Quantitative methodology for poly (butylene adipate-co-terephthalate) (PBAT) microplastic detection in soil and compost

Quantitative methodology for poly (butylene adipate-co-terephthalate) (PBAT) microplastic detection in soil and compost | 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 Quantitative methodology for poly (butylene adipate-co-terephthalate) (PBAT) microplastic detection in soil and compost Yvan D. Hernandez-Charpak, Harshal J. Kansara, Jeffrey S. Lodge, and 4 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-5285330/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 31 Jan, 2025 Read the published version in Environmental Science and Pollution Research → Version 1 posted 5 You are reading this latest preprint version Abstract With the increasing use of biodegradable plastics in agriculture and food packaging, it has become increasingly important to assess the effects of their fragmentation and mineralization in the environment (i.e. soil, compost). PBAT is a biodegradable polyester widely used in biodegradable mulch films that are intended to fragment and mineralize in soil. To study these effects, novel methodologies are needed to quantify PBAT microplastics in these diverse environments. This work seeks to answer whether Gas Chromatography Mass Spectrometry (GCMS) can be used as a tool to assess PBAT microplastics in soil. A method was developed that allows PBAT soil extraction by ultrasonication and GCMS quantification after a fatty acid methyl ester derivatization. To validate the method, an industrial compost degradation experiment was carried out to evidence the weight loss of PBAT film and quantify the micro- and nano-plastic generated from them. The presented method improved the existing resolution by, at least, one order of magnitude compared to reported methods. In conclusion, a novel, simple, affordable, and reproducible methodology for PBAT microplastics detection was developed improving the limits of detection and quantification. The method was tested on an industrial compost experiment, demonstrating the ability to trace the totality of the plastic over time, evidencing that PBAT is consumed in the industrial compost environment. Microplastics PBAT GCMS biodegradation soil extraction Microplastics detection Figures Figure 1 Figure 2 Figure 3 Figure 4 Introduction Growing populations and economic development require the use of agricultural mulching films (AMFs) for some crops, as they are inexpensive, easy to use, increase crop yield, diminish the use of pesticides and herbicides, and increase food quality (Espí et al., 2006 ; Gutierrez, 2019 ; Kasirajan & Ngouajio, 2012 ). The major setback is the disposal of the films at end-of-life, as it generates an additional cost to growers who must collect the films after each harvest and send it to landfills or incineration facilities, thereby increasing the environmental impact (Gutierrez, 2019 ). The conventional plastic used for AMFs is low-density polyethylene (LDPE), due to its low price and excellent mechanical performance. During end-of-life collection, small amounts of the plastic are left behind leading to microplastics (MPs) production (size < 5mm) (Jin et al., 2022 ; United Nations Environment Programme, 2022 ; Uwamungu et al., 2022 ). LDPE does not degrade under normal environmental conditions, thus leading to an accumulation of MPs, that can hinder soil health (United Nations Environment Programme, 2022 ; Yu et al., 2021 ). Poly (butylene adipate-co-terephthalate) (PBAT) is a biodegradable polymer that has attracted industry and academia’s attention due to its ductility and good processability (Bhagwat et al., 2020 ; Kyrikou & Briassoulis, 2007 ; Lawson & Taber, 2011 ; Nunes et al., 2020 ; Sintim et al., 2020 ; Tan et al., 2016 ). Additionally, due to its low glass transition temperature, it has a relatively high rate of soil degradability, making it a promising alternative to replace conventional plastics in AMF applications (Touchaleaume et al., 2016 ; Zumstein et al., 2018 ). Most biodegradable AMFs are PBAT based films that are compounded with other biodegradable resins like polylactic acid and even raw starch (Sintim et al., 2020 ; Touchaleaume et al., 2016 ). The effects of biodegradable, PBAT-based, AMFs on soil health have been described by Bandopadhyay and collaborators, as indirect (via microclimate modification) and direct (via incorporation in soil) (Bandopadhyay et al., 2018 ). The indirect effects are somewhat similar to the LDPE based films; however, the direct effects of the MPs are different. Astner and collaborators reviewed the interactions of MPs coming from the increasing AMF industry with agricultural soil ecosystems (Astner et al., 2023 ). Conventional films’ MPs accumulate with time, are ‘easily’ detectable and their lack of degradability leads to a continuous increase in their impact (Astner et al., 2023 ; He et al., 2018 ; Jin et al., 2022 ; Uwamungu et al., 2022 ; Zhang et al., 2018 ). Uwamungu and collaborators described their impacts on the different soil cycles such as bacterial, fungal and plant growth cycles (Astner et al., 2023 ; Uwamungu et al., 2022 ). PBAT based films degrade with time, leading to a stabilization of the MP concentration (Yu et al., 2021 ). Even though their impact is less than MP’s coming from conventional films, it is important to monitor and study how it affects microbial, fungi and plant cycles (Astner et al., 2023 ; Bandopadhyay et al., 2018 ). Nie and collaborators found negative impacts of 0.5% of PBAT MPs on bacterial abundance and diversities in water columns (Nie et al., 2022 ). On the other hand, Li and collaborators found that low content of PBAT MPs (0.02%) showed slight increase in diversity of landfill bacterial communities, but high contents (> 2%) would result in a decrease in bacterial diversity, concluding the existence of a certain dose-effect for different amounts of PBAT (Li et al., 2022a ). Liu and colleagues found similar results on latosol microbial diversity and dissolved organic matter, since low concentrations of PBAT (5%) showed an increase in dissolved organic matter, however, high concentration (10%) diminished the microbial diversity. Additionally, the authors reported that PBAT MPs impact on fungal richness is different than that for microbial activity (Y. Liu et al., 2023 ). The concentration of PBAT microplastics is related to its impact, and due to its biodegradability, this concentration is not constant. Astner and coauthors confirm that additional long-term studies are required (Astner et al., 2023 ), highlighting the need to assess PBAT MP concentration in and out of the laboratory setting to continue to study their effect on agricultural soils. The quantification of PBAT from different environments is a challenge. Cho and collaborators developed an effective gas chromatography coupled with mass spectrometry (GC-MS) method to quantify degraded PBAT film in wastewater (Cho, Kim, et al., 2022 ; Cho, Park, et al., 2022 ). The method dissolves the PBAT in chloroform (CHCl 3 ) and performs a fatty acid methyl ester derivatization (FAME) to break down the polymer chains allowing quantification of PBAT in CHCl 3 (Cho, Kim, et al., 2022 ). However, the limit of detection (LOD) and of quantification (LOQ) were reported to be 0.26 g/L (260 ppm) and 0.80 g/L (800 ppm) respectively, which are uncommonly high for a GCMS methodology (Wollein & Schramek, 2012 ). The potential of a methodology using FAME and GC was also detailed by Wortman and collaborators (Wortman et al., 2022 ). They reported a clear detection from soil of PBAT based plastics, however they did not assess concentration of PBAT in the soil. The lowest detected amount they reported was 0.08 mg of PBAT-based films [26]. Nelson and collaborators developed an analytical methodology to quantify microplastics from PBAT in soils (Nelson et al., 2019 ). Using proton nuclear magnetic resonance ( 1 H-NMR) they extracted PBAT in CHCl 3 and compared it with 1,4 dimethoxybenzene in deuterated-CHCl 3 (CDCl 3 ), allowing them to quantify very effectively the PBAT concentration. Their LOD and LOQ were determined to be 1.3 and 4.4 µg/ml of CDCl 3 , respectively. However, this methodology uses deuterated chloroform for the analysis, which is an expensive solvent, and their LOD and LOQ depend on the PBAT extraction from soil (Nelson et al., 2019 ). The authors explore three different extraction methods in the laboratory: Soxhlet, accelerated solvent and ultrasonication. Briefly, the accelerated solvent outperforms the others but demands a specific (and expensive) instrument; the Soxhlet extraction is usually used for non-soluble and is more expensive. Finally, ultrasonication is the most accessible method but more labor intensive, however it performs similarly to the two other methods (Nelson et al., 2019 ). In a review, Astner details the limits of NMR for PBAT quantifications due to the solvent-soil organic matter interactions leading to interferences in the spectra (Astner et al., 2023 ). This, however, should be less of a barrier using GCMS, which is a widely used methodology to find components in highly contaminated soil samples (Cho, Park, et al., 2022 ; Profumo et al., 2020 ). In the presented work we therefore detailed and tested in a real-world application, an accessible and reliable methodology that combines the ultrasonication process of the NMR methodologies(Astner et al., 2023 ; Nelson et al., 2019 ) with the FAME and GCMS analysis presented by Cho and collaborators (Cho, Kim, et al., 2022 ; Cho, Park, et al., 2022 ). Methodology Materials PBAT (EcoWorld®) was supplied by Jinhui Zhaolong High Technology Co. (Shanxi Province, P.R. China) with a melt flow index of \(\:4.8\pm\:0.4\) g/10min (190°C, 2.16kg, by ASTM D1238-A). Using this material, PBAT films for composting were manufactured in a three-layer blown film line Labtech Engineering Co. Thailand (model LF-400-COEX). The equipment utilizes three single-screw extruders feeding into a co-extrusion annular die with a 50 mm outside diameter and a gap of 0.8 mm. The extruders have a barrel diameter of 20.0 mm with an L/D = 30. For this work only one extruder was used at 15 rpm, with temperatures of 180°C; 180°C; 175°C; 170°C and 160°C from feed to the die to achieve a melting temperature of 170°C. The blow-up ratio (BUR) was maintained between 1.8 and 2.5 so the film thickness was kept under 75 µm, this led to a draw-down ratio (DDR) between 3.5 and 6. The ratio between rollers was maintained between 2 and 3 to avoid slipping. The calibration curves detailed in the following section were made with cryoground PBAT pellets as suggested by literature (Astner et al., 2019 ; Hrovat et al., 2024 ; Seghers et al., n.d.; Tewari et al., 2022 ). Briefly, pellets were pulverized in a SPEX SamplePrep 6870 Freezer/Mill® (SPEX SamplePrep, Metuchen, NJ, USA) High-Capacity Cryogenic Grinder (“cryo-mill”). The cryo-mill is a cryogenic grinder that contains one dual chamber, in which samples are continuously submerged in liquid nitrogen to maintain cryogenic temperatures. Approximately 30–35 grams of pellets were placed in the cryo-mill, and each sample underwent four cycles with a 10-min precool, a 6-min cycle time and a 3-min cooling in between cycles, with a rotation rate of 15 rpms. The particle size of the resulting powder was measured by stereo-microscope inspection to be less than 100 µm, which agrees with literature using similar methods (Astner et al., 2019 ; Hrovat et al., 2024 ; Seghers et al., n.d.; Tewari et al., 2022 ). Chemicals Two different grades of chloroform (CHCl 3 ) were used in this work, chloroform 1 (Sigma-Aldrich, C2432, 100–200 ppm amylenes as stabilizer, ≥ 99.5%), and chloroform 2 (Macron and VWR Chemicals, ACS grade). Sulfuric Acid (Barker, ACS grade), methanol (VWR, ACS grade), calcium chloride anhydrous (Sigma Aldrich, free-flowing, ACS reagent ≥ 96%) and water (EMD Corporation, HPLC grade) were also used. Sample preparation Soil Extraction To extract microplastics, an ultrasonication method was used following (Nelson et al., 2019 ; Profumo et al., 2020 ). The final protocol had the following steps: First, mix 10 grams of dried soil (24h at 105 ºC) with 30 mL of CHCl 3, sonicate (AUCMA, China, 43 kHz) for 35 minutes at 60ºC. Once finished, allow 15 minutes of cool down in the fridge to bring it to room temperature. Then, filtrate the solution through a Whatman paper filter 40 and wash with 30 mL of additional CHCl 3 . Follow with an additional filtration through a glass syringe with a Whatman filter PTFE 0.45 µm into a 100mL round bottom flask. Next, solvent was removed using rotary evaporation (60 rpm/35ºC). Finally, redissolve the remains of the flask in 2 mL of CHCL 3 . This solution can be stored in the fridge for further analysis. Fatty acid methyl ester derivatization (FAME) The initial dilutions of the FAME procedure are needed to lower the concentration to the levels of the instrument. If the samples are expected to have a concentration of ~ 1 mg/mL of CHCl 3 (1 mg/g of dry soil), these steps will dilute it to ~ 0.1 µg/mL of CHCl 3 , which is an adequate concentration for detection for the instrument. The control stock solution was made by dissolving 10.0 mg of cryo-grounded PBAT in 10.0 mL of CHCl 3 (~ 1 mg/mL of CHCl 3 or 1 mg/g of dry soil). From this stock solution, the samples for the calibration curve were made with the FAME proceeding but with different dilutions. Table 1 details the concentrations of the calibration samples, different than the second dilution (e.g. 200 µL in 1.8 mL) of the above protocol, to obtain nominal concentrations. Table 1 Calibration curves samples concentrations. Nominal concentration (ng/mL) 1 µg/mL solution (mL) Pure CHCl 3 (mL) Type of CHCl 3 50 0.1 1.9 1 and 2 100 0.2 1.8 1 and 2 150 0.3 1.7 1 and 2 200 0.4 1.6 1 and 2 250 0.5 1.5 1 and 2 500 * 1.0 1.0 2 only 750 * 1.5 0.5 2 only * Only for the second calibration curve. With each set of samples an additional control was made to determine a response factor correction so the measured response could be compared to the calibration curve. Gas Chromatography The samples were analyzed using GC-MS (Shimadzu, GCMS-QP2020nci) equipped with a fused silica capillary column (RXI-1MS, Restek, 30 m × 0.25 mm i.d. × 0.25 µm). The GC method consisted of a starting temperature in the oven of 50 ºC for 1 min, followed by a linear temperature gradient at a rate of 15ºC/min to 120ºC. The temperature was held for 2 min at 120ºC, and then increased at a rate of 10ºC/min to 300ºC, which was held for 5 min. The injector port temperature was set to 250ºC, and the injection mode was split with a ratio of 50, using helium as carrier gas with a column flow of 1.05 mL/min and a purge flow of 3.0 mL/min. The injection volume was set to 3 µL. Mass Spectroscopy To protect the detector from the multitude of volatiles and semi-volatiles present in the soil, the MS was set in selected ion monitoring mode (SIM) and turned on only during two time windows. Based on the results of Cho and collaborators, PBAT samples would only yield two peaks of interest from the GC. The first at around 8.6 min, and a second at 12.7 min [24]. Therefore, the MS detector was turned on from minutes 8 to 10 and from minutes 12.25 to 14. The ions to monitor were chosen from the spectra presented in the work of Cho and al. [24] and confirmed by a control sample from the calibration curve (see Results and Discussion section) that ran in total ion count (TIC) mode. For the adipic acid, dimethyl ester peak (RT: 8.6 min) the ions 114, 74 and 59 m/z were followed. For the terephthalic acid, dimethyl ester peak (RT: 12.6 min) the ions followed were 163, 194, 135 and 59 m/z. The MS electron impact ionization was configured at 70 eV. The GCMS analysis is depicted in Figure S1 of the Supplemental Material. Soil Extraction Experiment To assess the extraction efficiency of this methodology, samples of 0.1, 0.15, 0.2, 0.25, 1.0, 1.5, 2.0 and 2.5 µg of PBAT diluted in CHCl 3 (from a 10 mL solution of concentration 1.0 µg/mL) were each deposited in 10 grams of dry soil. The same nominal concentrations samples were made in CHCl 3 from the same stock solution. The comparison of the resulting calibration curves allows us to assess the quality of the method to quantify PBAT in soil. Industrial Compost Experiment The industrial compost was carried out over 90 days, with sampling at days 14, 23, 50, 59, 66, 73, 80 and 90. The aerated static pile (ASP) was ~ 4 meters tall and ~ 3 meters wide and structured as follows: 3.75 m of a mixture of food waste and 25 cm cover of woodchips. From the PBAT film described above, 75 mm-side squared samples were cut, in triplicates, and inserted in 1-mm holes PVC mesh bags (Saint-Gobain ADFORS) along with 100 grams of sieved soil (< 5 mm) to attempt to maximize the uniform contact between the film and the compost environment. So as not to lose the sample bags into the large pile, bags were placed in eight identical 5-gallon bins. Each bin represented one time point for sampling. The temperature of the bins and the compost are shown in Figure S2. Bins were then filled with composting material and the mesh bags placed into the bins about 2 to 3 cm apart from each other. After which the bins were placed in the center of the pile (~ 1m from the from the ground) and covered with about 2-2.5 meters of composting material. Mesh bags were carefully retrieved from the bins and stored in Ziplock bags to be transported back to the lab. Mesh bags were opened over a clean aluminum foil and the contents pulled out and dried at 60°C for 24 hours. The soil was then sieved through a size 14 mesh (1.4 mm), plastic pieces over the mesh were retrieved and weighed. The soil was kept and used with this methodology to quantify the PBAT micro- and nano- plastics attached to it. PBAT film weight loss was assessed as shown in Eq. 1 : $$\:\:W{L}_{n}\left[\%\right]=\left(1\:-\frac{{W}_{n}}{{W}_{0}}\:\right)\times\:100\left[\%\right]$$ 1 where \(\:{W}_{n}\) is the composted and cleaned sample weight and \(\:{W}_{0}\) is the initial sample weight. The standard deviation of the weight loss was propagated from the standard deviations of the weight averages, following Eq. 2 : $$\:{\sigma\:}_{W{L}_{n}}=\frac{{W}_{n}}{{W}_{0}}\:\sqrt{{\left(\frac{{\sigma\:}_{0}}{{W}_{0}}\right)}^{2}+{\left(\frac{{\sigma\:}_{n}}{{W}_{n}}\right)}^{2}-\frac{2*{\sigma\:}_{n0}}{{W}_{n}*{W}_{0}}}$$ 2 where \(\:{\sigma\:}_{i}\) is the standard deviation of the measurement \(\:i\) and \(\:{\sigma\:}_{n0}\) is the covariance of measurements 0 and \(\:n\) . Results and discussion Calibrations curves The first calibration curve was made with five samples at 50, 100, 150, 200 and 250 ng/mL of CHCl 3 concentrations, as shown in Table 1 . The compound used to quantify the co-polymer was adipic acid dimethyl ester. Figure S1 in the supplemental information, details the process of quantifying the GCMS response and the rules for consistency in the analysis, i.e. manual integration for the area response of the ionic response. The second calibration curve was made with two additional samples ( with concentrations of 500 and 750 ng/ml). Figure 1 shows the linear fits of each calibration curve. The first resulted in an equation of \(\:y=8786+250.2x\) with \(\:{R}^{2}=0.951\) and the second calibration curve was \(\:y=-4784+230.4x\) with an \(\:{R}^{2}=0.929\) . The 95% confidence interval of the slopes are \(\:\left[204.0;296.4\right]\) and \(\:[199.7;261.1]\) for the first and second calibration curves respectively. Figure 2 shows the residual analysis of the regressions. The larger values of the calibration curve are within reasonable error, even though they are close to being outliers. It is then clear that the slope is within this interval, independent of the used chloroform. Soil Extraction Experiment Figure 3 displays the results from the calibration curve from soil extraction compared to the one from chloroform. The sensitivity of the method diminishes due to the heterogeneity of the soil, because the extraction process can dissolve a wide variety of compounds than will hinder the ability to detect the adipate acid. Table 2 shows the summary of the theoretical limits of this work compared with literature. To calculate the theoretical LOD and LOQ of the presented method equations 3 and 4 were used: $$\:LOD=3.3\times\:\frac{{\sigma\:}_{m}}{m}\:$$ 3 $$\:LOQ=10\times\:\frac{{\sigma\:}_{m}}{m}\:$$ 4 where \(\:{\sigma\:}_{m}\) is the average of the standard deviations of the triplicate measurements used in the calibration curves and \(\:m\) the slope of the calibration curve. The lower R 2 can be explained by the large number of calibration levels lower than the calculated LOQ. It does, however, show the relevance of these samples, as they are mostly explained by linear regression. Table 2 Limits of detection and limits of quantification of PBAT concentration Method LOD LOQ R 2 GCMS from CHCl 3 (from the three independent calibration curves of this work) 102 ± 53 ng/ml 340 ± 178 ng/ml 0.95 ± 0.02 GCMS from CHCl 3 (Cho, Kim, et al., 2022 ; Cho, Park, et al., 2022 ) 260 µg/ml 800 µg/ml 0.996 GCMS from soil (This work) 0.44 µg/ml 1.5 µg/ml 0.75 NMR from soil (Nelson et al., 2019 ) 1.3 µg/ml 4.4 µg/ml 1.00 PBAT microplastics in industrial compost Figure 4 depicts the evolution of the total amounts of PBAT, a combination of macro and micro plastics, during the course of degradation in compost. By knowing the initial amounts of PBAT inserted in the mesh bag and the amount of soil surrounding the samples this method helps estimate the fraction of PBAT that corresponds to micro- and nano- plastics. The range of total PBAT detected moves away from the initial amount after 23 days, suggesting monomer consumption as the GCMS cannot account for the amount corresponding to total adipic acid. Even though the film was fully fragmented after 59 days, the micro and nano plastics persist 30 days after, representing close to 10% of the initial weight at the end of the experiment. It is important to understand the limitations of this methodology as well. Soil microplastics travel, migrate and interact with different actors within soil (Jin et al., 2022 ), hence this methodology should be applied in concert with a rigorous sampling methodology such as soil quartering (Ghimire, Flury, et al., 2020 ). The LOQ and LOD soil concentrations equivalent still need to be investigated. However, this method is effective in addressing the need for microplastic detection in soils of biodegradable polymers. Conclusions The use of biodegradable polyesters such as PBAT, PLA or PCL is increasing, and while evidence of their full biodegradability is available, little is known of the effects on their environment in the microplastic phase of biodegradation. It is important to analyze and understand these effects, hence it is necessary to quantify them correctly. The methodology presented here, although with a chemical pre-treatment (FAME), shows the potential for better resolution than the available methods in literature. Additionally, it is based on gas chromatography-mass spectrometry (GCMS), a widely used and available technique with low-cost solvents and chemicals. The combination of these factors makes this protocol a simple, affordable and reproduceable method for the detection of PBAT microplastic in soil and compost. Declarations Ethical Approval Not Applicable Consent to participate Not Applicable Consent to Publish Not Applicable Competing Interests The authors have no relevant financial or non-financial interests to disclose. Funding This work was supported by the Foundation for Food and Agriculture Research (FFAR) grant #CA19-SS-0000000013 and by New York Empire State Development through award #C190155. The views, results, findings, and interpretations presented in this manuscript are those of the authors and do not necessarily reflect the views or policies of New York State. Author Contributions Conceptualization: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Jeffrey S. Lodge, Nathan C. Eddingsaas, Christopher L. Lewis, Thomas A Trabold, Carlos A. Diaz; Methodology: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Nathan C. Eddingsaas, Christopher L. Lewis; Formal analysis and investigation: Yvan D. Hernandez-Charpak, Harshal J. Kansara; Writing - original draft preparation: Yvan D. Hernandez-Charpak; Writing - review and editing: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Jeffrey S. Lodge, Nathan C. Eddingsaas, Christopher L. Lewis, Thomas A Trabold, Carlos A. Diaz; Funding acquisition: Thomas A Trabold, Carlos A. Diaz; Resources: Nathan C. Eddingsaas, Thomas A Trabold, Carlos A. Diaz; Supervision: Thomas A Trabold, Carlos A. Diaz Acknowledgments The authors extend their gratitude to Robert Putney and Elias Putney of Impact Earth Rochester, for providing the opportunity to test the films at their industrial composting site. The authors also want to thank Sabit Nadhvee for his help in the initial measurement protocol development, Tom Allston for his help with the GCMS runs and Dr. Diana Rodriguez-Alberto for her time and advice on procedure and method. This work was possible through the support of the Foundation for Food and Agriculture Research (FFAR) grant #CA19-SS-0000000013 and by New York Empire State Development through award #C190155. The views, results, findings, and interpretations presented in this manuscript are those of the authors and do not necessarily reflect the views or policies of New York State. Data availability The authors declare that the data supporting the findings of this study are available within the paper. Should any raw data files be needed in another format they are available from the corresponding author upon reasonable request. References Astner AF, Gillmore AB, Yu Y, Flury M, DeBruyn JM, Schaeffer SM, Hayes DG (2023) Formation, behavior, properties and impact of micro- and nanoplastics on agricultural soil ecosystems (A Review). NanoImpact , 31 . https://doi.org/10.1016/j.impact.2023.100474 Astner AF, Hayes DG, O’Neill H, Evans BR, Pingali SV, Urban VS, Young TM (2019) Mechanical formation of micro- and nano-plastic materials for environmental studies in agricultural ecosystems. Sci Total Environ 685:1097–1106. https://doi.org/10.1016/j.scitotenv.2019.06.241 Bandopadhyay S, Martin-Closas L, Pelacho AM, DeBruyn JM (2018) Biodegradable Plastic Mulch Films: Impacts on Soil Microbial Communities and Ecosystem Functions. Front Microbiol 9(APR). https://doi.org/10.3389/fmicb.2018.00819 Bhagwat G, Gray K, Wilson SP, Muniyasamy S, Vincent SGT, Bush R, Palanisami T (2020) Benchmarking Bioplastics: A Natural Step Towards a Sustainable Future. In Journal of Polymers and the Environment (Vol. 28, Issue 12, pp. 3055–3075). Springer. https://doi.org/10.1007/s10924-020-01830-8 Cho JY, Kim SH, Cho DH, Jung HJ, Kim BC, Bhatia SK, Gurav R, Lee J, Park SH, Park K, Joo HS, Yang YH (2022) Simultaneous monitoring of each component on degradation of blended bioplastic using gas chromatography-mass spectrometry. Analytical Biochemistry , 655 . https://doi.org/10.1016/j.ab.2022.114832 Cho JY, Park SL, Kim SH, Jung HJ, Cho DH, Kim BC, Bhatia SK, Gurav R, Park SH, Park K, Yang YH (2022) Novel Poly(butylene adipate-co-terephthalate)-degrading Bacillus sp. JY35 from wastewater sludge and its broad degradation of various bioplastics. Waste Manag 144:1–10. https://doi.org/10.1016/j.wasman.2022.03.003 Espí E, Salmerón A, Fontecha A, García Y, Real AI (2006) Plastic films for agricultural applications. J Plast Film Sheeting 22(2):85–102. https://doi.org/10.1177/8756087906064220 Ghimire S, Flury M, Scheenstra EJ, Miles CA (2020) Sampling and degradation of biodegradable plastic and paper mulches in field after tillage incorporation. Science of the Total Environment , 703 . https://doi.org/10.1016/j.scitotenv.2019.135577 Ghimire S, Scheenstra E, Miles CA (2020) Soil-biodegradable mulches for growth, yield, and quality of sweet corn in a mediterranean-type climate. HortScience 55(3):317–325. https://doi.org/10.21273/HORTSCI14667-19 Gutierrez TJ (2019) In: Gutiérrez TJ (ed) Polymers for Agri-Food Applications. Springer Nature He D, Luo Y, Lu S, Liu M, Song Y, Lei L (2018) Microplastics in soils: Analytical methods, pollution characteristics and ecological risks. In TrAC - Trends in Analytical Chemistry (Vol. 109, pp. 163–172). Elsevier B.V. https://doi.org/10.1016/j.trac.2018.10.006 Hrovat B, Uurasjärvi E, Viitala M, del Pino AF, Mänttäri M, Papamatthaiakis N, Haapala A, Peiponen K-E, Roussey M, Koistinen A (2024) Preparation of synthetic micro- and nano plastics for method validation studies. Sci Total Environ 925:171821. https://doi.org/10.1016/j.scitotenv.2024.171821 Jin T, Tang J, Lyu H, Wang L, Gillmore AB, Schaeffer SM (2022) Activities of Microplastics (MPs) in Agricultural Soil: A Review of MPs Pollution from the Perspective of Agricultural Ecosystems. In Journal of Agricultural and Food Chemistry (Vol. 70, Issue 14, pp. 4182–4201). American Chemical Society. https://doi.org/10.1021/acs.jafc.1c07849 Kasirajan S, Ngouajio M (2012) Polyethylene and biodegradable mulches for agricultural applications: A review. Agron Sustain Dev 32(2):501–529. https://doi.org/10.1007/s13593-011-0068-3 Kyrikou I, Briassoulis D (2007) Biodegradation of agricultural plastic films: A critical review. J Polym Environ 15(2):125–150. https://doi.org/10.1007/s10924-007-0053-8 Lawson V, Taber HG (2011) Degradable Mulch Evaluation Li C, Cui Q, Li Y, Zhang K, Lu X, Zhang Y (2022a) Effect of LDPE and biodegradable PBAT primary microplastics on bacterial community after four months of soil incubation. J Hazard Mater 429:128353. https://doi.org/10.1016/j.jhazmat.2022.128353 Li C, Cui Q, Li Y, Zhang K, Lu X, Zhang Y (2022b) Effect of LDPE and biodegradable PBAT primary microplastics on bacterial community after four months of soil incubation. J Hazard Mater 429:128353. https://doi.org/10.1016/j.jhazmat.2022.128353 Liu L, Zou G, Zuo Q, Li C, Gu J, Kang L, Ma M, Liang K, Liu D, Du L (2022) Soil bacterial community and metabolism showed a more sensitive response to PBAT biodegradable mulch residues than that of LDPE mulch residues. Journal of Hazardous Materials , 438 . https://doi.org/10.1016/j.jhazmat.2022.129507 Liu Y, Zhang W, Chen M, Zhao X, Liu H, Ge M, Li N, Ning Z, Gao W, Fan C, Li Q (2023) Molecular insights into effects of PBAT microplastics on latosol microbial diversity and DOM chemodiversity. J Hazard Mater 450:131076. https://doi.org/10.1016/j.jhazmat.2023.131076 Muroi F, Tachibana Y, Kobayashi Y, Sakurai T, Kasuya KI (2016) Influences of poly(butylene adipate-co-terephthalate) on soil microbiota and plant growth. Polym Degrad Stab 129:338–346. https://doi.org/10.1016/j.polymdegradstab.2016.05.018 Nelson TF, Remke SC, Kohler HPE, McNeill K, Sander M (2019) Quantification of Synthetic Polyesters from Biodegradable Mulch Films in Soils. Environ Sci Technol. https://doi.org/10.1021/acs.est.9b05863 Nie Z, Wang L, Lin Y, Xiao N, Zhao J, Wan X, Hu J (2022) Effects of polylactic acid (PLA) and polybutylene adipate-co-terephthalate (PBAT) biodegradable microplastics on the abundance and diversity of denitrifying and anammox bacteria in freshwater sediment. Environ Pollut 315:120343. https://doi.org/10.1016/j.envpol.2022.120343 Nunes E, de Souza C, A. G., Rosa D (2020) dos S. Use of a chain extender as a dispersing agent of the CaCO3 into PBAT matrix. Journal of Composite Materials , 54 (10), 1373–1382. https://doi.org/10.1177/0021998319880282 Profumo A, Gorroni A, Guarnieri SA, Mellerio GG, Cucca L, Merli D (2020) GC-MS qualitative analysis of the volatile, semivolatile and volatilizable fractions of soil evidence for forensic application: A chemical fingerprinting. Talanta , 219 . https://doi.org/10.1016/j.talanta.2020.121304 Seghers J, Stefaniak EA, Spina R, La, Cella C, Mehn D, Gilliland D, Held A, Jacobsson U, Emteborg H (n.d.). Preparation of a reference material for microplastics in water-evaluation of homogeneity . https://doi.org/10.1007/s00216-021-03198-7/Published Sintim HY, Bary AI, Hayes DG, Wadsworth LC, Anunciado MB, English ME, Bandopadhyay S, Schaeffer SM, DeBruyn JM, Miles CA, Reganold JP, Flury M (2020) In situ degradation of biodegradable plastic mulch films in compost and agricultural soils. Sci Total Environ 727:138668. https://doi.org/10.1016/j.scitotenv.2020.138668 Tan Z, Yi Y, Wang H, Zhou W, Yang Y, Wang C (2016) Physical and Degradable Properties of Mulching Films Prepared from Natural Fibers and Biodegradable Polymers . https://doi.org/10.3390/app6050147 Tewari A, Almuhtaram H, McKie MJ, Andrews RC (2022) Microplastics for Use in Environmental Research. J Polym Environ 30(10):4320–4332. https://doi.org/10.1007/s10924-022-02519-w Touchaleaume F, Martin-Closas L, Angellier-Coussy H, Chevillard A, Cesar G, Gontard N, Gastaldi E (2016) Performance and environmental impact of biodegradable polymers as agricultural mulching films. Chemosphere 144:433–439. https://doi.org/10.1016/j.chemosphere.2015.09.006 United Nations Environment Programme (2022) Plastics in Agriculture - An Environmental Challenge . UNEP. https://wedocs.unep.org/bitstream/handle/20.500.11822/40403/Plastics_Agriculture.pdf Uwamungu JY, Wang Y, Shi G, Pan S, Wang Z, Wang L, Yang S (2022) Microplastic contamination in soil agro-ecosystems: A review. Environmental Advances, vol 9. Elsevier Ltd. https://doi.org/10.1016/j.envadv.2022.100273 Wollein U, Schramek N (2012) Simultaneous determination of alkyl mesilates and alkyl besilates in finished drug products by direct injection GC/MS. Eur J Pharm Sci 45(1–2):201–204. https://doi.org/10.1016/j.ejps.2011.11.008 Wortman SE, Jeske E, Samuelson MB, Drijber R (2022) A new method for detecting micro-fragments of biodegradable mulch films containing poly(butylene adipate-co-terephthalate) (PBAT) in soil. J Environ Qual 51(1):123–128. https://doi.org/10.1002/jeq2.20311 Yu Y, Griffin-LaHue DE, Miles CA, Hayes DG, Flury M (2021) Are micro- and nanoplastics from soil-biodegradable plastic mulches an environmental concern? J Hazard Mater Adv 4. https://doi.org/10.1016/j.hazadv.2021.100024 Zhang S, Yang X, Gertsen H, Peters P, Salánki T, Geissen V (2018) A simple method for the extraction and identification of light density microplastics from soil. Sci Total Environ 616–617:1056–1065. https://doi.org/10.1016/j.scitotenv.2017.10.213 Zumstein MT, Schintlmeister A, Nelson TF, Baumgartner R, Woebken D, Wagner M, Kohler HPE, McNeill K, Sander M (2018) Biodegradation of synthetic polymers in soils: Tracking carbon into CO2 and microbial biomass. Sci Adv 4(7). https://doi.org/10.1126/sciadv.aas9024 Supplementary Files SuplementalInformationv2.docx Cite Share Download PDF Status: Published Journal Publication published 31 Jan, 2025 Read the published version in Environmental Science and Pollution Research → Version 1 posted Reviewers agreed at journal 06 Nov, 2024 Reviewers invited by journal 06 Nov, 2024 Editor invited by journal 04 Nov, 2024 Editor assigned by journal 31 Oct, 2024 First submitted to journal 30 Oct, 2024 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. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. 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-5285330","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":374801524,"identity":"3564ad95-9a5c-44db-ae53-cf44356ffa32","order_by":0,"name":"Yvan D. Hernandez-Charpak","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Yvan","middleName":"D.","lastName":"Hernandez-Charpak","suffix":""},{"id":374801525,"identity":"4e36e1ff-423a-4e48-b7bc-9d6cb2f19179","order_by":1,"name":"Harshal J. Kansara","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Harshal","middleName":"J.","lastName":"Kansara","suffix":""},{"id":374801526,"identity":"03c5b641-e6fe-4e11-bacf-fa8267cf388f","order_by":2,"name":"Jeffrey S. Lodge","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Jeffrey","middleName":"S.","lastName":"Lodge","suffix":""},{"id":374801527,"identity":"782134ff-8ec2-4a16-be0d-e214684c30bb","order_by":3,"name":"Nathan C. Eddingsaas","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Nathan","middleName":"C.","lastName":"Eddingsaas","suffix":""},{"id":374801528,"identity":"762d8526-247b-48ab-a8e1-a2f29080ae46","order_by":4,"name":"Christopher L. Lewis","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Christopher","middleName":"L.","lastName":"Lewis","suffix":""},{"id":374801529,"identity":"d3a959b7-dfcf-47ec-be81-4a99cb7396e7","order_by":5,"name":"Thomas A Trabold","email":"","orcid":"","institution":"Rochester Institute of Technology","correspondingAuthor":false,"prefix":"","firstName":"Thomas","middleName":"A","lastName":"Trabold","suffix":""},{"id":374801530,"identity":"f60a8539-2452-4e62-8baf-a0f3aa84d37c","order_by":6,"name":"Carlos A Diaz","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAq0lEQVRIiWNgGAWjYFCCBBBhw8AGoniI15KQxsDGRqKWwwwMRGvhb09+uuHjj/P5fPINjA/ethGhReLMM7ObMxJuW7axMTAbziVGi4FEgtltnoTbBkC/sEnzEqcl/dvtPwnnQFrYfxOpJcfsNkPCAbAtzERpkTjzpuxmT1oyUEtis+Scc0Ro4W9P33bjh42dgXzz4YMf3pQRoQUJMDaQpn4UjIJRMApGAW4AAECCMWWa0xGjAAAAAElFTkSuQmCC","orcid":"https://orcid.org/0000-0003-1763-2146","institution":"Rochester Institute of Technology","correspondingAuthor":true,"prefix":"","firstName":"Carlos","middleName":"A","lastName":"Diaz","suffix":""}],"badges":[],"createdAt":"2024-10-17 22:33:37","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-5285330/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-5285330/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s11356-025-35978-4","type":"published","date":"2025-01-31T15:57:42+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":69567422,"identity":"1845246e-7b37-414f-b999-123537c5f728","added_by":"auto","created_at":"2024-11-21 17:58:54","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":26436,"visible":true,"origin":"","legend":"\u003cp\u003eCalibration curves relating GCMS response with adipic acid dimethyl ester concentration in CHCl\u003csub\u003e3.\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"Picture1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/bb22041204c335922490c7a8.jpg"},{"id":69567419,"identity":"3d60c285-0ea7-4754-a59d-139f68a079a7","added_by":"auto","created_at":"2024-11-21 17:58:54","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":45670,"visible":true,"origin":"","legend":"\u003cp\u003eResidual analysis of the linear regressions, evidencing the absence of outliers and normality of the standardized residuals.\u003c/p\u003e","description":"","filename":"Picture2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/614815c0289bad5a1dd3748a.jpg"},{"id":69567662,"identity":"759b78be-4dd5-4827-830c-30f50efa192e","added_by":"auto","created_at":"2024-11-21 18:06:54","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":141111,"visible":true,"origin":"","legend":"\u003cp\u003eSoil extraction experiment result. Detection of adipic acid dimethyl ester from chloroform versus soil. The detection and quantification limits from soil are shown to be about 5 times less sensitive than from chloroform.\u003c/p\u003e","description":"","filename":"Picture3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/69412d7b5606e7479cf8e023.jpg"},{"id":69567420,"identity":"ce154195-8495-456a-97fb-6272f0133548","added_by":"auto","created_at":"2024-11-21 17:58:54","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":30670,"visible":true,"origin":"","legend":"\u003cp\u003eFull PBAT mass loss obtained by combining the data from the film weight loss and the microplastic concentration detected with GCMS in the surrounding soil of the mesh bag.\u003c/p\u003e","description":"","filename":"Picture4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/180c05ab74fdab843f842b16.jpg"},{"id":75351500,"identity":"cb930153-08cf-431e-bb91-1c37264f9500","added_by":"auto","created_at":"2025-02-03 16:12:03","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":960869,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/48c35248-106f-41de-85a0-301f9ba00d65.pdf"},{"id":69567421,"identity":"2c549155-269e-4ae6-9713-21b3b1ccda97","added_by":"auto","created_at":"2024-11-21 17:58:54","extension":"docx","order_by":5,"title":"","display":"","copyAsset":false,"role":"supplement","size":2350025,"visible":true,"origin":"","legend":"","description":"","filename":"SuplementalInformationv2.docx","url":"https://assets-eu.researchsquare.com/files/rs-5285330/v1/d1e72e2549c82e6fbce0fb44.docx"}],"financialInterests":"","formattedTitle":"Quantitative methodology for poly (butylene adipate-co-terephthalate) (PBAT) microplastic detection in soil and compost","fulltext":[{"header":"Introduction","content":"\u003cp\u003eGrowing populations and economic development require the use of agricultural mulching films (AMFs) for some crops, as they are inexpensive, easy to use, increase crop yield, diminish the use of pesticides and herbicides, and increase food quality (Esp\u0026iacute; et al., \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e2006\u003c/span\u003e; Gutierrez, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Kasirajan \u0026amp; Ngouajio, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2012\u003c/span\u003e). The major setback is the disposal of the films at end-of-life, as it generates an additional cost to growers who must collect the films after each harvest and send it to landfills or incineration facilities, thereby increasing the environmental impact (Gutierrez, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). The conventional plastic used for AMFs is low-density polyethylene (LDPE), due to its low price and excellent mechanical performance. During end-of-life collection, small amounts of the plastic are left behind leading to microplastics (MPs) production (size\u0026thinsp;\u0026lt;\u0026thinsp;5mm) (Jin et al., \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; United Nations Environment Programme, \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Uwamungu et al., \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). LDPE does not degrade under normal environmental conditions, thus leading to an accumulation of MPs, that can hinder soil health (United Nations Environment Programme, \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Yu et al., \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Poly (butylene adipate-co-terephthalate) (PBAT) is a biodegradable polymer that has attracted industry and academia\u0026rsquo;s attention due to its ductility and good processability (Bhagwat et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2020\u003c/span\u003e; Kyrikou \u0026amp; Briassoulis, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2007\u003c/span\u003e; Lawson \u0026amp; Taber, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Nunes et al., \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2020\u003c/span\u003e; Sintim et al., \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2020\u003c/span\u003e; Tan et al., \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). Additionally, due to its low glass transition temperature, it has a relatively high rate of soil degradability, making it a promising alternative to replace conventional plastics in AMF applications (Touchaleaume et al., \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Zumstein et al., \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Most biodegradable AMFs are PBAT based films that are compounded with other biodegradable resins like polylactic acid and even raw starch (Sintim et al., \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2020\u003c/span\u003e; Touchaleaume et al., \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2016\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe effects of biodegradable, PBAT-based, AMFs on soil health have been described by Bandopadhyay and collaborators, as indirect (via microclimate modification) and direct (via incorporation in soil) (Bandopadhyay et al., \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). The indirect effects are somewhat similar to the LDPE based films; however, the direct effects of the MPs are different. Astner and collaborators reviewed the interactions of MPs coming from the increasing AMF industry with agricultural soil ecosystems (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). Conventional films\u0026rsquo; MPs accumulate with time, are \u0026lsquo;easily\u0026rsquo; detectable and their lack of degradability leads to a continuous increase in their impact (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; He et al., \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Jin et al., \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Uwamungu et al., \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Zhang et al., \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Uwamungu and collaborators described their impacts on the different soil cycles such as bacterial, fungal and plant growth cycles (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Uwamungu et al., \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). PBAT based films degrade with time, leading to a stabilization of the MP concentration (Yu et al., \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Even though their impact is less than MP\u0026rsquo;s coming from conventional films, it is important to monitor and study how it affects microbial, fungi and plant cycles (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Bandopadhyay et al., \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Nie and collaborators found negative impacts of 0.5% of PBAT MPs on bacterial abundance and diversities in water columns (Nie et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). On the other hand, Li and collaborators found that low content of PBAT MPs (0.02%) showed slight increase in diversity of landfill bacterial communities, but high contents (\u0026gt;\u0026thinsp;2%) would result in a decrease in bacterial diversity, concluding the existence of a certain dose-effect for different amounts of PBAT (Li et al., \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2022a\u003c/span\u003e). Liu and colleagues found similar results on latosol microbial diversity and dissolved organic matter, since low concentrations of PBAT (5%) showed an increase in dissolved organic matter, however, high concentration (10%) diminished the microbial diversity. Additionally, the authors reported that PBAT MPs impact on fungal richness is different than that for microbial activity (Y. Liu et al., \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). The concentration of PBAT microplastics is related to its impact, and due to its biodegradability, this concentration is not constant. Astner and coauthors confirm that additional long-term studies are required (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e), highlighting the need to assess PBAT MP concentration in and out of the laboratory setting to continue to study their effect on agricultural soils.\u003c/p\u003e \u003cp\u003eThe quantification of PBAT from different environments is a challenge. Cho and collaborators developed an effective gas chromatography coupled with mass spectrometry (GC-MS) method to quantify degraded PBAT film in wastewater (Cho, Kim, et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Cho, Park, et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). The method dissolves the PBAT in chloroform (CHCl\u003csub\u003e3\u003c/sub\u003e) and performs a fatty acid methyl ester derivatization (FAME) to break down the polymer chains allowing quantification of PBAT in CHCl\u003csub\u003e3\u003c/sub\u003e (Cho, Kim, et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). However, the limit of detection (LOD) and of quantification (LOQ) were reported to be 0.26 g/L (260 ppm) and 0.80 g/L (800 ppm) respectively, which are uncommonly high for a GCMS methodology (Wollein \u0026amp; Schramek, \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2012\u003c/span\u003e). The potential of a methodology using FAME and GC was also detailed by Wortman and collaborators (Wortman et al., \u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). They reported a clear detection from soil of PBAT based plastics, however they did not assess concentration of PBAT in the soil. The lowest detected amount they reported was 0.08 mg of PBAT-based films [26]. Nelson and collaborators developed an analytical methodology to quantify microplastics from PBAT in soils (Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). Using proton nuclear magnetic resonance (\u003csup\u003e1\u003c/sup\u003eH-NMR) they extracted PBAT in CHCl\u003csub\u003e3\u003c/sub\u003e and compared it with 1,4 dimethoxybenzene in deuterated-CHCl\u003csub\u003e3\u003c/sub\u003e (CDCl\u003csub\u003e3\u003c/sub\u003e), allowing them to quantify very effectively the PBAT concentration. Their LOD and LOQ were determined to be 1.3 and 4.4 \u0026micro;g/ml of CDCl\u003csub\u003e3\u003c/sub\u003e, respectively. However, this methodology uses deuterated chloroform for the analysis, which is an expensive solvent, and their LOD and LOQ depend on the PBAT extraction from soil (Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). The authors explore three different extraction methods in the laboratory: Soxhlet, accelerated solvent and ultrasonication. Briefly, the accelerated solvent outperforms the others but demands a specific (and expensive) instrument; the Soxhlet extraction is usually used for non-soluble and is more expensive. Finally, ultrasonication is the most accessible method but more labor intensive, however it performs similarly to the two other methods (Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). In a review, Astner details the limits of NMR for PBAT quantifications due to the solvent-soil organic matter interactions leading to interferences in the spectra (Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). This, however, should be less of a barrier using GCMS, which is a widely used methodology to find components in highly contaminated soil samples (Cho, Park, et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Profumo et al., \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). In the presented work we therefore detailed and tested in a real-world application, an accessible and reliable methodology that combines the ultrasonication process of the NMR methodologies(Astner et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e) with the FAME and GCMS analysis presented by Cho and collaborators (Cho, Kim, et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Cho, Park, et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).\u003c/p\u003e"},{"header":"Methodology","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eMaterials\u003c/h2\u003e \u003cp\u003ePBAT (EcoWorld\u0026reg;) was supplied by Jinhui Zhaolong High Technology Co. (Shanxi Province, P.R. China) with a melt flow index of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:4.8\\pm\\:0.4\\)\u003c/span\u003e\u003c/span\u003e g/10min (190\u0026deg;C, 2.16kg, by ASTM D1238-A). Using this material, PBAT films for composting were manufactured in a three-layer blown film line Labtech Engineering Co. Thailand (model LF-400-COEX). The equipment utilizes three single-screw extruders feeding into a co-extrusion annular die with a 50 mm outside diameter and a gap of 0.8 mm. The extruders have a barrel diameter of 20.0 mm with an L/D\u0026thinsp;=\u0026thinsp;30. For this work only one extruder was used at 15 rpm, with temperatures of 180\u0026deg;C; 180\u0026deg;C; 175\u0026deg;C; 170\u0026deg;C and 160\u0026deg;C from feed to the die to achieve a melting temperature of 170\u0026deg;C. The blow-up ratio (BUR) was maintained between 1.8 and 2.5 so the film thickness was kept under 75 \u0026micro;m, this led to a draw-down ratio (DDR) between 3.5 and 6. The ratio between rollers was maintained between 2 and 3 to avoid slipping.\u003c/p\u003e \u003cp\u003eThe calibration curves detailed in the following section were made with cryoground PBAT pellets as suggested by literature (Astner et al., \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Hrovat et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2024\u003c/span\u003e; Seghers et al., n.d.; Tewari et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). Briefly, pellets were pulverized in a SPEX SamplePrep 6870 Freezer/Mill\u0026reg; (SPEX SamplePrep, Metuchen, NJ, USA) High-Capacity Cryogenic Grinder (\u0026ldquo;cryo-mill\u0026rdquo;). The cryo-mill is a cryogenic grinder that contains one dual chamber, in which samples are continuously submerged in liquid nitrogen to maintain cryogenic temperatures. Approximately 30\u0026ndash;35 grams of pellets were placed in the cryo-mill, and each sample underwent four cycles with a 10-min precool, a 6-min cycle time and a 3-min cooling in between cycles, with a rotation rate of 15 rpms. The particle size of the resulting powder was measured by stereo-microscope inspection to be less than 100 \u0026micro;m, which agrees with literature using similar methods (Astner et al., \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Hrovat et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2024\u003c/span\u003e; Seghers et al., n.d.; Tewari et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2022\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eChemicals\u003c/h3\u003e\n\u003cp\u003eTwo different grades of chloroform (CHCl\u003csub\u003e3\u003c/sub\u003e) were used in this work, chloroform 1 (Sigma-Aldrich, C2432, 100\u0026ndash;200 ppm amylenes as stabilizer, \u0026ge;\u0026thinsp;99.5%), and chloroform 2 (Macron and VWR Chemicals, ACS grade). Sulfuric Acid (Barker, ACS grade), methanol (VWR, ACS grade), calcium chloride anhydrous (Sigma Aldrich, free-flowing, ACS reagent\u0026thinsp;\u0026ge;\u0026thinsp;96%) and water (EMD Corporation, HPLC grade) were also used.\u003c/p\u003e\n\u003ch3\u003eSample preparation\u003c/h3\u003e\n\u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003eSoil Extraction\u003c/h2\u003e \u003cp\u003eTo extract microplastics, an ultrasonication method was used following (Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Profumo et al., \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The final protocol had the following steps: First, mix 10 grams of dried soil (24h at 105 \u0026ordm;C) with 30 mL of CHCl\u003csub\u003e3,\u003c/sub\u003e sonicate (AUCMA, China, 43 kHz) for 35 minutes at 60\u0026ordm;C. Once finished, allow 15 minutes of cool down in the fridge to bring it to room temperature. Then, filtrate the solution through a Whatman paper filter 40 and wash with 30 mL of additional CHCl\u003csub\u003e3\u003c/sub\u003e. Follow with an additional filtration through a glass syringe with a Whatman filter PTFE 0.45 \u0026micro;m into a 100mL round bottom flask. Next, solvent was removed using rotary evaporation (60 rpm/35\u0026ordm;C). Finally, redissolve the remains of the flask in 2 mL of CHCL\u003csub\u003e3\u003c/sub\u003e. This solution can be stored in the fridge for further analysis.\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eFatty acid methyl ester derivatization (FAME)\u003c/h3\u003e\n\u003cp\u003e \u003c/p\u003e \u003cp\u003eThe initial dilutions of the FAME procedure are needed to lower the concentration to the levels of the instrument. If the samples are expected to have a concentration of ~\u0026thinsp;1 mg/mL of CHCl\u003csub\u003e3\u003c/sub\u003e (1 mg/g of dry soil), these steps will dilute it to ~\u0026thinsp;0.1 \u0026micro;g/mL of CHCl\u003csub\u003e3\u003c/sub\u003e, which is an adequate concentration for detection for the instrument. The control stock solution was made by dissolving 10.0 mg of cryo-grounded PBAT in 10.0 mL of CHCl\u003csub\u003e3\u003c/sub\u003e (~\u0026thinsp;1 mg/mL of CHCl\u003csub\u003e3\u003c/sub\u003e or 1 mg/g of dry soil). From this stock solution, the samples for the calibration curve were made with the FAME proceeding but with different dilutions. Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e details the concentrations of the calibration samples, different than the second dilution (e.g. 200 \u0026micro;L in 1.8 mL) of the above protocol, to obtain nominal concentrations.\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\u003eCalibration curves samples concentrations.\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=\"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\u003eNominal concentration (ng/mL)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1 \u0026micro;g/mL solution (mL)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003ePure CHCl\u003csub\u003e3\u003c/sub\u003e (mL)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eType of CHCl\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e50\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.9\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1 and 2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1 and 2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e150\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.7\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1 and 2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e200\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.4\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1 and 2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e250\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1 and 2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e500\u003csup\u003e*\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1.0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e2 only\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e750\u003csup\u003e*\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e2 only\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colspan=\"4\" nameend=\"c4\" namest=\"c1\"\u003e \u003cp\u003e\u003csup\u003e*\u003c/sup\u003eOnly for the second calibration curve.\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\u003eWith each set of samples an additional control was made to determine a response factor correction so the measured response could be compared to the calibration curve.\u003c/p\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eGas Chromatography\u003c/h2\u003e \u003cp\u003eThe samples were analyzed using GC-MS (Shimadzu, GCMS-QP2020nci) equipped with a fused silica capillary column (RXI-1MS, Restek, 30 m \u0026times; 0.25 mm i.d. \u0026times; 0.25 \u0026micro;m). The GC method consisted of a starting temperature in the oven of 50 \u0026ordm;C for 1 min, followed by a linear temperature gradient at a rate of 15\u0026ordm;C/min to 120\u0026ordm;C. The temperature was held for 2 min at 120\u0026ordm;C, and then increased at a rate of 10\u0026ordm;C/min to 300\u0026ordm;C, which was held for 5 min. The injector port temperature was set to 250\u0026ordm;C, and the injection mode was split with a ratio of 50, using helium as carrier gas with a column flow of 1.05 mL/min and a purge flow of 3.0 mL/min. The injection volume was set to 3 \u0026micro;L.\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eMass Spectroscopy\u003c/h3\u003e\n\u003cp\u003eTo protect the detector from the multitude of volatiles and semi-volatiles present in the soil, the MS was set in selected ion monitoring mode (SIM) and turned on only during two time windows. Based on the results of Cho and collaborators, PBAT samples would only yield two peaks of interest from the GC. The first at around 8.6 min, and a second at 12.7 min [24]. Therefore, the MS detector was turned on from minutes 8 to 10 and from minutes 12.25 to 14. The ions to monitor were chosen from the spectra presented in the work of Cho and al. [24] and confirmed by a control sample from the calibration curve (see \u003cspan refid=\"Sec12\" class=\"InternalRef\"\u003eResults and Discussion\u003c/span\u003e section) that ran in total ion count (TIC) mode. For the adipic acid, dimethyl ester peak (RT: 8.6 min) the ions 114, 74 and 59 m/z were followed. For the terephthalic acid, dimethyl ester peak (RT: 12.6 min) the ions followed were 163, 194, 135 and 59 m/z. The MS electron impact ionization was configured at 70 eV. The GCMS analysis is depicted in Figure \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e of the Supplemental Material.\u003c/p\u003e\n\u003ch3\u003eSoil Extraction Experiment\u003c/h3\u003e\n\u003cp\u003eTo assess the extraction efficiency of this methodology, samples of 0.1, 0.15, 0.2, 0.25, 1.0, 1.5, 2.0 and 2.5 \u0026micro;g of PBAT diluted in CHCl\u003csub\u003e3\u003c/sub\u003e (from a 10 mL solution of concentration 1.0 \u0026micro;g/mL) were each deposited in 10 grams of dry soil. The same nominal concentrations samples were made in CHCl\u003csub\u003e3\u003c/sub\u003e from the same stock solution. The comparison of the resulting calibration curves allows us to assess the quality of the method to quantify PBAT in soil.\u003c/p\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003eIndustrial Compost Experiment\u003c/h2\u003e \u003cp\u003eThe industrial compost was carried out over 90 days, with sampling at days 14, 23, 50, 59, 66, 73, 80 and 90. The aerated static pile (ASP) was ~\u0026thinsp;4 meters tall and ~\u0026thinsp;3 meters wide and structured as follows: 3.75 m of a mixture of food waste and 25 cm cover of woodchips. From the PBAT film described above, 75 mm-side squared samples were cut, in triplicates, and inserted in 1-mm holes PVC mesh bags (Saint-Gobain ADFORS) along with 100 grams of sieved soil (\u0026lt;\u0026thinsp;5 mm) to attempt to maximize the uniform contact between the film and the compost environment.\u003c/p\u003e \u003cp\u003eSo as not to lose the sample bags into the large pile, bags were placed in eight identical 5-gallon bins. Each bin represented one time point for sampling. The temperature of the bins and the compost are shown in Figure S2. Bins were then filled with composting material and the mesh bags placed into the bins about 2 to 3 cm apart from each other. After which the bins were placed in the center of the pile (~\u0026thinsp;1m from the from the ground) and covered with about 2-2.5 meters of composting material. Mesh bags were carefully retrieved from the bins and stored in Ziplock bags to be transported back to the lab. Mesh bags were opened over a clean aluminum foil and the contents pulled out and dried at 60\u0026deg;C for 24 hours. The soil was then sieved through a size 14 mesh (1.4 mm), plastic pieces over the mesh were retrieved and weighed. The soil was kept and used with this methodology to quantify the PBAT micro- and nano- plastics attached to it.\u003c/p\u003e \u003cp\u003ePBAT film weight loss was assessed as shown in Eq.\u0026nbsp;\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e:\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$\\:\\:W{L}_{n}\\left[\\%\\right]=\\left(1\\:-\\frac{{W}_{n}}{{W}_{0}}\\:\\right)\\times\\:100\\left[\\%\\right]$$\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\\(\\:{W}_{n}\\)\u003c/span\u003e\u003c/span\u003e is the composted and cleaned sample weight and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{W}_{0}\\)\u003c/span\u003e\u003c/span\u003e is the initial sample weight. The standard deviation of the weight loss was propagated from the standard deviations of the weight averages, following Eq.\u0026nbsp;\u003cspan refid=\"Equ2\" class=\"InternalRef\"\u003e2\u003c/span\u003e:\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$$\\:{\\sigma\\:}_{W{L}_{n}}=\\frac{{W}_{n}}{{W}_{0}}\\:\\sqrt{{\\left(\\frac{{\\sigma\\:}_{0}}{{W}_{0}}\\right)}^{2}+{\\left(\\frac{{\\sigma\\:}_{n}}{{W}_{n}}\\right)}^{2}-\\frac{2*{\\sigma\\:}_{n0}}{{W}_{n}*{W}_{0}}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{\\sigma\\:}_{i}\\)\u003c/span\u003e\u003c/span\u003e is the standard deviation of the measurement \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:i\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{\\sigma\\:}_{n0}\\)\u003c/span\u003e\u003c/span\u003e is the covariance of measurements 0 and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:n\\)\u003c/span\u003e\u003c/span\u003e.\u003c/p\u003e \u003c/div\u003e"},{"header":"Results and discussion","content":"\u003cdiv id=\"Sec13\" class=\"Section2\"\u003e \u003ch2\u003eCalibrations curves\u003c/h2\u003e \u003cp\u003eThe first calibration curve was made with five samples at 50, 100, 150, 200 and 250 ng/mL of CHCl\u003csub\u003e3\u003c/sub\u003e concentrations, as shown in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The compound used to quantify the co-polymer was adipic acid dimethyl ester. Figure \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e in the supplemental information, details the process of quantifying the GCMS response and the rules for consistency in the analysis, i.e. manual integration for the area response of the ionic response. The second calibration curve was made with two additional samples ( with concentrations of 500 and 750 ng/ml). Figure\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e shows the linear fits of each calibration curve. The first resulted in an equation of \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:y=8786+250.2x\\)\u003c/span\u003e\u003c/span\u003e with \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{R}^{2}=0.951\\)\u003c/span\u003e\u003c/span\u003e and the second calibration curve was \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:y=-4784+230.4x\\)\u003c/span\u003e\u003c/span\u003e with an \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{R}^{2}=0.929\\)\u003c/span\u003e\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe 95% confidence interval of the slopes are \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:\\left[204.0;296.4\\right]\\)\u003c/span\u003e\u003c/span\u003e and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:[199.7;261.1]\\)\u003c/span\u003e\u003c/span\u003e for the first and second calibration curves respectively. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e shows the residual analysis of the regressions. The larger values of the calibration curve are within reasonable error, even though they are close to being outliers. It is then clear that the slope is within this interval, independent of the used chloroform.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section2\"\u003e \u003ch2\u003eSoil Extraction Experiment\u003c/h2\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e displays the results from the calibration curve from soil extraction compared to the one from chloroform. The sensitivity of the method diminishes due to the heterogeneity of the soil, because the extraction process can dissolve a wide variety of compounds than will hinder the ability to detect the adipate acid.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e shows the summary of the theoretical limits of this work compared with literature. To calculate the theoretical LOD and LOQ of the presented method equations \u003cspan refid=\"Equ3\" class=\"InternalRef\"\u003e3\u003c/span\u003e and \u003cspan refid=\"Equ4\" class=\"InternalRef\"\u003e4\u003c/span\u003e were used:\u003cdiv id=\"Equ3\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ3\" name=\"EquationSource\"\u003e\n$$\\:LOD=3.3\\times\\:\\frac{{\\sigma\\:}_{m}}{m}\\:$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e3\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ4\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ4\" name=\"EquationSource\"\u003e\n$$\\:LOQ=10\\times\\:\\frac{{\\sigma\\:}_{m}}{m}\\:$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e4\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{\\sigma\\:}_{m}\\)\u003c/span\u003e\u003c/span\u003e is the average of the standard deviations of the triplicate measurements used in the calibration curves and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:m\\)\u003c/span\u003e\u003c/span\u003e the slope of the calibration curve.\u003c/p\u003e \u003cp\u003eThe lower R\u003csup\u003e2\u003c/sup\u003e can be explained by the large number of calibration levels lower than the calculated LOQ. It does, however, show the relevance of these samples, as they are mostly explained by linear regression.\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\u003eLimits of detection and limits of quantification of PBAT concentration\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=\"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\u003eMethod\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eLOD\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eLOQ\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eR\u003csup\u003e2\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eGCMS from CHCl\u003csub\u003e3\u003c/sub\u003e (from the three independent calibration curves of this work)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e102\u0026thinsp;\u0026plusmn;\u0026thinsp;53 ng/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e340\u0026thinsp;\u0026plusmn;\u0026thinsp;178 ng/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e0.95\u0026thinsp;\u0026plusmn;\u0026thinsp;0.02\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eGCMS from CHCl\u003csub\u003e3\u003c/sub\u003e (Cho, Kim, et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Cho, Park, et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2022\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e260 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e800 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e0.996\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eGCMS from soil (This work)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0.44 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1.5 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e0.75\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNMR from soil (Nelson et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2019\u003c/span\u003e)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1.3 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e4.4 \u0026micro;g/ml\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e1.00\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=\"Sec15\" class=\"Section2\"\u003e \u003ch2\u003ePBAT microplastics in industrial compost\u003c/h2\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e depicts the evolution of the total amounts of PBAT, a combination of macro and micro plastics, during the course of degradation in compost. By knowing the initial amounts of PBAT inserted in the mesh bag and the amount of soil surrounding the samples this method helps estimate the fraction of PBAT that corresponds to micro- and nano- plastics. The range of total PBAT detected moves away from the initial amount after 23 days, suggesting monomer consumption as the GCMS cannot account for the amount corresponding to total adipic acid. Even though the film was fully fragmented after 59 days, the micro and nano plastics persist 30 days after, representing close to 10% of the initial weight at the end of the experiment.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eIt is important to understand the limitations of this methodology as well. Soil microplastics travel, migrate and interact with different actors within soil (Jin et al., \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2022\u003c/span\u003e), hence this methodology should be applied in concert with a rigorous sampling methodology such as soil quartering (Ghimire, Flury, et al., \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The LOQ and LOD soil concentrations equivalent still need to be investigated. However, this method is effective in addressing the need for microplastic detection in soils of biodegradable polymers.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusions","content":"\u003cp\u003eThe use of biodegradable polyesters such as PBAT, PLA or PCL is increasing, and while evidence of their full biodegradability is available, little is known of the effects on their environment in the microplastic phase of biodegradation. It is important to analyze and understand these effects, hence it is necessary to quantify them correctly. The methodology presented here, although with a chemical pre-treatment (FAME), shows the potential for better resolution than the available methods in literature. Additionally, it is based on gas chromatography-mass spectrometry (GCMS), a widely used and available technique with low-cost solvents and chemicals. The combination of these factors makes this protocol a simple, affordable and reproduceable method for the detection of PBAT microplastic in soil and compost.\u003c/p\u003e"},{"header":"Declarations","content":" \u003cp\u003e \u003cstrong\u003eEthical Approval\u003c/strong\u003e \u003cp\u003eNot Applicable\u003c/p\u003e \u003c/p\u003e \u003cp\u003e \u003cstrong\u003eConsent to participate\u003c/strong\u003e \u003cp\u003eNot Applicable\u003c/p\u003e \u003c/p\u003e \u003cp\u003e \u003cstrong\u003eConsent to Publish\u003c/strong\u003e \u003cp\u003eNot Applicable\u003c/p\u003e \u003c/p\u003e\u003cp\u003e \u003ch2\u003eCompeting Interests\u003c/h2\u003e \u003cp\u003eThe authors have no relevant financial or non-financial interests to disclose.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eFunding\u003c/h2\u003e \u003cp\u003eThis work was supported by the Foundation for Food and Agriculture Research (FFAR) grant #CA19-SS-0000000013 and by New York Empire State Development through award #C190155. The views, results, findings, and interpretations presented in this manuscript are those of the authors and do not necessarily reflect the views or policies of New York State.\u003c/p\u003e\u003ch2\u003eAuthor Contributions\u003c/h2\u003e \u003cp\u003eConceptualization: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Jeffrey S. Lodge, Nathan C. Eddingsaas, Christopher L. Lewis, Thomas A Trabold, Carlos A. Diaz; Methodology: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Nathan C. Eddingsaas, Christopher L. Lewis; Formal analysis and investigation: Yvan D. Hernandez-Charpak, Harshal J. Kansara; Writing - original draft preparation: Yvan D. Hernandez-Charpak; Writing - review and editing: Yvan D. Hernandez-Charpak, Harshal J. Kansara, Jeffrey S. Lodge, Nathan C. Eddingsaas, Christopher L. Lewis, Thomas A Trabold, Carlos A. Diaz; Funding acquisition: Thomas A Trabold, Carlos A. Diaz; Resources: Nathan C. Eddingsaas, Thomas A Trabold, Carlos A. Diaz; Supervision: Thomas A Trabold, Carlos A. Diaz\u003c/p\u003e\u003ch2\u003eAcknowledgments\u003c/h2\u003e \u003cp\u003eThe authors extend their gratitude to Robert Putney and Elias Putney of Impact Earth Rochester, for providing the opportunity to test the films at their industrial composting site. The authors also want to thank Sabit Nadhvee for his help in the initial measurement protocol development, Tom Allston for his help with the GCMS runs and Dr. Diana Rodriguez-Alberto for her time and advice on procedure and method. This work was possible through the support of the Foundation for Food and Agriculture Research (FFAR) grant #CA19-SS-0000000013 and by New York Empire State Development through award #C190155. The views, results, findings, and interpretations presented in this manuscript are those of the authors and do not necessarily reflect the views or policies of New York State.\u003c/p\u003e\u003ch2\u003eData availability\u003c/h2\u003e \u003cp\u003eThe authors declare that the data supporting the findings of this study are available within the paper. Should any raw data files be needed in another format they are available from the corresponding author upon reasonable request.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eAstner AF, Gillmore AB, Yu Y, Flury M, DeBruyn JM, Schaeffer SM, Hayes DG (2023) Formation, behavior, properties and impact of micro- and nanoplastics on agricultural soil ecosystems (A Review). \u003cem\u003eNanoImpact\u003c/em\u003e, \u003cem\u003e31\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.impact.2023.100474\u003c/span\u003e\u003cspan address=\"10.1016/j.impact.2023.100474\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eAstner AF, Hayes DG, O\u0026rsquo;Neill H, Evans BR, Pingali SV, Urban VS, Young TM (2019) Mechanical formation of micro- and nano-plastic materials for environmental studies in agricultural ecosystems. Sci Total Environ 685:1097\u0026ndash;1106. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.scitotenv.2019.06.241\u003c/span\u003e\u003cspan address=\"10.1016/j.scitotenv.2019.06.241\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eBandopadhyay S, Martin-Closas L, Pelacho AM, DeBruyn JM (2018) Biodegradable Plastic Mulch Films: Impacts on Soil Microbial Communities and Ecosystem Functions. Front Microbiol 9(APR). \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.3389/fmicb.2018.00819\u003c/span\u003e\u003cspan address=\"10.3389/fmicb.2018.00819\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eBhagwat G, Gray K, Wilson SP, Muniyasamy S, Vincent SGT, Bush R, Palanisami T (2020) Benchmarking Bioplastics: A Natural Step Towards a Sustainable Future. In \u003cem\u003eJournal of Polymers and the Environment\u003c/em\u003e (Vol. 28, Issue 12, pp. 3055\u0026ndash;3075). Springer. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1007/s10924-020-01830-8\u003c/span\u003e\u003cspan address=\"10.1007/s10924-020-01830-8\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eCho JY, Kim SH, Cho DH, Jung HJ, Kim BC, Bhatia SK, Gurav R, Lee J, Park SH, Park K, Joo HS, Yang YH (2022) Simultaneous monitoring of each component on degradation of blended bioplastic using gas chromatography-mass spectrometry. \u003cem\u003eAnalytical Biochemistry\u003c/em\u003e, \u003cem\u003e655\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.ab.2022.114832\u003c/span\u003e\u003cspan address=\"10.1016/j.ab.2022.114832\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eCho JY, Park SL, Kim SH, Jung HJ, Cho DH, Kim BC, Bhatia SK, Gurav R, Park SH, Park K, Yang YH (2022) Novel Poly(butylene adipate-co-terephthalate)-degrading Bacillus sp. JY35 from wastewater sludge and its broad degradation of various bioplastics. Waste Manag 144:1\u0026ndash;10. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.wasman.2022.03.003\u003c/span\u003e\u003cspan address=\"10.1016/j.wasman.2022.03.003\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eEsp\u0026iacute; E, Salmer\u0026oacute;n A, Fontecha A, Garc\u0026iacute;a Y, Real AI (2006) Plastic films for agricultural applications. J Plast Film Sheeting 22(2):85\u0026ndash;102. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1177/8756087906064220\u003c/span\u003e\u003cspan address=\"10.1177/8756087906064220\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eGhimire S, Flury M, Scheenstra EJ, Miles CA (2020) Sampling and degradation of biodegradable plastic and paper mulches in field after tillage incorporation. \u003cem\u003eScience of the Total Environment\u003c/em\u003e, \u003cem\u003e703\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.scitotenv.2019.135577\u003c/span\u003e\u003cspan address=\"10.1016/j.scitotenv.2019.135577\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eGhimire S, Scheenstra E, Miles CA (2020) Soil-biodegradable mulches for growth, yield, and quality of sweet corn in a mediterranean-type climate. HortScience 55(3):317\u0026ndash;325. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.21273/HORTSCI14667-19\u003c/span\u003e\u003cspan address=\"10.21273/HORTSCI14667-19\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eGutierrez TJ (2019) In: Guti\u0026eacute;rrez TJ (ed) Polymers for Agri-Food Applications. Springer Nature\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eHe D, Luo Y, Lu S, Liu M, Song Y, Lei L (2018) Microplastics in soils: Analytical methods, pollution characteristics and ecological risks. In \u003cem\u003eTrAC - Trends in Analytical Chemistry\u003c/em\u003e (Vol. 109, pp. 163\u0026ndash;172). Elsevier B.V. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.trac.2018.10.006\u003c/span\u003e\u003cspan address=\"10.1016/j.trac.2018.10.006\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eHrovat B, Uurasj\u0026auml;rvi E, Viitala M, del Pino AF, M\u0026auml;ntt\u0026auml;ri M, Papamatthaiakis N, Haapala A, Peiponen K-E, Roussey M, Koistinen A (2024) Preparation of synthetic micro- and nano plastics for method validation studies. Sci Total Environ 925:171821. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.scitotenv.2024.171821\u003c/span\u003e\u003cspan address=\"10.1016/j.scitotenv.2024.171821\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJin T, Tang J, Lyu H, Wang L, Gillmore AB, Schaeffer SM (2022) Activities of Microplastics (MPs) in Agricultural Soil: A Review of MPs Pollution from the Perspective of Agricultural Ecosystems. In \u003cem\u003eJournal of Agricultural and Food Chemistry\u003c/em\u003e (Vol. 70, Issue 14, pp. 4182\u0026ndash;4201). American Chemical Society. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1021/acs.jafc.1c07849\u003c/span\u003e\u003cspan address=\"10.1021/acs.jafc.1c07849\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eKasirajan S, Ngouajio M (2012) Polyethylene and biodegradable mulches for agricultural applications: A review. Agron Sustain Dev 32(2):501\u0026ndash;529. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1007/s13593-011-0068-3\u003c/span\u003e\u003cspan address=\"10.1007/s13593-011-0068-3\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eKyrikou I, Briassoulis D (2007) Biodegradation of agricultural plastic films: A critical review. J Polym Environ 15(2):125\u0026ndash;150. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1007/s10924-007-0053-8\u003c/span\u003e\u003cspan address=\"10.1007/s10924-007-0053-8\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLawson V, Taber HG (2011) \u003cem\u003eDegradable Mulch Evaluation\u003c/em\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLi C, Cui Q, Li Y, Zhang K, Lu X, Zhang Y (2022a) Effect of LDPE and biodegradable PBAT primary microplastics on bacterial community after four months of soil incubation. J Hazard Mater 429:128353. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.jhazmat.2022.128353\u003c/span\u003e\u003cspan address=\"10.1016/j.jhazmat.2022.128353\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLi C, Cui Q, Li Y, Zhang K, Lu X, Zhang Y (2022b) Effect of LDPE and biodegradable PBAT primary microplastics on bacterial community after four months of soil incubation. J Hazard Mater 429:128353. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.jhazmat.2022.128353\u003c/span\u003e\u003cspan address=\"10.1016/j.jhazmat.2022.128353\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLiu L, Zou G, Zuo Q, Li C, Gu J, Kang L, Ma M, Liang K, Liu D, Du L (2022) Soil bacterial community and metabolism showed a more sensitive response to PBAT biodegradable mulch residues than that of LDPE mulch residues. \u003cem\u003eJournal of Hazardous Materials\u003c/em\u003e, \u003cem\u003e438\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.jhazmat.2022.129507\u003c/span\u003e\u003cspan address=\"10.1016/j.jhazmat.2022.129507\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eLiu Y, Zhang W, Chen M, Zhao X, Liu H, Ge M, Li N, Ning Z, Gao W, Fan C, Li Q (2023) Molecular insights into effects of PBAT microplastics on latosol microbial diversity and DOM chemodiversity. J Hazard Mater 450:131076. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.jhazmat.2023.131076\u003c/span\u003e\u003cspan address=\"10.1016/j.jhazmat.2023.131076\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eMuroi F, Tachibana Y, Kobayashi Y, Sakurai T, Kasuya KI (2016) Influences of poly(butylene adipate-co-terephthalate) on soil microbiota and plant growth. Polym Degrad Stab 129:338\u0026ndash;346. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.polymdegradstab.2016.05.018\u003c/span\u003e\u003cspan address=\"10.1016/j.polymdegradstab.2016.05.018\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eNelson TF, Remke SC, Kohler HPE, McNeill K, Sander M (2019) Quantification of Synthetic Polyesters from Biodegradable Mulch Films in Soils. Environ Sci Technol. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1021/acs.est.9b05863\u003c/span\u003e\u003cspan address=\"10.1021/acs.est.9b05863\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eNie Z, Wang L, Lin Y, Xiao N, Zhao J, Wan X, Hu J (2022) Effects of polylactic acid (PLA) and polybutylene adipate-co-terephthalate (PBAT) biodegradable microplastics on the abundance and diversity of denitrifying and anammox bacteria in freshwater sediment. Environ Pollut 315:120343. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.envpol.2022.120343\u003c/span\u003e\u003cspan address=\"10.1016/j.envpol.2022.120343\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eNunes E, de Souza C, A. G., Rosa D (2020) dos S. Use of a chain extender as a dispersing agent of the CaCO3 into PBAT matrix. \u003cem\u003eJournal of Composite Materials\u003c/em\u003e, \u003cem\u003e54\u003c/em\u003e(10), 1373\u0026ndash;1382. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1177/0021998319880282\u003c/span\u003e\u003cspan address=\"10.1177/0021998319880282\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eProfumo A, Gorroni A, Guarnieri SA, Mellerio GG, Cucca L, Merli D (2020) GC-MS qualitative analysis of the volatile, semivolatile and volatilizable fractions of soil evidence for forensic application: A chemical fingerprinting. \u003cem\u003eTalanta\u003c/em\u003e, \u003cem\u003e219\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.talanta.2020.121304\u003c/span\u003e\u003cspan address=\"10.1016/j.talanta.2020.121304\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSeghers J, Stefaniak EA, Spina R, La, Cella C, Mehn D, Gilliland D, Held A, Jacobsson U, Emteborg H (n.d.). \u003cem\u003ePreparation of a reference material for microplastics in water-evaluation of homogeneity\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1007/s00216-021-03198-7/Published\u003c/span\u003e\u003cspan address=\"10.1007/s00216-021-03198-7/Published\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSintim HY, Bary AI, Hayes DG, Wadsworth LC, Anunciado MB, English ME, Bandopadhyay S, Schaeffer SM, DeBruyn JM, Miles CA, Reganold JP, Flury M (2020) In situ degradation of biodegradable plastic mulch films in compost and agricultural soils. Sci Total Environ 727:138668. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.scitotenv.2020.138668\u003c/span\u003e\u003cspan address=\"10.1016/j.scitotenv.2020.138668\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eTan Z, Yi Y, Wang H, Zhou W, Yang Y, Wang C (2016) \u003cem\u003ePhysical and Degradable Properties of Mulching Films Prepared from Natural Fibers and Biodegradable Polymers\u003c/em\u003e. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.3390/app6050147\u003c/span\u003e\u003cspan address=\"10.3390/app6050147\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eTewari A, Almuhtaram H, McKie MJ, Andrews RC (2022) Microplastics for Use in Environmental Research. J Polym Environ 30(10):4320\u0026ndash;4332. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1007/s10924-022-02519-w\u003c/span\u003e\u003cspan address=\"10.1007/s10924-022-02519-w\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eTouchaleaume F, Martin-Closas L, Angellier-Coussy H, Chevillard A, Cesar G, Gontard N, Gastaldi E (2016) Performance and environmental impact of biodegradable polymers as agricultural mulching films. Chemosphere 144:433\u0026ndash;439. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.chemosphere.2015.09.006\u003c/span\u003e\u003cspan address=\"10.1016/j.chemosphere.2015.09.006\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eUnited Nations Environment Programme (2022) \u003cem\u003ePlastics in Agriculture - An Environmental Challenge\u003c/em\u003e. UNEP. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://wedocs.unep.org/bitstream/handle/20.500.11822/40403/Plastics_Agriculture.pdf\u003c/span\u003e\u003cspan address=\"https://wedocs.unep.org/bitstream/handle/20.500.11822/40403/Plastics_Agriculture.pdf\" targettype=\"URL\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eUwamungu JY, Wang Y, Shi G, Pan S, Wang Z, Wang L, Yang S (2022) Microplastic contamination in soil agro-ecosystems: A review. Environmental Advances, vol 9. Elsevier Ltd. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.envadv.2022.100273\u003c/span\u003e\u003cspan address=\"10.1016/j.envadv.2022.100273\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eWollein U, Schramek N (2012) Simultaneous determination of alkyl mesilates and alkyl besilates in finished drug products by direct injection GC/MS. Eur J Pharm Sci 45(1\u0026ndash;2):201\u0026ndash;204. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.ejps.2011.11.008\u003c/span\u003e\u003cspan address=\"10.1016/j.ejps.2011.11.008\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eWortman SE, Jeske E, Samuelson MB, Drijber R (2022) A new method for detecting micro-fragments of biodegradable mulch films containing poly(butylene adipate-co-terephthalate) (PBAT) in soil. J Environ Qual 51(1):123\u0026ndash;128. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1002/jeq2.20311\u003c/span\u003e\u003cspan address=\"10.1002/jeq2.20311\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eYu Y, Griffin-LaHue DE, Miles CA, Hayes DG, Flury M (2021) Are micro- and nanoplastics from soil-biodegradable plastic mulches an environmental concern? J Hazard Mater Adv 4. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.hazadv.2021.100024\u003c/span\u003e\u003cspan address=\"10.1016/j.hazadv.2021.100024\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eZhang S, Yang X, Gertsen H, Peters P, Sal\u0026aacute;nki T, Geissen V (2018) A simple method for the extraction and identification of light density microplastics from soil. Sci Total Environ 616\u0026ndash;617:1056\u0026ndash;1065. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.scitotenv.2017.10.213\u003c/span\u003e\u003cspan address=\"10.1016/j.scitotenv.2017.10.213\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eZumstein MT, Schintlmeister A, Nelson TF, Baumgartner R, Woebken D, Wagner M, Kohler HPE, McNeill K, Sander M (2018) Biodegradation of synthetic polymers in soils: Tracking carbon into CO2 and microbial biomass. Sci Adv 4(7). \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1126/sciadv.aas9024\u003c/span\u003e\u003cspan address=\"10.1126/sciadv.aas9024\" 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":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":true,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"environmental-science-and-pollution-research","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"espr","sideBox":"Learn more about [Environmental Science and Pollution Research](https://www.springer.com/journal/11356)","snPcode":"11356","submissionUrl":"https://submission.nature.com/new-submission/11356/3","title":"Environmental Science and Pollution Research","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Microplastics, PBAT, GCMS, biodegradation, soil extraction, Microplastics detection","lastPublishedDoi":"10.21203/rs.3.rs-5285330/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-5285330/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eWith the increasing use of biodegradable plastics in agriculture and food packaging, it has become increasingly important to assess the effects of their fragmentation and mineralization in the environment (i.e. soil, compost). PBAT is a biodegradable polyester widely used in biodegradable mulch films that are intended to fragment and mineralize in soil. To study these effects, novel methodologies are needed to quantify PBAT microplastics in these diverse environments. This work seeks to answer whether Gas Chromatography Mass Spectrometry (GCMS) can be used as a tool to assess PBAT microplastics in soil. A method was developed that allows PBAT soil extraction by ultrasonication and GCMS quantification after a fatty acid methyl ester derivatization. To validate the method, an industrial compost degradation experiment was carried out to evidence the weight loss of PBAT film and quantify the micro- and nano-plastic generated from them. The presented method improved the existing resolution by, at least, one order of magnitude compared to reported methods. In conclusion, a novel, simple, affordable, and reproducible methodology for PBAT microplastics detection was developed improving the limits of detection and quantification. The method was tested on an industrial compost experiment, demonstrating the ability to trace the totality of the plastic over time, evidencing that PBAT is consumed in the industrial compost environment.\u003c/p\u003e","manuscriptTitle":"Quantitative methodology for poly (butylene adipate-co-terephthalate) (PBAT) microplastic detection in soil and compost","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-11-21 17:58:49","doi":"10.21203/rs.3.rs-5285330/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"reviewerAgreed","content":"","date":"2024-11-07T01:18:23+00:00","index":0,"fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-11-06T11:07:22+00:00","index":"","fulltext":""},{"type":"editorInvited","content":"Environmental Science and Pollution Research","date":"2024-11-04T11:35:28+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-10-31T04:32:46+00:00","index":"","fulltext":""},{"type":"submitted","content":"Environmental Science and Pollution Research","date":"2024-10-30T16:00:00+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"environmental-science-and-pollution-research","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"espr","sideBox":"Learn more about [Environmental Science and Pollution Research](https://www.springer.com/journal/11356)","snPcode":"11356","submissionUrl":"https://submission.nature.com/new-submission/11356/3","title":"Environmental Science and Pollution Research","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"25a7cf44-cca9-49aa-88ed-468d05fda551","owner":[],"postedDate":"November 21st, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2025-02-03T16:06:31+00:00","versionOfRecord":{"articleIdentity":"rs-5285330","link":"https://doi.org/10.1007/s11356-025-35978-4","journal":{"identity":"environmental-science-and-pollution-research","isVorOnly":false,"title":"Environmental Science and Pollution Research"},"publishedOn":"2025-01-31 15:57:42","publishedOnDateReadable":"January 31st, 2025"},"versionCreatedAt":"2024-11-21 17:58:49","video":"","vorDoi":"10.1007/s11356-025-35978-4","vorDoiUrl":"https://doi.org/10.1007/s11356-025-35978-4","workflowStages":[]},"version":"v1","identity":"rs-5285330","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-5285330","identity":"rs-5285330","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}