11\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ11\" name=\"EquationSource\"\u003e\n$$\\text{l}\\text{n}{\\text{K}}_{\\text{d}}=\\frac{\\varDelta {\\text{S}}^{0}}{\\text{R}}- \\frac{\\varDelta {\\text{H}}^{0}}{\\text{R}\\text{T}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e10\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eWhere\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{0}\\)\u003c/span\u003e\u003c/span\u003e and\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{C}}_{\\text{e}}\\)\u003c/span\u003e\u003c/span\u003e are the initial and equilibrium concentrations of CIP in (mg/L), R is the gas constant (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(8.314 \\text{J}/\\text{m}\\text{o}\\text{l}.\\text{K}\\)\u003c/span\u003e\u003c/span\u003e) and T is the temperature (K). \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{K}}_{\\text{d} }\\)\u003c/span\u003e\u003c/span\u003eis the equilibrium constant. Figure\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e11\u003c/span\u003e displays Van't Hoff plots of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({\\text{l}\\text{n}\\text{K}}_{\\text{d}}\\)\u003c/span\u003e\u003c/span\u003e against 1/T. The slope (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(-\\varDelta {\\text{H}}^{0}/\\text{R}\\)\u003c/span\u003e\u003c/span\u003e) and intercept (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{S}}^{0}/\\text{R}\\)\u003c/span\u003e\u003c/span\u003e) were used to calculate the \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{H}}^{0}\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{S}}^{0}\\)\u003c/span\u003e\u003c/span\u003e, respectively. Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e contains the obtained thermodynamic parameters. With an increase in temperature, the free energy change \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{G}}^{0}\\)\u003c/span\u003e\u003c/span\u003e becomes less negative, which is consistent with a decrease in removal efficiency, and CIP adsorption was a spontaneous process. While the negative \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{S}}^{0}\\)\u003c/span\u003e\u003c/span\u003evalue for adsorption indicated decreased randomness at the solid/liquid interface in the adsorption process, the negative \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\varDelta {\\text{H}}^{0}\\)\u003c/span\u003e\u003c/span\u003e value for adsorption proved that the CIP adsorption process was exothermic(Chafyq et al. 2021, Seera et al. 2021).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eThe obtained thermodynamics parameters of CIP adsorption on hydrogel at different temperatures\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eT(K)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003e∆H\u003csup\u003eo\u003c/sup\u003e (kJ/mol)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003e∆S\u003csup\u003eo\u003c/sup\u003e (J/mol.K)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003e∆G\u003csup\u003eo\u003c/sup\u003e (kJ/mol)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e288\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e\u0026ndash;18.194\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e\u0026ndash; 40.075\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e\u0026ndash; 6.610\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e298\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e\u0026ndash; 6.310\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e303\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e\u0026ndash; 6.116\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e308\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e\u0026ndash; 5.768\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e\n\u003ch3\u003eIn vitro release of CIP drug\u003c/h3\u003e\n\u003cp\u003eThe drug release profiles from hydrogels (Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e12\u003c/span\u003e) show that the CIP drug release at pH 7.4 has been demonstrated to be greater than that observed at pH 1.2, which is consistent with their swelling data. The CIP drug cumulative release ratio is 36% after 2 hours, 50% after 5 hours, 71% after 12 hours, and reaches a high of 85.15% after 30 hours at simulated intestinal fluid (pH\u0026thinsp;=\u0026thinsp;7.4).CIP is not highly soluble in neutral pH ranges. As a result, the drug release results show that the swelling amount of the drug-loaded hydrogel in media has a greater influence on drug release than CIP solubility. At pH\u0026thinsp;=\u0026thinsp;7.4, the high swelling ratio of hydrogel results in the formation of larger pore sizes within the hydrogel network, which promotes drug diffusion from larger pore sizes in hydrogel. Furthermore, at pH\u0026thinsp;=\u0026thinsp;7.4, CIP includes both anionic carboxylate and cationic amine groups, while the hydrogel just has anionic carboxylate. In truth, anionic groups on hydrogel and protonated amine on CIP drug lead to electrostatic attraction among drug and carrier, resulting in sustained CIP drug release(Sabzi et al. \u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e2020\u003c/span\u003e, Alinavaz et al. \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The results obtained demonstrated that this protecting system proved an excellent method for passing CIP into the intestine and increasing the therapeutic effectiveness of the medicine, which is sensitive to pH level in the stomach.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e\n\u003ch3\u003eEffect of temperature on CIP release\u003c/h3\u003e\n\u003cp\u003eThe release of CIP drug from hydrogel was investigated at two different temperatures (37 and 39\u0026deg;C) at pH\u0026thinsp;=\u0026thinsp;7.4. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig12\" class=\"InternalRef\"\u003e13\u003c/span\u003e, there is significant variation in CIP release rate at 37\u0026deg;C and 39\u0026deg;C. The lowest amount of drug release (71%) was recorded at 27\u0026deg;C, and the highest amount of drug release (99%) was noticed at 37\u0026deg;C. Because the ratio of swelling rises with temperature due to the adaptable nature of the hydrogel network, water rapidly penetrates the network and swells. Hence, increased the rate of drug release. Additionally, as the temperature rose, the drug molecules in the hydrogel moved faster, accelerating the rate of release(Hajikarimi and Sadeghi \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e2020\u003c/span\u003e, Thippeswamy et al. \u003cspan citationid=\"CR65\" class=\"CitationRef\"\u003e2021\u003c/span\u003e).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e"},{"header":"Conclusion","content":"\u003cp\u003eThe grafting copolymerization method was employed to develop a novel bio-adsorbent of pectin grafted poly (acrylic acid -co- itaconic acid) hydrogel for CIP drug adsorption and controlled release. In deionized water, the bio-adsorbent hydrogel shown best swelling levels at reaction conditions (MBA\u0026thinsp;=\u0026thinsp;0.05 g, pectin\u0026thinsp;=\u0026thinsp;1g, AA\u0026thinsp;=\u0026thinsp;5mL, IA\u0026thinsp;=\u0026thinsp;0.7 g, KPS\u0026thinsp;=\u0026thinsp;0.07 g) and demonstrated the highest swelling capacity of 2602% at pH\u0026thinsp;=\u0026thinsp;7.4. At optimized conditions (pH\u0026thinsp;=\u0026thinsp;6, contact time\u0026thinsp;=\u0026thinsp;120 min, temperature\u0026thinsp;=\u0026thinsp;15\u003csup\u003eo\u003c/sup\u003eC, adsorbent dosage\u0026thinsp;=\u0026thinsp;0.05g), the maximum % adsorption of CIP drug onto hydrogel (94.05%) was recorded. CIP adsorption fit better with the Freundlich isotherm (R\u003csup\u003e2\u003c/sup\u003e\u0026thinsp;=\u0026thinsp;0.9986), indicating that the adsorption process of CIP drug was multilayer. According to the thermodynamic parameters, adsorption is a spontaneous and exothermic process. The low enthalpy value associated with the adsorption suggests that the interaction among the drug and the hydrogel is physisorption in nature. According to the results of the in vitro release experiment, the cumulative release of the CIP drug after 30 hours was higher in simulated intestinal fluid (85.15%) than in simulated stomach fluid (41. 31%). Also, the influence of temperature upon drug release revealed that drug release raised with temperature. Consequently, drug loading into a hydrogel might be able to prevent the negative effects of drug on the stomach. The oral route of CIP drug loading on hydrogel can effectively extend the action time of CIP drug as well as improve its bioavailability. As a result, this hydrogel can be used in future studies as a sustained-release drugs carrier.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgements\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAuthors\u0026nbsp;would like to thanks University of Al-Qadisiyah, Iraq for providing necessary support and facilities for completion of project\u003cspan dir=\"RTL\"\u003e.\u003c/span\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll authors contributed to the design and conduct of the study. Materials preparation , experiments, data collection, analysis and written \u0026nbsp;were performed by \u0026nbsp; Wissam L Penyan\u003csup\u003e\u0026nbsp;\u003c/sup\u003eand Laith S.Jassim. all authors commented on previous versions of the manuscript. Finally, all authors read and approved the final manuscript.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding\u003c/strong\u003e No funding was received to assist with the preparation of this manuscript.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of interest\u0026nbsp;\u003c/strong\u003eThe authors have no competing interests to declare that are relevant to the content of this article.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eAjaz N, Khan IU, Khalid I, Khan RU, Khan HA, Asghar S, Khalid SH, Shahzad Y, Yousaf AM, Hussain T, Sabir N (2020) In vitro and toxicological assessment of dexamethasone sodium phosphate loaded pH sensitive Pectin-g-poly (AA)/PVP semi interpenetrating network. Mater Today Commun 25:101325\u003c/li\u003e\n\u003cli\u003eAlinavaz S, Mahdavinia GR, Jafari H, Hazrati M, Akbari A (2021) Hydroxyapatite (HA)-based hybrid bionanocomposite hydrogels: Ciprofloxacin delivery, release kinetics and antibacterial activity. 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Environ Technol 33(17):2019-2025\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Hydrogel, Swelling behavior, Ciprofloxacin drug, Adsorption, controlled release","lastPublishedDoi":"10.21203/rs.3.rs-3698789/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3698789/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn the current study, a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co-itaconic acid) hydrogel is synthesized by free radical copolymerization using acrylic acid and itaconic acid as monomers grafted on natural pectin. N, N\u0026prime;-Methylenebisacrylamide is used as a crosslinking agent, and potassium persulfate as an initiator. Various techniques, such as FTIR, SEM, XRD, and TGA, were used to characterize the synthesized bio-adsorbent hydrogel. The effect of several variables on the swelling behavior of the synthesized hydrogel was examined, like cross linker amount, pectin amount, initiator amount, and monomers amount. Furthermore, the swelling process was investigated at various pH levels. In order to establish suitable adsorption conditions, several adsorption parameters were examined, such as pH, equilibrium time, adsorbent amount, and temperature. The adsorption data were examined using the Langmuir, Freundlich, and Temkin models. The results showed that the adsorption is typically heterogeneous and of the multilayer type, as they were more consistent with the Freundlich model. The adsorption process is exothermic and spontaneous, according to thermodynamic parameters measured. In vitro drug release experiment results showed that after 30 hours, the CIP drug was released significantly higher in the simulated intestinal fluid (pH\u0026thinsp;=\u0026thinsp;7.4) than in the simulated stomach fluid (pH\u0026thinsp;=\u0026thinsp;1.2). The drug release of CIP from the hydrogel was measured at different temperatures: 30\u0026deg;Cand 40\u0026deg;C. These findings demonstrate that the hydrogel is highly efficient in ciprofloxacin adsorption and pH sensitive, making it appropriate for drug delivery in the small intestine.\u003c/p\u003e","manuscriptTitle":"Synthesis, characterization and swelling behavior of a novel bio-adsorbent based on pectin grafted poly (acrylic acid -co- itaconic acid) hydrogels for adsorption and controlled release of ciprofloxacin","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-01-03 09:11:29","doi":"10.21203/rs.3.rs-3698789/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"24a8b333-42d7-46b2-b95e-6d04ce018b30","owner":[],"postedDate":"January 3rd, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2024-04-20T07:45:59+00:00","versionOfRecord":[],"versionCreatedAt":"2024-01-03 09:11:29","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3698789","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3698789","identity":"rs-3698789","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}