Synthesis, characterization and detection of amoxicillin on 𝜷-AgVO3 modified carbon paste electrode and investigation of adsorption by DFT approach

Synthesis, characterization and detection of amoxicillin on 𝜷-AgVO3 modified carbon paste electrode and investigation of adsorption by DFT approach | 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 detection of amoxicillin on 𝜷-AgVO3 modified carbon paste electrode and investigation of adsorption by DFT approach Ayad Atika, lina HERMOUCHE, ibtissam El ABDOUNI, Elhassan Benhsina, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3985793/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 The weighty industrialization, rapid urbanization and the changing lifestyle have been considered as a worldwide threat, these human activities produce a huge pollutant element especially in water such as antibiotics, heavy metals etc.. Hence, the sensing and quantification of trace pollutants in aquatic system have been becoming a necessity tool to develop. In this work, we synthesis the silver metavanadate AgVO 3 through solid state reaction, the obtained powder was analyzed using X-ray diffraction, infrared spectroscopy and scanning electronic microscopy to check the structure and purity of the silver metavanadate. The elaborated compound as a modifier of carbon paste electrode to investigate the sensing of amoxicillin in aqueous solution by means of square wave voltammetry. The effect of electrochemical and chemical parameters on the current intensity was optimized. Under optimized conditions, the prepared electrode had a detection limit of 0.731µM. The interaction between amoxicillin molecule and AgVO 3 surface was also investigated, which shows spontaneous adsorption process. AXM sensing silver metavanadate AgVO3 adsorption process 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 Introduction Since the discovery of penicillin in 1929, the antibiotics have been widely employed to improve humans and animal’s health for example they used to treat infections in humans and to upsurge the weight of livestock in aquaculture or to prohibit damage by bacteria in plant. However, these substances have a huge effect on environment and human health after their use despite their advantages, the remains of these compounds in sewage, rivers, and other water sources. Amoxicillin (AMX) is among the most common consuming antibiotics, the mean structure of this molecule is 6-aminopenicillanic acid, which comprises of a thiazolidine ring fused to a -lactam ring with a side chain with a primary amine group inexistent in all other penicillin’s except epicillin and bacampicillin [ 1 – 4 ]. The development of new sensitive method for organic compounds is still required especially for environmental water samples, food animal products and biological fluids. While several analytical methods have been already established with high sensitivity like spectrofluorometry, enzymatic quantification, high performance liquid chromatography (HPLC), liquid chromatography coupled to tandem mass spectrometry (LC–MS-MS), UV spectrophotometry, and fluorescence sensors [ 5 – 9 ]. Nonetheless, those methods require expensive instrumentation, highly trained personnel, time-consuming for purification processes and repetitive extractions. In the literature, a limited studies were reported on sensing of AMX using modified electrode through electrochemical process, N. Hareesha et al. have been studied an effective and a selective electrochemical way to detect amoxicillin in presence of dopamine through cyclic voltammetry method, cetyltrimethylammonium bromide drop-casted carbon paste electrode was used to investigate the detection of AMX. The prepared modified sensor delivers a higher electrocatalytic nature for the oxidation of amoxicillin in phosphate buffer saline [ 10 ]. The synergy between functionalized materials was tested for AMX sensing, as shown by the work of J. Song et al., where (TiO 2 -g-C 3 N 4 ) and gold nanoparticles (Au NPs) shows high sensitivity, strong anti-interference ability, high reproducibility, and high stability, in the detection of amoxicillin in actual wastewater. The sensor achieved the detection limit of 0.2 nM [ 11 ]. Transition metal oxide was also tested as modified electrode for AMX detection as showed the work of R. Dumitru and her co-works, where CuBi 2 O 4 particles was used toward the amoxicillin sensing, the electrode was constructed from CuBi 2 O 4 /CNF paste electrode and a comparison with the CNF paste electrode. The cyclic voltametric explorations indicate a good electroanalytical performance for AMX detection [ 12 ]. The detection and quantification of AMX became important nowadays, in this context we explored the electrochemical sensing of AMX using silver metavanadate, obtained via solid state method, and characterized using, X ray diffraction, Infrared spectroscopy and MEB spectroscopy. I- Experimental section I- 1. Materials The chemicals reagents used in the present work, silver carbonate Ag 2 CO 3 (Aldrich, 99%), vanadium oxide (Merck; 99.5%), Hydrochloric acid (Fluka; 37%) sodium hydroxide NaOH (Merck ; 98%) Carbon graphite powder of the Lorraine brand (purity 99%, diameter 22 µm) were used without further purification. Amoxicillin was obtained from a local pharmacy. I- 2. Synthesis of AgVO 3 The elaboration of AgVO 3 was carried out using solid state reaction using a mixture of vanadium oxide V 2 O 5 and silver carbonate Ag 2 CO 3 . The reagents were grounded in an agate mortar and then put into a porcelain crucible. The obtained mixture was introduced into a furnace and heated in a successive stage of temperature from 300 to 450°C. I- 3. Preparation of the electrodes and solutions The stock solution (1.10 − 3 M) was prepared by dissolving amoxicillin in HCl solution (0.2 M) (pH = 0.68). This electrolyte was chosen after testing various buffer solutions. Carbon graphite powder was supplied to obtain the modified/unmodified paste. For paste compaction, analytical grade paraffin oil was used. Distilled water was used throughout the work. The modified paste carbon electrode was prepared by intimately mixing of 25% (w/w) paraffin oil with 75% (w/w) compound 𝜷-AgVO 3 /graphite powder in a mortar until obtention of a smooth homogeneous paste. The quantity of modifier was varied from 5–50% to investigate its effect on the detection of amoxicillin ions. The obtained past was packed into an insulin syringe used as a cylindrical cavity holder (5mm diameter). Electrical contact was made with copper wires. The unmodified electrode (EPC) was prepared according to the same protocol 75:25 (w/w) mass ratio of graphite and paraffin oil. Before starting a new series of experiments, the active surface of the prepared electrodes was renewed mechanically by polishing with abrasive paper (P220), smoothed on a piece of wet filter paper and rinsed with distilled water to remove contamination and to obtain a uniform fresh surface. The prepared CPE and 𝜷-AgVO 3 -CPE were stored by covering the active surface with aluminum foil. I- 4. Analytical procedure The electrochemical measurement response of the 𝜷-AgVO 3 -CPE electrode in the presence of amoxicillin ions was performed by adding 40 mL of the prepared stock solution at a fixed concentration (1.10 −3 M, pH = 0.68) into the electrochemical cell. Before each electrochemical recording, the electrode was preconcentrated in an open circuit for 30 s with stirring of the mixing solution at 250 rpm. The electrochemical behavior of amoxicillin ions on the surface of the modified electrode was studied by cyclic voltammetry (CV) recording in the range of -1.0 to 1.0V using a scan rate range of 10 to 200 mV.s − 1 . The electrocatalytic properties of the modified electrode, in terms of the detection of these ions, were established by square wave voltammetry (SWV) recording values between − 0.5 and 0.7 V for which the amplitude, frequency, potential and deposition time were 25 mV, 50 Hz, -1.0 V and 20 seconds respectively. Optimal conditions were obtained by measuring the variation in peak current intensity as a function of electrochemical and chemical parameters such as deposition potential, deposition time, electrolyte pH and mass ratio of modifier p(𝜷-AgVO 3 )/p (graphite). These conditions were applied to evaluate the performance and reliability of our modified electrode to detect amoxicillin ions at different concentrations. I.5. Molecular Dynamic Simulation (MDS) details To well understand properties on the adsorption process of AMX molecules ions on AgVO 3 substrates, the molecular dynamics simulations (MDS) was done through Materials Studio 7.0 package, utilizing Monte Carlo simulations using the COMPASS force field and considering periodic boundary conditions [ 13 – 15 ]. The crystallographic data of the studied AgVO 3 was obtained from [ 16 ], “AgVO 3 ” structure has cell parameters (a = 18.677 Å, b = 3.692 Å, c = 8.148 Å, and β = 105.04°). The simulations were accomplished on AgVO 3 periodic crystal surfaces in a simulation box with deafferents plans (110) (110) (110) (110) (Fig. 1 ) with a large vacuum region of 40 Å thickness. The adsorption (E Ads ), rigid adsorption (E Rigid ) and deformation (E Def ) energies of AMX molecule ion on AgVO 3 surface was estimated using equations. E Ads = E System -(E AgVO3/Surface +E Isolate AMX ) (3), E Rigidads = E System - (E AgVO3/Surface + E AdsAMX ) (4), E Def = E AdsAMX - E Isolate AMX (5) where, E System is the total energy of the investigated system, E AgVO3/Surface represents the energy of AgVO 3 surface, E Isolate AMX means the energies of isolate (free) AMX molecule ion. II- Result and discussion II- 1. Characterization of meta-vanadate of silver The synthesis powder of the β-AgVO 3 was characterized by X-ray diffraction, and the obtained data were refined through le Bail method. The pattern was fitted using a pseudo-Voigt function, and the linear interpolation between a set of manual points and refinable heights is set as background. The refinement was done taking into account the cell parameters taking in the reference [ 16 ]. The experimental spectrum matches well the calculated one (Fig. 2 ), and the crystallography parameters and reliability factors obtained from this refinement are displayed in Table 1 , which indicate that the powder is pure. Table 1 Crystallographic, and refinement parameters of β-AgVO 3 Crystal data Chemical formula AgVO 3 Crystal system, space group Triclinic, P 1 Temperature (K) 293 a , b , c (Å) 18.1061 (2), 3.5799 (3), 8.0349 (4) a, b, g (°) 90, 104.437 (3), 90 V (Å 3 ) 504.36 (6) Z 8 Refinement R p 0.126 R exp 0.145 R wp 0.182 c 2 1.588 The infrared spectroscopy of the elaborated vanadate is given in Fig. 3 , all the bands belong to the main vibration of vanadate. The SEM image of the prepared β-AgVO 3 compound is shown in Fig. 4 . This image shows that the synthesized sample is largely rod-shaped. In addition, irregularly shaped particles are also deposited on the surface of the rod-shaped particles. The EDX spectrum shows that the material consists only of silver, vanadate and oxygen (Fig. 5 ). This is in agreement with the XRD results. II- 2. Electrochemical study II-2. a. Cyclic voltmeter (CV) Cyclic voltammograms was recorded at a scan rate of 50 mV.s − 1 at a potential range from − 1.0 V to 1.0 V vs ECS using β-AgVO 3 -EPC (25% w/w) and EPC in the presence of 1.10 − 3 M of AMX ions dissolved in HCl (0.2 M), the obtained curve is shown in Fig. 6 . On the ECP electrode, it can be seen that the cyclic voltammogram in the presence of AMX shows no redox peaks, concluding an insignificant affinity of AMX ions towards this electrode. In contrast, the voltammogramm recorded on the β-AgVO 3 -EPC electrode illustrates a significant increase in redox peak current intensities relative to the presence of AMX ions at potentials Ep ox = 19 mV and Ep red = -34 mV, confirming that the electrode has been effectively modified by silver vanadate particles. This increase may be related to the good affinity of the β-AgVO 3 particles towards the target ions, which could be due to the surface of the modified electrode due to the large specific surface area, und the particle size of the modifier. The nature of the electrochemical system was determined by the ipa/ipc ratio which is different from 1, approving the quasi-reversibility of the system. The redox potential difference (ΔEp = Epa - Epc) was 53 mV, which is close to 59/n mV (n = 1); this confirms that the number of electrons and protons involved in the surface/solution interface is equal. b- Effect of scanning speed The effect of scan rate on the electrochemical response of the modified β-AgVO 3 -EPC electrode in the presence of AMX ions in the scan range of 10mV.s − 1 to 100 mV.s − 1 is shown in Fig. 7 (a). The linear variation of the intensity of the anodic and cathodic AMX peaks as a function of the square root of the scan rate is shown in Fig. 7 (b). The observed linearity in this scan rate range clearly indicates that the redox reaction process of AMX on the electrode surface is controlled by diffusion [ 5 ] according to the Sevick-Randles relationship [ 6 ]: I (pa, pc) = 2.69×105×n 3/2 ×A×D 1/2 × v 1/2 × [AMX] Eq. (4) The linear regression (n = 3) between the current intensity of the ox-red peaks and the square root of the scanning speed is represented (Fig. 7 b) by equations (5) and (6) with correlation coefficients equal to 0.997 and 0.986, respectively. Ipa = 0.086(v 1/2 ) + 0.1415 (R²= 0.980) Eq. (5) Ipc = -0.164 (v 1/2 ) − 0.388 (R²= 0.950) Eq. (6) On the other hand, the intensity of the AMX oxidation and reduction peaks varies proportionally with the scan rate (Fig. 7 c). This dependence suggests that the process is not only controlled by diffusion, but also by charge transfer (equations 7 and 8) [ 7 ]. Ipa = 0.005 (v) + 0.425 (R²= 0.962) Eq. (7) Ipc = − 0.010 (v) − 0.942 (R²= 0.892) Eq. (8) Where, the coverage rate (Γ) of AMX on the surface of the β-AgVO 3 -EPC electrode obtained is equal to 1.84 × 10 − 5 mol.cm − 2 calculated using Eq. 9. Ip = (n²F²A Γ)/4RT ʋ Eq. (9) Figure 7 (d) shows the linear variation of the AMX redox peak potential with the logarithm of the scan rate. Equations 10 and 11 representing this linearity are as follows: Epa (V) = 0.092 log ν + 0.0198 (R² = 0.9693) Eq. (10) Epc (V) = -0.136 log ν − 0.0850 (R² = 0.9923) Eq. (11) According to the Tafel equation, the anode and cathode potential slopes as a function of log ν are equal to -2.3RT/αnF and 2.3RT/(1-α) nF, respectively. These slopes can be used to calculate the kinetic parameters. The anodic charge transfer coefficient α is estimated to be 0.55. This value is then inserted into Eq. 12 to calculate the electronic transfer constant (ket). In our case the value of ket is 0.7 s − 1 . Log kₑt = α Log (1-α)+(1- α) Log α - Log - α (1-α)nFΔEp2.3 RT Eq. (12). c. Square wave voltammetry (SWV) study Using the SWV technic, the obtained voltammograms (Fig. 8 ) was recorded on the modified and unmodified electrodes in the presence of AMX ions. As shown in the Fig. 8 , the voltamogram associated with the EPC electrode shows no significant peak. However, an intense peak appears at a potential of 0.14 V signifying the redox of AMX. The increase in peak intensity as well as its shape can be attributed to the high conductivity of the modified β-AgVO 3 -ECP electrode. Based on these results it can be supposed that there is an improvement in the catalytic activity of the modified electrode due to the properties associated with the β-AgVO 3 modifier which causes a good interaction with the target matrix molecules. These results are consistent with those obtained with cyclic voltammetry. d. Reaction mechanism of AMX on the β-AgVO 3 electrode The process of the electrochemical reaction of the AMX molecule on the surface of the β-AgVO 3 -EPC electrode can be divided into three steps [ 8 ]: Step 1: The AMX molecule loses an electron, while the O-H hydroxyl group of the benzene ring breaks, and the protons move to the benzene ring with a rich electron cloud; Step 2: Due to the high electronegativity of the oxygen atom with a single electron, the electron clouds of the benzene ring aggregate towards the oxygen atom, favouring the formation of C = O bonds and at the same time Step 3: After rearrangement, β-C, obtaining an electron, reaches a relatively stable state, at the same time, the proton also transfers to β-C and forms a bond, forming a relatively stable conjugated structure. III. Optimization of physico-chemical parameters III.1 Effect of the pH of the electrolyte To study the effect of the variation of the pH of the electrolyte medium on the detection of the AMX molecule, an experimental study was carried out by varying the pH of the HCl electrolyte (0.2M) in the presence of 10 − 3 M of this molecule (Fig. 9 ). It was found that for pH values below 4, the current has an irrelevant intensity. This is attributed to the protonation of the amino group of the AMX molecule which gave rise to a cationic species. This protonation prevents interaction with the surface of the modified electrode resulting in relatively low current intensities. Above pH 4, a decrease in current intensity is observed, which is due to the deprotonation of the amino group as well as the phenolate group blocking the formation of a bond with the silver vanadate, resulting in a drop in the electrocatalytic properties of the modified electrode. At pH 4, the peak redox current reaches its maximum. This can be explained by the carboxylic deprotonation of AMX which facilitates the interactions with the surface of the modified electrode and makes the deposition of this molecule more fluid. For further work we chose pH = 4 as optimal. III.2 Effect of percentage by weight of modifier The effect of the particulate content of β-AgVO 3 in the carbon paste (Fig. 10 ) was evaluated in the percentage range from 2.5 to 25% (w/w). We find that the current intensity increases proportionally with the increase of the amount of the inserted modifier until the mass of the modifier is about 5% of the total mass. Then, above this value, the current intensity decreases significantly as the amount of β-AgVO 3 increases. This is due to the decrease in the conductivity of the electrode caused by the excess of these particles on the electrode surface, which decreases its efficiency [ 9 ]. For this reason, we set 5% (w/w) of β-AgVO 3 particles as the optimum percentage for preparing a modified carbon paste electrode throughout this work. IV. Calibration In order to validate our proposed method, a quantitative study for the detection of the AMX molecule on the prepared electrode at different concentrations was conducted under the optimal conditions determined in this work. This detection was established by using square wave voltammetry (SWV) to plot the I vs [AMX] calibration curves. Figure 11 clearly shows the linear relationship between peak current intensity and AMX ion concentration in two dynamic ranges which are 500 µM to 7.81 µM and 1.952 µM to 0.24 µM, according to the following linear regression equations (Eqs. 12 and 13): Ip (µA) = 1.341 [AMX] (µM) + 474.339 (R² = 0.992) (Eq. 12) Ip (µA) = 143.584 [AMX] (µM) − 13.861 (R² = 0.969) (Eq. 13) The statistical characteristics of the prepared electrode, such as the limit of detection (LOD) and limit of quantification (LOQ), were determined by LOD = 3σ/m and LOQ = 10σ/m, where σ represents the standard deviation (σ) calculated using the mathematical equation below (Eq. 14) for three successive measurements in the analytical blank. \(\varvec{\sigma }=\sqrt{\frac{1}{\mathbf{n}-1}\sum _{\mathbf{i}=0}^{\mathbf{n}}(\mathbf{I}\mathbf{i}-\mathbf{I}\mathbf{m})²}\) (Eq. 14) Where: n: the number of repetitions; Ii: the experimental value of the current intensity for each measurement; Im: the arithmetic means of the current intensities calculated at the same concentration; m: the slope of the calibration graph. From this method it can be deduced that the limit of detection (LOD) and the limit of quantification (LOQ) are in the order of 0.731 µM and 2.437 µM, respectively. Furthermore, the repeatability of the proposed method was calculated using the relative standard deviation (RSD) which equals 0.7% for n = 3. This result affirms the good accuracy and sensitivity of our electrode in terms of detection of the AMX molecule. By comparing the obtained detection limit with those of the literature (Table 2), it can be confirmed that the β-AgVO 3 -EPC electrode can be used as an effective electroanalytical method to detect and determine the AMX molecule with good accuracy even at low concentration. Tableau 2 . Comparison of the detection limit obtained on β-AgVO 3 -EPC with the literature in terms of the determination of AMX Electrode Technic LD Ref. Polyglutamic acid - graphene - EPC VC 0.118 µM [ 17 ] Polymeta-phenylenediamine - EPC SWV / VC 8.49 µM [ 18 ] Nickel-curcumin complex - EPC SWV 5 µM [ 19 ] carbon nanotube modified carbonvitreous- EPC VC 0.2µM [ 20 ] Polyglutamic acid/glutaraldehydefilm - EPC VC / SWV 0.92 µM [ 21 ] β-AgVO 3 - EPC SWV 0.731 µM This work III.5. Study of adsorption of AMX on AgVO 3 surface The adsorption of AMX molecule on the AgVO 3 surface was done to well understand the interaction between the adsorbate and adsorbent area. The adsorption was investigated on different surfaces of AgVO 3 (100), (001) and (111) to obtain the most stable adsorbent plan. Table 3 summers the adsorption energy, rigid energy and deformation energy of the adsorption of AMX onto AgVO 3 surface. Tableau 3 . Adsorption energy, rigid energy and deformation energy of the adsorption of AMX onto AgVO 3 surface Plan Adsorption E Rigid E Deformation E (100) -56.655 -7.369 -49.533 (001) -58.214 -8.434 -49.783 (111) -57.353 -8.858 -48.495 Examination of the AMX molecule onto AgVO 3 adsorption indicates that the adsorption of can be related to the contribution of the electrons of oxygen, vanadium and silver (chemical adsorption). Moreover, (100) surface is the most adsorption plan with an adsorption energy of -56.655 kcal/mol. The negative value of these energy shows the spontaneity of the adsorption process of the AMX onto the AgVO 3 surface. The deformation energy of the molecule suggests that the conformational rearrangement induced by the AMX adsorption provides both the AMX and the AgVO 3 surface less stable. This strong interaction between AMX molecule and AgVO 3 surface can clearly explain the potential sensing properties of the AMX by AgVO 3 . The previews adsorption of the AMX was also done via at al. which shows a remarkable. Conclusion The present work is devoted to the development a silver meta-vanadate modified carbon paste electrode for the AMX molecule detection in the liquid phase using cyclic voltammetry and square wave voltammetry as analytical techniques. Indeed, the optimized experimental conditions were described by determining the impact of physicochemical parameters including scan rate, pH of the electrolyte medium, and mass of the modifier percentage effect. Our study has shown that the intensity of the peak corresponding to the electroactivity of the analyzed element increases with the optimized experimental conditions up to a limit from which the peak profile changes and its intensity decreases. Furthermore, the limit of detection (LOD) and the limit of quantification (LOQ) are in the order of 0.731 µM and 2.437 µM. 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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-3985793","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":276432874,"identity":"f1d5ca2b-18e9-4bdc-9cc7-5a780c2597b0","order_by":0,"name":"Ayad Atika","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA+klEQVRIiWNgGAWjYJACCSDmkWBgPmDwgYEhgVgtBkAtbAmFM0jRAiR4DD7zEKOFf0bywxsMNX9kJNsPGG62bbPL42dvYPzwMQePDTfSjC0YjhnwSPMkJBvntiUXS/YcYJacuQ2PNTcSzIDeMOCRY0g4BtTCnLjhRgIbMy8eLfI30r9JMPwDauF/2P7bsq2esBaDGzlmEoxtQIdJJDMYM7YdJqzF8MybYgvGPmMeyRnPGAx7zh1PnNlzsBmvX+SOp2+8wfBNzl7ifP4Hgx9l1Yn97M0HP3zE532BBAbmPzAOIxuYbMCjHgj4DyDz/uBQNQpGwSgYBSMaAACm2VA1WBPQMAAAAABJRU5ErkJggg==","orcid":"","institution":"Mohammed V University of Rabat: Universite Mohammed V de Rabat","correspondingAuthor":true,"prefix":"","firstName":"Ayad","middleName":"","lastName":"Atika","suffix":""},{"id":276432875,"identity":"b7669637-7442-44a3-915a-93d68cb761f0","order_by":1,"name":"lina HERMOUCHE","email":"","orcid":"","institution":"Mohammed V University of Rabat: Universite Mohammed V de Rabat","correspondingAuthor":false,"prefix":"","firstName":"lina","middleName":"","lastName":"HERMOUCHE","suffix":""},{"id":276432876,"identity":"e5cbc908-8433-4ce2-836a-543e29f691a5","order_by":2,"name":"ibtissam El ABDOUNI","email":"","orcid":"","institution":"Hassan II University of Casablanca Faculty of Sciences Ben M'Sik: Universite Hassan II de Casablanca Faculte des Sciences Ben M'Sik","correspondingAuthor":false,"prefix":"","firstName":"ibtissam","middleName":"El","lastName":"ABDOUNI","suffix":""},{"id":276432877,"identity":"1ff3fcd4-ab78-41ab-a21b-811dd2dbd086","order_by":3,"name":"Elhassan Benhsina","email":"","orcid":"","institution":"Mohammed V University of Rabat: Universite Mohammed V de Rabat","correspondingAuthor":false,"prefix":"","firstName":"Elhassan","middleName":"","lastName":"Benhsina","suffix":""},{"id":276432878,"identity":"9cfa69db-5329-4b17-970b-64122e315ce6","order_by":4,"name":"Souad EL HAJJAJI","email":"","orcid":"","institution":"Mohammed V University of Rabat: Universite Mohammed V de Rabat","correspondingAuthor":false,"prefix":"","firstName":"Souad","middleName":"EL","lastName":"HAJJAJI","suffix":""}],"badges":[],"createdAt":"2024-02-24 18:33:33","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3985793/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3985793/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":52186744,"identity":"e2dde828-abee-4910-babf-79d4257921b2","added_by":"auto","created_at":"2024-03-07 18:32:30","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":723380,"visible":true,"origin":"","legend":"\u003cp\u003ePeriodic crystal surfaces of AgVO\u003csub\u003e3\u003c/sub\u003e in a simulation box with a plan (010) a- top view and b- side view\u003c/p\u003e","description":"","filename":"Picture1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/7f311b8ce27aaea60c17ae3f.jpg"},{"id":52186743,"identity":"5126fb23-b680-4a47-ac35-16c97fabbc8e","added_by":"auto","created_at":"2024-03-07 18:32:30","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":41092,"visible":true,"origin":"","legend":"\u003cp\u003ea) Calculated, observed X-ray diffraction patterns and their difference as well as Bragg positions of the β-AgVO\u003csub\u003e3\u003c/sub\u003e, b) Projection of the β-AgVO\u003csub\u003e3\u003c/sub\u003e structure on (a, c) plan.\u003c/p\u003e","description":"","filename":"Picture2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/c67fb09faa3f2e888fab0a5f.jpg"},{"id":52185894,"identity":"ade1119f-660e-4445-8d5a-a1d5b0d745c6","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":13613,"visible":true,"origin":"","legend":"\u003cp\u003eInfrared spectroscopy of β-AgVO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"Picture3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/f49f8c103c08c3b4532237de.jpg"},{"id":52185901,"identity":"7e289014-cac6-4e59-85a2-cbcb768c07ab","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":451764,"visible":true,"origin":"","legend":"\u003cp\u003eSEM micrographs of the prepared β-AgVO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"Picture4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/ce153e7e5114cc04d00949f6.jpg"},{"id":52185891,"identity":"e4210eff-4f78-4ca7-86e4-e4acb7fe1756","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":9697,"visible":true,"origin":"","legend":"\u003cp\u003eEDX spectrum of the prepared β-AgVO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"Picture5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/8c6f0f4e1a8a483b494b79a2.jpg"},{"id":52185892,"identity":"19e888d7-4cac-44d7-9a19-b5bb5f675e8c","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":13086,"visible":true,"origin":"","legend":"\u003cp\u003eCyclic voltammograms recorded by AgVO\u003csub\u003e3\u003c/sub\u003e–CPE and CPE.\u003c/p\u003e","description":"","filename":"Picture6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/df978e91a58d80defb319cbb.jpg"},{"id":52185895,"identity":"0aea5f6b-f6a9-4dbb-bbe7-90f0bee3e726","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":42315,"visible":true,"origin":"","legend":"\u003cp\u003ea- Cyclic voltammograms recorded at different scan rates using AgVO\u003csub\u003e3\u003c/sub\u003e/CPE electrode; b current intensity depends of the v\u003csup\u003e1/2\u003c/sup\u003e; c variation of Ip versus scan rate v (mV/s), and d variation of Epa,c versus log(v/mV s\u003csup\u003e-1\u003c/sup\u003e)\u003c/p\u003e","description":"","filename":"Picture7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/c6737ede9c9b419fa4539c4a.jpg"},{"id":52186746,"identity":"553899b4-23f6-40ce-88e7-4e6ad1914db2","added_by":"auto","created_at":"2024-03-07 18:32:30","extension":"jpg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":15229,"visible":true,"origin":"","legend":"\u003cp\u003eSWV voltammograms recorded by AgVO\u003csub\u003e3\u003c/sub\u003e–CPE and CPE\u003c/p\u003e","description":"","filename":"Picture8.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/a615f0b61dc4aa224c9d0715.jpg"},{"id":52185897,"identity":"08a25889-fdc2-4fca-8982-bc45cd853b23","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":32767,"visible":true,"origin":"","legend":"\u003cp\u003epH Effect on the response of the AgVO\u003csub\u003e3\u003c/sub\u003e–CPE modified electrode on current intensity in studied electrode.\u003c/p\u003e","description":"","filename":"Picture9.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/445e7788ecaa2707569db0f7.jpg"},{"id":52186745,"identity":"856ccfcc-96da-4b5c-91d4-f3c4ca80f0f4","added_by":"auto","created_at":"2024-03-07 18:32:30","extension":"jpg","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":22653,"visible":true,"origin":"","legend":"\u003cp\u003eeffect of the amount of modifier AgVO\u003csub\u003e3\u003c/sub\u003e on current intensity in studied electrode\u003c/p\u003e","description":"","filename":"Picture10.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/e97bf8efce5c89527d2f4800.jpg"},{"id":52185902,"identity":"395a5670-67b1-49da-9f1b-9f68a5ec4877","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":361000,"visible":true,"origin":"","legend":"\u003cp\u003eSWV voltammograms recorded at different concentrations of AMX from 500 µM to 0.24 µM under optimal conditions with the β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode.\u003c/p\u003e","description":"","filename":"Picture11.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/840607c016942bf8c8fe6e8f.jpg"},{"id":52185899,"identity":"6b8dce46-8a46-437f-872f-9a6292466f18","added_by":"auto","created_at":"2024-03-07 18:24:30","extension":"jpg","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":310453,"visible":true,"origin":"","legend":"\u003cp\u003eEquilibrium adsorption configuration of\u0026nbsp;AMX\u0026nbsp;onto the AgVO\u003csub\u003e3\u003c/sub\u003e surface: Top view.\u003c/p\u003e","description":"","filename":"Picture12.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/5bdb56d680ff78879c5c1b07.jpg"},{"id":63915193,"identity":"d554ef0a-30cd-437b-96e9-11a226d26242","added_by":"auto","created_at":"2024-09-03 17:22:50","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2660937,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3985793/v1/0d014a98-5cc8-436e-96ce-dea7515ac994.pdf"}],"financialInterests":"","formattedTitle":"Synthesis, characterization and detection of amoxicillin on 𝜷-AgVO3 modified carbon paste electrode and investigation of adsorption by DFT approach","fulltext":[{"header":"Introduction","content":"\u003cp\u003eSince the discovery of penicillin in 1929, the antibiotics have been widely employed to improve humans and animal\u0026rsquo;s health for example they used to treat infections in humans and to upsurge the weight of livestock in aquaculture or to prohibit damage by bacteria in plant. However, these substances have a huge effect on environment and human health after their use despite their advantages, the remains of these compounds in sewage, rivers, and other water sources. Amoxicillin (AMX) is among the most common consuming antibiotics, the mean structure of this molecule is 6-aminopenicillanic acid, which comprises of a thiazolidine ring fused to a -lactam ring with a side chain with a primary amine group inexistent in all other penicillin\u0026rsquo;s except epicillin and bacampicillin [\u003cspan additionalcitationids=\"CR2 CR3\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe development of new sensitive method for organic compounds is still required especially for environmental water samples, food animal products and biological fluids. While several analytical methods have been already established with high sensitivity like spectrofluorometry, enzymatic quantification, high performance liquid chromatography (HPLC), liquid chromatography coupled to tandem mass spectrometry (LC\u0026ndash;MS-MS), UV spectrophotometry, and fluorescence sensors [\u003cspan additionalcitationids=\"CR6 CR7 CR8\" citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. Nonetheless, those methods require expensive instrumentation, highly trained personnel, time-consuming for purification processes and repetitive extractions.\u003c/p\u003e \u003cp\u003eIn the literature, a limited studies were reported on sensing of AMX using modified electrode through electrochemical process, N. Hareesha et al. have been studied an effective and a selective electrochemical way to detect amoxicillin in presence of dopamine through cyclic voltammetry method, cetyltrimethylammonium bromide drop-casted carbon paste electrode was used to investigate the detection of AMX. The prepared modified sensor delivers a higher electrocatalytic nature for the oxidation of amoxicillin in phosphate buffer saline [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. The synergy between functionalized materials was tested for AMX sensing, as shown by the work of J. Song et al., where (TiO\u003csub\u003e2\u003c/sub\u003e-g-C\u003csub\u003e3\u003c/sub\u003eN\u003csub\u003e4\u003c/sub\u003e) and gold nanoparticles (Au NPs) shows high sensitivity, strong anti-interference ability, high reproducibility, and high stability, in the detection of amoxicillin in actual wastewater. The sensor achieved the detection limit of 0.2 nM [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. Transition metal oxide was also tested as modified electrode for AMX detection as showed the work of R. Dumitru and her co-works, where CuBi\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e particles was used toward the amoxicillin sensing, the electrode was constructed from CuBi\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e/CNF paste electrode and a comparison with the CNF paste electrode. The cyclic voltametric explorations indicate a good electroanalytical performance for AMX detection [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. The detection and quantification of AMX became important nowadays, in this context we explored the electrochemical sensing of AMX using silver metavanadate, obtained via solid state method, and characterized using, X ray diffraction, Infrared spectroscopy and MEB spectroscopy.\u003c/p\u003e"},{"header":"I- Experimental section","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eI- 1. Materials\u003c/h2\u003e \u003cp\u003eThe chemicals reagents used in the present work, silver carbonate Ag\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e (Aldrich, 99%), vanadium oxide (Merck; 99.5%), Hydrochloric acid (Fluka; 37%) sodium hydroxide NaOH (Merck ; 98%) Carbon graphite powder of the Lorraine brand (purity 99%, diameter 22 \u0026micro;m) were used without further purification. Amoxicillin was obtained from a local pharmacy.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003eI- 2. Synthesis of AgVO\u003csub\u003e3\u003c/sub\u003e\u003c/h2\u003e \u003cp\u003eThe elaboration of AgVO\u003csub\u003e3\u003c/sub\u003e was carried out using solid state reaction using a mixture of vanadium oxide V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e and silver carbonate Ag\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e. The reagents were grounded in an agate mortar and then put into a porcelain crucible. The obtained mixture was introduced into a furnace and heated in a successive stage of temperature from 300 to 450\u0026deg;C.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e\u003cb\u003eI- 3. Preparation of the electrodes and solutions\u003c/b\u003e\u003c/h2\u003e \u003cp\u003eThe stock solution (1.10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e M) was prepared by dissolving amoxicillin in HCl solution (0.2 M) (pH\u0026thinsp;=\u0026thinsp;0.68). This electrolyte was chosen after testing various buffer solutions. Carbon graphite powder was supplied to obtain the modified/unmodified paste. For paste compaction, analytical grade paraffin oil was used. Distilled water was used throughout the work.\u003c/p\u003e \u003cp\u003eThe modified paste carbon electrode was prepared by intimately mixing of 25% (w/w) paraffin oil with 75% (w/w) compound \u0026#120631;-AgVO\u003csub\u003e3\u003c/sub\u003e/graphite powder in a mortar until obtention of a smooth homogeneous paste. The quantity of modifier was varied from 5\u0026ndash;50% to investigate its effect on the detection of amoxicillin ions. The obtained past was packed into an insulin syringe used as a cylindrical cavity holder (5mm diameter). Electrical contact was made with copper wires. The unmodified electrode (EPC) was prepared according to the same protocol 75:25 (w/w) mass ratio of graphite and paraffin oil. Before starting a new series of experiments, the active surface of the prepared electrodes was renewed mechanically by polishing with abrasive paper (P220), smoothed on a piece of wet filter paper and rinsed with distilled water to remove contamination and to obtain a uniform fresh surface. The prepared CPE and \u0026#120631;-AgVO\u003csub\u003e3\u003c/sub\u003e-CPE were stored by covering the active surface with aluminum foil.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e\u003cb\u003eI- 4. Analytical procedure\u003c/b\u003e\u003c/h2\u003e \u003cp\u003eThe electrochemical measurement response of the \u0026#120631;-AgVO\u003csub\u003e3\u003c/sub\u003e-CPE electrode in the presence of amoxicillin ions was performed by adding 40 mL of the prepared stock solution at a fixed concentration (1.10\u003csup\u003e\u0026minus;3\u003c/sup\u003eM, pH\u0026thinsp;=\u0026thinsp;0.68) into the electrochemical cell. Before each electrochemical recording, the electrode was preconcentrated in an open circuit for 30 s with stirring of the mixing solution at 250 rpm.\u003c/p\u003e \u003cp\u003eThe electrochemical behavior of amoxicillin ions on the surface of the modified electrode was studied by cyclic voltammetry (CV) recording in the range of -1.0 to 1.0V using a scan rate range of 10 to 200 mV.s\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. The electrocatalytic properties of the modified electrode, in terms of the detection of these ions, were established by square wave voltammetry (SWV) recording values between \u0026minus;\u0026thinsp;0.5 and 0.7 V for which the amplitude, frequency, potential and deposition time were 25 mV, 50 Hz, -1.0 V and 20 seconds respectively.\u003c/p\u003e \u003cp\u003eOptimal conditions were obtained by measuring the variation in peak current intensity as a function of electrochemical and chemical parameters such as deposition potential, deposition time, electrolyte pH and mass ratio of modifier p(\u0026#120631;-AgVO\u003csub\u003e3\u003c/sub\u003e)/p (graphite). These conditions were applied to evaluate the performance and reliability of our modified electrode to detect amoxicillin ions at different concentrations.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003eI.5. Molecular Dynamic Simulation (MDS) details\u003c/h2\u003e \u003cp\u003eTo well understand properties on the adsorption process of AMX molecules ions \u003cem\u003eon\u003c/em\u003e AgVO\u003csub\u003e3\u003c/sub\u003e substrates, the molecular dynamics simulations (MDS) was done through Materials Studio 7.0 package, utilizing Monte Carlo simulations using the COMPASS force field and considering periodic boundary conditions [\u003cspan additionalcitationids=\"CR14\" citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. The crystallographic data of the studied AgVO\u003csub\u003e3\u003c/sub\u003e was obtained from [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], \u0026ldquo;AgVO\u003csub\u003e3\u003c/sub\u003e\u0026rdquo; structure has cell parameters (a\u0026thinsp;=\u0026thinsp;18.677 \u0026Aring;, b\u0026thinsp;=\u0026thinsp;3.692 \u0026Aring;, c\u0026thinsp;=\u0026thinsp;8.148 \u0026Aring;, and β\u0026thinsp;=\u0026thinsp;105.04\u0026deg;). The simulations were accomplished on AgVO\u003csub\u003e3\u003c/sub\u003e periodic crystal surfaces in a simulation box with deafferents plans (110) (110) (110) (110) (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e) with a large vacuum region of 40 \u0026Aring; thickness. The adsorption (E\u003csub\u003eAds\u003c/sub\u003e), rigid adsorption (E\u003csub\u003eRigid\u003c/sub\u003e) and deformation (E\u003csub\u003eDef\u003c/sub\u003e) energies of AMX molecule ion on AgVO\u003csub\u003e3\u003c/sub\u003e surface was estimated using equations.\u003c/p\u003e \u003cp\u003eE\u003csub\u003eAds\u003c/sub\u003e= E\u003csub\u003eSystem\u003c/sub\u003e-(E\u003csub\u003eAgVO3/Surface\u003c/sub\u003e+E\u003csub\u003eIsolate AMX\u003c/sub\u003e) (3), E\u003csub\u003eRigidads\u003c/sub\u003e= E\u003csub\u003eSystem\u003c/sub\u003e- (E\u003csub\u003eAgVO3/Surface\u003c/sub\u003e + E\u003csub\u003eAdsAMX\u003c/sub\u003e) (4), E\u003csub\u003eDef\u003c/sub\u003e = E\u003csub\u003eAdsAMX\u003c/sub\u003e - E\u003csub\u003eIsolate AMX\u003c/sub\u003e (5) where, E\u003csub\u003eSystem\u003c/sub\u003e is the total energy of the investigated system, E\u003csub\u003eAgVO3/Surface\u003c/sub\u003e represents the energy of AgVO\u003csub\u003e3\u003c/sub\u003e surface, E\u003csub\u003eIsolate AMX\u003c/sub\u003e means the energies of isolate (free) AMX molecule ion.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"II- Result and discussion","content":"\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003eII- 1. Characterization of meta-vanadate of silver\u003c/h2\u003e \u003cp\u003eThe synthesis powder of the β-AgVO\u003csub\u003e3\u003c/sub\u003e was characterized by X-ray diffraction, and the obtained data were refined through le Bail method. The pattern was fitted using a pseudo-Voigt function, and the linear interpolation between a set of manual points and refinable heights is set as background. The refinement was done taking into account the cell parameters taking in the reference [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. The experimental spectrum matches well the calculated one (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), and the crystallography parameters and reliability factors obtained from this refinement are displayed in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e, which indicate that the powder is pure.\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\u003eCrystallographic, and refinement parameters of β-AgVO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"2\"\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 \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c2\" namest=\"c1\"\u003e \u003cp\u003eCrystal data\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eChemical formula\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eAgVO\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eCrystal system, space group\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTriclinic, \u003cem\u003eP\u003c/em\u003e1\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTemperature (K)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e293\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003ea\u003c/em\u003e, \u003cem\u003eb\u003c/em\u003e, \u003cem\u003ec\u003c/em\u003e (\u0026Aring;)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e18.1061 (2), 3.5799 (3), 8.0349 (4)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ea, b, g (\u0026deg;)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e90, 104.437 (3), 90\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eV\u003c/em\u003e (\u0026Aring;\u003csup\u003e3\u003c/sup\u003e)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e504.36 (6)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eZ\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e8\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c2\" namest=\"c1\"\u003e \u003cp\u003e\u003cb\u003eRefinement\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eR\u003c/em\u003e\u003csub\u003ep\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.126\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eR\u003c/em\u003e\u003csub\u003eexp\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.145\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eR\u003c/em\u003e\u003csub\u003ewp\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.182\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ec\u003csup\u003e2\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1.588\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 infrared spectroscopy of the elaborated vanadate is given in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e, all the bands belong to the main vibration of vanadate.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe SEM image of the prepared β-AgVO\u003csub\u003e3\u003c/sub\u003e compound is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. This image shows that the synthesized sample is largely rod-shaped. In addition, irregularly shaped particles are also deposited on the surface of the rod-shaped particles. The EDX spectrum shows that the material consists only of silver, vanadate and oxygen (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e). This is in agreement with the XRD results.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003eII- 2. Electrochemical study\u003c/h2\u003e \u003cdiv id=\"Sec11\" class=\"Section3\"\u003e \u003ch2\u003eII-2. a. Cyclic voltmeter (CV)\u003c/h2\u003e \u003cp\u003eCyclic voltammograms was recorded at a scan rate of 50 mV.s\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e at a potential range from \u0026minus;\u0026thinsp;1.0 V to 1.0 V vs ECS using β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC (25% w/w) and EPC in the presence of 1.10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003eM of AMX ions dissolved in HCl (0.2 M), the obtained curve is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e. On the ECP electrode, it can be seen that the cyclic voltammogram in the presence of AMX shows no redox peaks, concluding an insignificant affinity of AMX ions towards this electrode. In contrast, the voltammogramm recorded on the β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode illustrates a significant increase in redox peak current intensities relative to the presence of AMX ions at potentials Ep\u003csub\u003eox\u003c/sub\u003e = 19 mV and Ep\u003csub\u003ered\u003c/sub\u003e = -34 mV, confirming that the electrode has been effectively modified by silver vanadate particles. This increase may be related to the good affinity of the β-AgVO\u003csub\u003e3\u003c/sub\u003e particles towards the target ions, which could be due to the surface of the modified electrode due to the large specific surface area, und the particle size of the modifier.\u003c/p\u003e \u003cp\u003eThe nature of the electrochemical system was determined by the ipa/ipc ratio which is different from 1, approving the quasi-reversibility of the system. The redox potential difference (ΔEp\u0026thinsp;=\u0026thinsp;Epa - Epc) was 53 mV, which is close to 59/n mV (n\u0026thinsp;=\u0026thinsp;1); this confirms that the number of electrons and protons involved in the surface/solution interface is equal.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003eb- Effect of scanning speed\u003c/h2\u003e \u003cp\u003eThe effect of scan rate on the electrochemical response of the modified β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode in the presence of AMX ions in the scan range of 10mV.s\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e to 100 mV.s\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e(a). The linear variation of the intensity of the anodic and cathodic AMX peaks as a function of the square root of the scan rate is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e(b). The observed linearity in this scan rate range clearly indicates that the redox reaction process of AMX on the electrode surface is controlled by diffusion [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e] according to the Sevick-Randles relationship [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]:\u003c/p\u003e \u003cp\u003eI (pa, pc)\u0026thinsp;=\u0026thinsp;2.69\u0026times;105\u0026times;n\u003csup\u003e3/2\u003c/sup\u003e\u0026times;A\u0026times;D\u003csup\u003e1/2\u003c/sup\u003e\u0026times; v\u003csup\u003e1/2\u003c/sup\u003e\u0026times; [AMX] Eq.\u0026nbsp;(4)\u003c/p\u003e \u003cp\u003eThe linear regression (n\u0026thinsp;=\u0026thinsp;3) between the current intensity of the ox-red peaks and the square root of the scanning speed is represented (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003eb) by equations (5) and (6) with correlation coefficients equal to 0.997 and 0.986, respectively.\u003c/p\u003e \u003cp\u003eIpa\u0026thinsp;=\u0026thinsp;0.086(v\u003csup\u003e1/2\u003c/sup\u003e)\u0026thinsp;+\u0026thinsp;0.1415 (R\u0026sup2;= 0.980) Eq.\u0026nbsp;(5)\u003c/p\u003e \u003cp\u003eIpc = -0.164 (v\u003csup\u003e1/2\u003c/sup\u003e) \u0026minus;\u0026thinsp;0.388 (R\u0026sup2;= 0.950) Eq.\u0026nbsp;(6)\u003c/p\u003e \u003cp\u003eOn the other hand, the intensity of the AMX oxidation and reduction peaks varies proportionally with the scan rate (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ec). This dependence suggests that the process is not only controlled by diffusion, but also by charge transfer (equations 7 and 8) [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIpa\u0026thinsp;=\u0026thinsp;0.005 (v)\u0026thinsp;+\u0026thinsp;0.425 (R\u0026sup2;= 0.962) Eq.\u0026nbsp;(7)\u003c/p\u003e \u003cp\u003eIpc\u0026thinsp;=\u0026thinsp;\u0026minus;\u0026thinsp;0.010 (v) \u0026minus;\u0026thinsp;0.942 (R\u0026sup2;= 0.892) Eq.\u0026nbsp;(8)\u003c/p\u003e \u003cp\u003eWhere, the coverage rate (Γ) of AMX on the surface of the β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode obtained is equal to 1.84 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e mol.cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e calculated using Eq.\u0026nbsp;9. Ip = (n\u0026sup2;F\u0026sup2;A Γ)/4RT ʋ Eq.\u0026nbsp;(9)\u003c/p\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e(d) shows the linear variation of the AMX redox peak potential with the logarithm of the scan rate. Equations\u0026nbsp;10 and 11 representing this linearity are as follows:\u003c/p\u003e \u003cp\u003eEpa (V)\u0026thinsp;=\u0026thinsp;0.092 log ν\u0026thinsp;+\u0026thinsp;0.0198 (R\u0026sup2; = 0.9693) Eq.\u0026nbsp;(10)\u003c/p\u003e \u003cp\u003eEpc (V) = -0.136 log ν \u0026minus;\u0026thinsp;0.0850 (R\u0026sup2; = 0.9923) Eq.\u0026nbsp;(11)\u003c/p\u003e \u003cp\u003eAccording to the Tafel equation, the anode and cathode potential slopes as a function of log ν are equal to -2.3RT/αnF and 2.3RT/(1-α) nF, respectively. These slopes can be used to calculate the kinetic parameters. The anodic charge transfer coefficient α is estimated to be 0.55. This value is then inserted into Eq.\u0026nbsp;12 to calculate the electronic transfer constant (ket). In our case the value of ket is 0.7 s\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Log kₑt\u0026thinsp;=\u0026thinsp;α Log (1-α)+(1- α) Log α - Log - α (1-α)nFΔEp2.3 RT Eq.\u0026nbsp;(12).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec13\" class=\"Section2\"\u003e \u003ch2\u003ec. Square wave voltammetry (SWV) study\u003c/h2\u003e \u003cp\u003eUsing the SWV technic, the obtained voltammograms (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e) was recorded on the modified and unmodified electrodes in the presence of AMX ions. As shown in the Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e, the voltamogram associated with the EPC electrode shows no significant peak. However, an intense peak appears at a potential of 0.14 V signifying the redox of AMX. The increase in peak intensity as well as its shape can be attributed to the high conductivity of the modified β-AgVO\u003csub\u003e3\u003c/sub\u003e-ECP electrode. Based on these results it can be supposed that there is an improvement in the catalytic activity of the modified electrode due to the properties associated with the β-AgVO\u003csub\u003e3\u003c/sub\u003e modifier which causes a good interaction with the target matrix molecules. These results are consistent with those obtained with cyclic voltammetry.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section2\"\u003e \u003ch2\u003ed. Reaction mechanism of AMX on the β-AgVO\u003csub\u003e3\u003c/sub\u003e electrode\u003c/h2\u003e \u003cp\u003eThe process of the electrochemical reaction of the AMX molecule on the surface of the β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode can be divided into three steps [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]:\u003c/p\u003e \u003cp\u003eStep 1: The AMX molecule loses an electron, while the O-H hydroxyl group of the benzene ring breaks, and the protons move to the benzene ring with a rich electron cloud;\u003c/p\u003e \u003cp\u003eStep 2: Due to the high electronegativity of the oxygen atom with a single electron, the electron clouds of the benzene ring aggregate towards the oxygen atom, favouring the formation of C\u0026thinsp;=\u0026thinsp;O bonds and at the same time\u003c/p\u003e \u003cp\u003eStep 3: After rearrangement, β-C, obtaining an electron, reaches a relatively stable state, at the same time, the proton also transfers to β-C and forms a bond, forming a relatively stable conjugated structure.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec15\" class=\"Section2\"\u003e \u003ch2\u003eIII. Optimization of physico-chemical parameters\u003c/h2\u003e \u003cdiv id=\"Sec16\" class=\"Section3\"\u003e \u003ch2\u003eIII.1 Effect of the pH of the electrolyte\u003c/h2\u003e \u003cp\u003eTo study the effect of the variation of the pH of the electrolyte medium on the detection of the AMX molecule, an experimental study was carried out by varying the pH of the HCl electrolyte (0.2M) in the presence of 10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003eM of this molecule (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e). It was found that for pH values below 4, the current has an irrelevant intensity. This is attributed to the protonation of the amino group of the AMX molecule which gave rise to a cationic species. This protonation prevents interaction with the surface of the modified electrode resulting in relatively low current intensities.\u003c/p\u003e \u003cp\u003eAbove pH 4, a decrease in current intensity is observed, which is due to the deprotonation of the amino group as well as the phenolate group blocking the formation of a bond with the silver vanadate, resulting in a drop in the electrocatalytic properties of the modified electrode.\u003c/p\u003e \u003cp\u003eAt pH 4, the peak redox current reaches its maximum. This can be explained by the carboxylic deprotonation of AMX which facilitates the interactions with the surface of the modified electrode and makes the deposition of this molecule more fluid. For further work we chose pH\u0026thinsp;=\u0026thinsp;4 as optimal.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec17\" class=\"Section2\"\u003e \u003ch2\u003eIII.2 Effect of percentage by weight of modifier\u003c/h2\u003e \u003cp\u003eThe effect of the particulate content of β-AgVO\u003csub\u003e3\u003c/sub\u003e in the carbon paste (Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e) was evaluated in the percentage range from 2.5 to 25% (w/w). We find that the current intensity increases proportionally with the increase of the amount of the inserted modifier until the mass of the modifier is about 5% of the total mass. Then, above this value, the current intensity decreases significantly as the amount of β-AgVO\u003csub\u003e3\u003c/sub\u003e increases. This is due to the decrease in the conductivity of the electrode caused by the excess of these particles on the electrode surface, which decreases its efficiency [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. For this reason, we set 5% (w/w) of β-AgVO\u003csub\u003e3\u003c/sub\u003e particles as the optimum percentage for preparing a modified carbon paste electrode throughout this work.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec18\" class=\"Section2\"\u003e \u003ch2\u003eIV. Calibration\u003c/h2\u003e \u003cp\u003eIn order to validate our proposed method, a quantitative study for the detection of the AMX molecule on the prepared electrode at different concentrations was conducted under the optimal conditions determined in this work. This detection was established by using square wave voltammetry (SWV) to plot the I vs [AMX] calibration curves. Figure\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e clearly shows the linear relationship between peak current intensity and AMX ion concentration in two dynamic ranges which are 500 \u0026micro;M to 7.81 \u0026micro;M and 1.952 \u0026micro;M to 0.24 \u0026micro;M, according to the following linear regression equations (Eqs.\u0026nbsp;12 and 13):\u003c/p\u003e \u003cp\u003eIp (\u0026micro;A)\u0026thinsp;=\u0026thinsp;1.341 [AMX] (\u0026micro;M)\u0026thinsp;+\u0026thinsp;474.339 (R\u0026sup2; = 0.992) (Eq.\u0026nbsp;12)\u003c/p\u003e \u003cp\u003eIp (\u0026micro;A)\u0026thinsp;=\u0026thinsp;143.584 [AMX] (\u0026micro;M) \u0026minus;\u0026thinsp;13.861 (R\u0026sup2; = 0.969) (Eq.\u0026nbsp;13)\u003c/p\u003e \u003cp\u003eThe statistical characteristics of the prepared electrode, such as the limit of detection (LOD) and limit of quantification (LOQ), were determined by LOD\u0026thinsp;=\u0026thinsp;3σ/m and LOQ\u0026thinsp;=\u0026thinsp;10σ/m, where σ represents the standard deviation (σ) calculated using the mathematical equation below (Eq.\u0026nbsp;14) for three successive measurements in the analytical blank.\u003c/p\u003e \u003cp\u003e \u003cspan class=\"InlineEquation\"\u003e \u003cspan class=\"mathinline\"\u003e\\(\\varvec{\\sigma }=\\sqrt{\\frac{1}{\\mathbf{n}-1}\\sum _{\\mathbf{i}=0}^{\\mathbf{n}}(\\mathbf{I}\\mathbf{i}-\\mathbf{I}\\mathbf{m})\u0026sup2;}\\)\u003c/span\u003e \u003c/span\u003e (Eq.\u0026nbsp;14)\u003c/p\u003e \u003cp\u003eWhere: n: the number of repetitions; Ii: the experimental value of the current intensity for each measurement; Im: the arithmetic means of the current intensities calculated at the same concentration; m: the slope of the calibration graph.\u003c/p\u003e \u003cp\u003eFrom this method it can be deduced that the limit of detection (LOD) and the limit of quantification (LOQ) are in the order of 0.731 \u0026micro;M and 2.437 \u0026micro;M, respectively. Furthermore, the repeatability of the proposed method was calculated using the relative standard deviation (RSD) which equals 0.7% for n\u0026thinsp;=\u0026thinsp;3. This result affirms the good accuracy and sensitivity of our electrode in terms of detection of the AMX molecule.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eBy comparing the obtained detection limit with those of the literature (Table\u0026nbsp;2), it can be confirmed that the β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC electrode can be used as an effective electroanalytical method to detect and determine the AMX molecule with good accuracy even at low concentration.\u003c/p\u003e \u003cp\u003e \u003cb\u003eTableau 2\u003c/b\u003e. Comparison of the detection limit obtained on β-AgVO\u003csub\u003e3\u003c/sub\u003e-EPC with the literature in terms of the determination of AMX\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"No\" id=\"Taba\" border=\"1\"\u003e \u003ccolgroup cols=\"4\"\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 \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eElectrode\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTechnic\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eLD\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eRef.\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePolyglutamic acid - graphene - EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eVC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.118 \u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e[\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePolymeta-phenylenediamine - EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSWV / VC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e8.49 \u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e[\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e]\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNickel-curcumin complex - EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSWV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e5 \u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e[\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ecarbon nanotube modified carbonvitreous- EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eVC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.2\u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e[\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ePolyglutamic acid/glutaraldehydefilm - EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eVC / SWV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.92 \u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e[\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eβ-AgVO\u003csub\u003e3\u003c/sub\u003e- EPC\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSWV\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.731 \u0026micro;M\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cb\u003eThis work\u003c/b\u003e\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 \u003cdiv id=\"Sec19\" class=\"Section2\"\u003e \u003ch2\u003e\u003cb\u003eIII.5. Study of adsorption of AMX on AgVO\u003c/b\u003e\u003csub\u003e\u003cb\u003e3\u003c/b\u003e\u003c/sub\u003e \u003cb\u003esurface\u003c/b\u003e\u003c/h2\u003e \u003cp\u003eThe adsorption of AMX molecule on the AgVO\u003csub\u003e3\u003c/sub\u003e surface was done to well understand the interaction between the adsorbate and adsorbent area. The adsorption was investigated on different surfaces of AgVO\u003csub\u003e3\u003c/sub\u003e (100), (001) and (111) to obtain the most stable adsorbent plan. Table\u0026nbsp;3 summers the adsorption energy, rigid energy and deformation energy of the adsorption of AMX onto AgVO\u003csub\u003e3\u003c/sub\u003e surface.\u003c/p\u003e \u003cp\u003e \u003cb\u003eTableau 3\u003c/b\u003e. Adsorption energy, rigid energy and deformation energy of the adsorption of AMX onto AgVO\u003csub\u003e3\u003c/sub\u003e surface\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"No\" id=\"Tabb\" border=\"1\"\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\u003ePlan\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eAdsorption E\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eRigid E\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eDeformation E\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e(100)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e-56.655\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e-7.369\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e-49.533\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e(001)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e-58.214\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e-8.434\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e-49.783\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e(111)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e-57.353\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e-8.858\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e-48.495\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\u003eExamination of the AMX molecule onto AgVO\u003csub\u003e3\u003c/sub\u003e adsorption indicates that the adsorption of can be related to the contribution of the electrons of oxygen, vanadium and silver (chemical adsorption). Moreover, (100) surface is the most adsorption plan with an adsorption energy of -56.655 kcal/mol. The negative value of these energy shows the spontaneity of the adsorption process of the AMX onto the AgVO\u003csub\u003e3\u003c/sub\u003e surface.\u003c/p\u003e \u003cp\u003eThe deformation energy of the molecule suggests that the conformational rearrangement induced by the AMX adsorption provides both the AMX and the AgVO\u003csub\u003e3\u003c/sub\u003e surface less stable.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThis strong interaction between AMX molecule and AgVO\u003csub\u003e3\u003c/sub\u003e surface can clearly explain the potential sensing properties of the AMX by AgVO\u003csub\u003e3\u003c/sub\u003e. The previews adsorption of the AMX was also done via at al. which shows a remarkable.\u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusion","content":"\u003cp\u003eThe present work is devoted to the development a silver meta-vanadate modified carbon paste electrode for the AMX molecule detection in the liquid phase using cyclic voltammetry and square wave voltammetry as analytical techniques. Indeed, the optimized experimental conditions were described by determining the impact of physicochemical parameters including scan rate, pH of the electrolyte medium, and mass of the modifier percentage effect. Our study has shown that the intensity of the peak corresponding to the electroactivity of the analyzed element increases with the optimized experimental conditions up to a limit from which the peak profile changes and its intensity decreases. Furthermore, the limit of detection (LOD) and the limit of quantification (LOQ) are in the order of 0.731 \u0026micro;M and 2.437 \u0026micro;M. The interaction between AMX and AgVO\u003csub\u003e3\u003c/sub\u003e surface was also investigated, the obtained result indicates the spontaneity of the adsorption process of the AMX onto the AgVO\u003csub\u003e3\u003c/sub\u003e surface.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e \u003ch2\u003eDeclaration of interest\u003c/h2\u003e \u003cp\u003eThe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eAcknowledgments :\u003c/h2\u003e \u003cp\u003eThe authors disclosed that they didn't receive financial support for the research in this article.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eLarsson DGJ (2014) Antibiotics in the environment. 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Sens Actuators B Chem 133:398\u0026ndash;403. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.snb.2008.02.045\u003c/span\u003e\u003cspan address=\"10.1016/j.snb.2008.02.045\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e\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":true,"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":"AXM sensing, silver metavanadate AgVO3, adsorption process","lastPublishedDoi":"10.21203/rs.3.rs-3985793/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3985793/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe weighty industrialization, rapid urbanization and the changing lifestyle have been considered as a worldwide threat, these human activities produce a huge pollutant element especially in water such as antibiotics, heavy metals etc.. Hence, the sensing and quantification of trace pollutants in aquatic system have been becoming a necessity tool to develop. In this work, we synthesis the silver metavanadate AgVO\u003csub\u003e3\u003c/sub\u003e through solid state reaction, the obtained powder was analyzed using X-ray diffraction, infrared spectroscopy and scanning electronic microscopy to check the structure and purity of the silver metavanadate. The elaborated compound as a modifier of carbon paste electrode to investigate the sensing of amoxicillin in aqueous solution by means of square wave voltammetry. The effect of electrochemical and chemical parameters on the current intensity was optimized. Under optimized conditions, the prepared electrode had a detection limit of 0.731\u0026micro;M. The interaction between amoxicillin molecule and AgVO\u003csub\u003e3\u003c/sub\u003e surface was also investigated, which shows spontaneous adsorption process.\u003c/p\u003e","manuscriptTitle":"Synthesis, characterization and detection of amoxicillin on 𝜷-AgVO3 modified carbon paste electrode and investigation of adsorption by DFT approach","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-03-07 18:24:25","doi":"10.21203/rs.3.rs-3985793/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":"e1afbaa2-9817-4961-ade3-22490cd8ab9a","owner":[],"postedDate":"March 7th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2024-09-03T17:14:41+00:00","versionOfRecord":[],"versionCreatedAt":"2024-03-07 18:24:25","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3985793","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3985793","identity":"rs-3985793","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}