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Vial-coated thin film microextraction for perfluoroalkyl carboxylic acids (PFCAs) determination in water by GC–MS
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100147
J․Mabel Luna-Díaz , Luz O․ Leal-Quezada , Laura Ferrer , Edwin Palacio
{"title":"Vial-coated thin film microextraction for perfluoroalkyl carboxylic acids (PFCAs) determination in water by GC–MS","authors":"J․Mabel Luna-Díaz ,&nbsp;Luz O․ Leal-Quezada ,&nbsp;Laura Ferrer ,&nbsp;Edwin Palacio","doi":"10.1016/j.sampre.2025.100147","DOIUrl":"10.1016/j.sampre.2025.100147","url":null,"abstract":"<div><div>Perfluoroalkyl carboxylic acids (PFCAs), a subclass of perfluoroalkyl substances (PFAs) commonly detected in water, are of increasing concern due to their persistence, bioaccumulative nature, and harmful effects on health. Determining PFCAs in environmental matrices is challenging because they are typically present at ng L⁻¹ levels and tend to adsorb onto materials like filtration membranes, causing significant losses during analysis. To address these challenges, a thin-film microextraction (TFME)-coated vial was designed for PFCA (C5–C10) extraction, coupled with gas chromatography-mass spectrometry (GC–MS). Glass was selected as the support material due to its low adsorption rate and superior chemical resistance compared to other polymers. The TFME coating, made from a weak anion exchange resin and polyacrylonitrile (10 % w/w) as a binder polymer, effectively extracts analytes from complex matrices while minimizing co-extraction of interfering macromolecules. The method eliminates the need for sample filtration, preventing PFCA loss in filtration membranes. Under optimal conditions, the extraction efficiency ranged from 70 to 100 %. Detection and quantification limits were 0.13–2.1 ng L⁻¹ and 0.42–7.1 ng L⁻¹, respectively. Intra- and inter-assay relative standard deviations (% RSD) were 4.9–2.2 % and 4.8–2.3 %, respectively, with a linear working range of 10–1000 ng L⁻¹ for the TFME-coated device. This method is suitable for PFCA determination in drinking water and complies with the Directive 2020/2184, which sets a maximum allowable limit of 500 ng L⁻¹ for total PFAs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100147"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130333","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Towards eco-metabolomics: NADES-guided extraction enables semi-quantitative metabolomics for Melissa officinalis
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100154
Chiara Spaggiari , Isa Sara Aimee Hiemstra , Antoinette Kazbar , Gabriele Costantino , Laura Righetti
{"title":"Towards eco-metabolomics: NADES-guided extraction enables semi-quantitative metabolomics for Melissa officinalis","authors":"Chiara Spaggiari ,&nbsp;Isa Sara Aimee Hiemstra ,&nbsp;Antoinette Kazbar ,&nbsp;Gabriele Costantino ,&nbsp;Laura Righetti","doi":"10.1016/j.sampre.2025.100154","DOIUrl":"10.1016/j.sampre.2025.100154","url":null,"abstract":"<div><div>In recent years, there has been a growing emphasis on the development of green extraction techniques that minimize environmental impact while maximizing yield of the extracted compounds. To this aim, in this study we investigated the potential of green solvents for extracting bioactive compounds from <em>Melissa officinalis</em> (MO) leaves. Specifically, we focus on the application of 20 Natural Deep Eutectic Solvents (NADES) with a relative polarity ranging from 0.34 to 1.29. Their extraction affinity against a set of 11 plant metabolites was predicted using COSMO-RS software and experimentally validated using quantitative LC<img>HRMS analysis. Subsequently, the same extracts were subjected to non-target metabolomics to uncover the NADES selectivity towards the wide spectrum of MO leaf metabolites. Data preprocessing and feature alignment were performed using MZmine, and aligned features were annotated using SIRIUS+CSI:FingerID.</div><div>Overall, 249 and 195, metabolites were annotated in positive and negative ionization ion mode, respectively. Additionally, to have a more accurate view of the different NADES extraction capacity, we adopted a semi-quantitative approach that enables the prediction of concentration for all the annotated metabolites (N = 444).</div><div>The results highlighted the selectivity of some NADES in extracting very diverse biochemical classes, providing valuable insights into the composition and concentration of bioactive compounds. Interestingly, thymol-menthol NADES demonstrated the ability to efficiently extract a broad range of bioactive compounds, yielding a metabolome comparable to that obtained with conventional ethanolic. Overall, the entire workflow facilitated the green extraction and annotation of known bioactive molecules that had never been described in MO.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100154"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143395307","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Electrospun chitosan modified montmorillonite/polyvinyl alcohol nanofibers as suitable coating for fiber-in-tube solid-phase microextraction of trace amounts of tricyclic antidepressants in biological fluids
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100145
Saeed Pourhosseini, Yadollah Yamini, Seyedeh Sara Nasrollahi
{"title":"Electrospun chitosan modified montmorillonite/polyvinyl alcohol nanofibers as suitable coating for fiber-in-tube solid-phase microextraction of trace amounts of tricyclic antidepressants in biological fluids","authors":"Saeed Pourhosseini,&nbsp;Yadollah Yamini,&nbsp;Seyedeh Sara Nasrollahi","doi":"10.1016/j.sampre.2024.100145","DOIUrl":"10.1016/j.sampre.2024.100145","url":null,"abstract":"<div><div>Chitosan intercalated montmorillonite and polyvinyl alcohol-citric acid (PVA/CA) nanofibers were electrospun onto stainless steel wires. The fibers were placed inside a stainless steel tube and utilized for fiber-in-tube solid phase microextraction (FIT-SPME) to detect trace levels of tricyclic antidepressant drugs (TCAs) in biological samples. The analytes were separated and quantified using gas chromatography coupled with mass spectrometric detection (GC–MS). The effects of various parameters on the extraction efficiency, including pH (9), extraction time (25 min), extraction flow rate (3 mL min<sup>-1</sup>), salt addition (0 % w/v), type of eluent (ethanol 99 %), eluent volume (300 µL), and desorption flow rate (70 µL min<sup>-1</sup>), were investigated and optimized. Under optimal conditions, the linear dynamic range for doxepin, and sertraline was found to be 0.08–750.0 ng mL<sup>-1</sup>; for amitriptyline, desipramine, and trimipramine, it was 10.0–750.0 ng mL<sup>-1</sup>; and for carbamazepine and maprotiline, it was 50.0–750.0 ng mL<sup>-1</sup>. The proposed method exhibited low limits of detections in the range of 0.02–15.2 ng mL<sup>-1</sup>. Additionally, coefficients of determination (R²) exceeding 0.9911 were achieved, indicating excellent linearity for the calibration curves. To assess the feasibility of the FIT-SPME-GC–MS method, extraction and analysis of TCAs were performed on plasma and urine samples. Relative recovery percentages (RR%) ranged from 90.3 % to 117.6 %.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100145"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143131051","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Endogenous HiBiT-tagging combined with affinity complementation: A new strategy for small open reading frame-encoded polypeptide detection in bacteria
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100143
Laure Simoens, Veronique Jonckheere, Dominiek Catteeuw, Petra Van Damme
{"title":"Endogenous HiBiT-tagging combined with affinity complementation: A new strategy for small open reading frame-encoded polypeptide detection in bacteria","authors":"Laure Simoens,&nbsp;Veronique Jonckheere,&nbsp;Dominiek Catteeuw,&nbsp;Petra Van Damme","doi":"10.1016/j.sampre.2024.100143","DOIUrl":"10.1016/j.sampre.2024.100143","url":null,"abstract":"<div><div>Bacterial genome annotations are continuously refined with the advent of novel techniques. Ribosome profiling, or Ribo-seq, utilizing next-generation sequencing to link genomic regions with translational activity, has uncovered numerous small open reading frames (sORFs) - arbitrarily defined as ORFs no longer than 300 base pairs - as a generally under-annotated class of genomic elements in both eukaryotic and prokaryotic genomes. While sORFs can function as regulatory elements, they may also translate into small proteins (equal to or shorter than 100 amino acids), classified as sORF-encoded polypeptides (SEPs). The inherent limitations of ribosome profiling necessitate the experimental validation of predicted (s)ORFs at the protein expression level. However, the small size and unique biochemical characteristics of SEPs pose significant challenges for traditional protein detection methods, like mass spectrometry and immunoblotting. In this study, we introduce HiBiT blotting, a luminescent, complementation-based protein detection method, as a highly sensitive alternative to antibody-based immunoblotting for investigating SEP expression in <em>Salmonella enterica</em> (serovar) Typhimurium (<em>S.</em> Typhimurium) at endogenous levels. We demonstrate its complementarity to mass spectrometry as an expression validation tool. Additionally, employing a biochemical fractionation approach, we determined the subcellular localization of validated <em>S.</em> Typhimurium SEPs, initiating exploration into the functional aspects of these SEPs, and proposed enrichment strategies that may facilitate future experimental validation of Ribo-seq-predicted sORFs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100143"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130330","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mixed matrix membranes based on cellulose acetate recycled from cigarette butts and metal-organic frameworks for thin film solid-phase microextraction: Determination of phenols in environmental waters
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100150
Massimo G. De Cesaris , María J. Trujillo-Rodríguez , Jorge Pasán , Alessandra Gentili , Verónica Pino
{"title":"Mixed matrix membranes based on cellulose acetate recycled from cigarette butts and metal-organic frameworks for thin film solid-phase microextraction: Determination of phenols in environmental waters","authors":"Massimo G. De Cesaris ,&nbsp;María J. Trujillo-Rodríguez ,&nbsp;Jorge Pasán ,&nbsp;Alessandra Gentili ,&nbsp;Verónica Pino","doi":"10.1016/j.sampre.2025.100150","DOIUrl":"10.1016/j.sampre.2025.100150","url":null,"abstract":"<div><div>The recovery of raw materials from waste is a viable strategy to transition to more circular and greener methodologies. In this study, cigarette filters were recycled to obtain cellulose acetate and re-used as a support for a sorbent material in a microextraction procedure. Thus, this biosorbent was combined with a metal-organic framework (MIL-101(<em>Fe</em>)) and configurated in a membrane format of 300 µm of thickness via solvent casting. The developed mixed matrix membranes were characterized by Fourier-transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy, and energy dispersion X-ray. Kinetic adsorption studies for a group of 14 phenols (chlorophenols, alkylphenols, and bisphenols) present in waters and partitioning to the membrane systems were performed to gain insights into the extraction mechanisms of the membranes. The kinetics were fitted to pseudo-first order and interparticle diffusion models, with data indicating that chloro‑ and alkyl-phenols were adsorbed faster than bisphenols. Besides, the resulting membranes were utilized in thin film solid-phase microextraction (TF-SPME) in combination with high-performance liquid chromatography (HPLC) with diode array detection (DAD) and fluorescent detector (FLD). The optimized method using these mixed matrix membranes (with dish shape and 1 cm of diameter) required 60 min of extraction with agitation followed by 10 min of desorption in 500 µL of basic ethanol. Low limits of detection, down to 2.13 µg·L<sup>-1</sup>, were achieved, together with good performance in SPMS and BAGI metrics, with scores of 5.89 and 62.5, respectively. The performance with river waters was accompanied by adequate relative recoveries (74.3–117 %), reproducibility (with inter-day RSD values lower than 18 %), and absolute recoveries (up to 59 %).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100150"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143131054","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Tailoring a MOF-on-MOF (ZIF-8-on-NH2-MIL-53(Al)) Hybrid Composite for Micro Solid Phase Extraction of Furosemide in artificial biological fluids prior to LC-q-TOF/MS detection
IF 5.2
Advances in Sample Preparation Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100157
Zinar Pinar Gumus , Mustafa Soylak
{"title":"Tailoring a MOF-on-MOF (ZIF-8-on-NH2-MIL-53(Al)) Hybrid Composite for Micro Solid Phase Extraction of Furosemide in artificial biological fluids prior to LC-q-TOF/MS detection","authors":"Zinar Pinar Gumus ,&nbsp;Mustafa Soylak","doi":"10.1016/j.sampre.2025.100157","DOIUrl":"10.1016/j.sampre.2025.100157","url":null,"abstract":"<div><div>Furosemide, a powerful diuretic that increases urine excretion, is used to treat many diseases. However, due to its abuse in sport, it is considered a doping substance. As a result, it has been banned by the World Anti-Doping Agency (WADA) and included in the group of diuretics and masking agents. Given the clinical significance of furosemide and its dependable application in athletics, this research employed the \"MOF-on-MOF\" hybrid material composite to leverage the synergistic effects of various components for detecting this drug in biological samples. After characterization of the ZIF-8-on-NH<sub>2</sub>-MIL-53(Al) composite by FT-IR, XRD, TGA, XPS, BET and SEM-EDX techniques, the µ-SPE procedure was optimized using liquid chromatography-time of flight mass spectrometry (LC-q-TOF/MS) based on the recovery values. The optimum conditions were determined as pH 6, adsorbent amount of 20 mg, and total adsorption-desorption time of 7 min. The recovery values of the solid-phase extraction method for simulated body fluids samples under optimum conditions were between 77.5 % and 93.4 %. The µ-SPE technique was effectively utilized on physiological samples using the ZIF-8-on-NH<sub>2</sub>-MIL-53(Al) composite under optimal conditions. This study's findings will inform future research into the design of 'MOF-on-MOF' hybrids for various applications.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100157"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143438238","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Extraction of synthetic cathinones from biological samples: A systematic review 从生物样本中提取合成卡西酮:系统综述
IF 5.2
Advances in Sample Preparation Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100133
Mengjie Gu, Shutong Xue, Menghan Hou, Xiantao Shen
{"title":"Extraction of synthetic cathinones from biological samples: A systematic review","authors":"Mengjie Gu,&nbsp;Shutong Xue,&nbsp;Menghan Hou,&nbsp;Xiantao Shen","doi":"10.1016/j.sampre.2024.100133","DOIUrl":"10.1016/j.sampre.2024.100133","url":null,"abstract":"<div><div>Analysis of biological samples containing synthetic cathinones has become a significant area of interest for researchers in recent years, because synthetic cathinones can cause adverse reactions such as delusions and hallucinations. Generally, the intricate nature of the sample matrix and exceedingly low drug concentration in biological samples present significant challenges for the determination of target substances. Accordingly, scientists were dedicated to the advancement of effective sample preparation techniques to address these difficulties. However, the current reviews involved in synthetic cathinones all focused on detection methods. A systematic review focusing on sample preparation for the quantification of synthetic cathinones is still lacking. In light of that, this paper reviewed the most commonly used sample preparation techniques for synthetic cathinones. Recent advances in sample preparation techniques for synthetic cathinones in different biological samples such as blood, urine, oral fluid and hair samples were discussed. In addition, we prospected the challenges and the future perspectives of biological sample preparation techniques for synthetic cathinones determination.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100133"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142527745","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Core-shell polymer microspheres with strong cation-exchange character for the extraction of basic pharmaceuticals from aqueous samples 具有强阳离子交换特性的核壳聚合物微球用于从水样品中提取基本药物
IF 5.2
Advances in Sample Preparation Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100136
Alberto Moral , Alan Corrigan , Francesc Borrull , Peter A.G. Cormack , Núria Fontanals , Rosa Maria Marcé
{"title":"Core-shell polymer microspheres with strong cation-exchange character for the extraction of basic pharmaceuticals from aqueous samples","authors":"Alberto Moral ,&nbsp;Alan Corrigan ,&nbsp;Francesc Borrull ,&nbsp;Peter A.G. Cormack ,&nbsp;Núria Fontanals ,&nbsp;Rosa Maria Marcé","doi":"10.1016/j.sampre.2024.100136","DOIUrl":"10.1016/j.sampre.2024.100136","url":null,"abstract":"<div><div>The application of core-shell materials as packing materials for liquid chromatography columns is common in analytical chemistry, however their use as sorbents in solid-phase extraction (SPE) is surprisingly underexplored. In the present study, core-shell polymer microspheres with strong cation-exchange character were designed and synthesized. These new materials benefit from having hypercrosslinked and relatively thin functional shells, which raises the specific surface areas and sorption capacities of the sorbents and allows for relatively shorter diffusion path lengths for analytes.</div><div>The core-shell polymer microspheres were evaluated as SPE sorbents for the extraction of basic pharmaceuticals from environmental water samples. Following optimization of the pH and volume of the loading solution, as well as optimization of the loading step, the SPE method was validated in terms of apparent and relative recoveries, matrix effect, limits of detection and quantification and precision. The method yielded very promising results in terms of apparent recoveries (&gt;39 %) and matrix effect (&lt;±29 %) and was applied successfully to the determination of basic pharmaceuticals in environmental water samples (river water, effluent wastewater and influent wastewater).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100136"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142702243","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A miniaturized QuEChERS-DLLME method for simultaneous determination of acetamide, acrylamide, and glycidamide in infant formula using GC–MS 利用气相色谱-质谱同时测定婴儿配方奶粉中乙酰胺、丙烯酰胺和缩水甘油醚的微型 QuEChERS-DLLME 方法
IF 5.2
Advances in Sample Preparation Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100141
J.A. Custodio-Mendoza , M.P. España Fariñas , A.M. Ares-Fuentes , M.A. Kurek , A.M. Carro Díaz
{"title":"A miniaturized QuEChERS-DLLME method for simultaneous determination of acetamide, acrylamide, and glycidamide in infant formula using GC–MS","authors":"J.A. Custodio-Mendoza ,&nbsp;M.P. España Fariñas ,&nbsp;A.M. Ares-Fuentes ,&nbsp;M.A. Kurek ,&nbsp;A.M. Carro Díaz","doi":"10.1016/j.sampre.2024.100141","DOIUrl":"10.1016/j.sampre.2024.100141","url":null,"abstract":"<div><div>Infant formula is the only food product suitable for infants during the first months of life. Therefore, evaluating food contaminants is essential for ensuring infant food safety. We developed a miniaturized QuEChERS (µ-QuEChERS) method combined with Dispersive Liquid-Liquid Microextraction (DLLME) to detect acrylamide, glycidamide, and acetamide in IF simultaneously. Several parameters were optimized, including sample size, extraction solvent, clean-up sorbent type, and amount, among others, using an asymmetrical factorial design. The method also incorporated xanthydrol derivatization under light-protected, acidic conditions within the DLLME process, improving selectivity and enrichment.</div><div>The µ-QuEChERS-DLLME method was validated according to FDA guidelines, demonstrating high selectivity, specificity, and excellent linearity (<em>r</em>² ≥ 0.9995). Recovery rates ranged from 91.0 % to 110.1 %, with precision (RSD ≤ 9.1 %). The method's sustainability was evaluated using the AGREEprep tool. It was applied to analyze acrylamide, glycidamide, and acetamide in 8 infant formula samples. Acetamide was quantifiable in one sample (230 ng/g), while acrylamide levels ranged from below the quantification limit to 50 ng/g, consistent with previous studies. This demonstrates the method's robustness for amide analysis in infant formula.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100141"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142721808","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Microextraction by packed sorbent: Introducing a novel hybrid silica-based chitosan-graphene oxide biosorbent for the evaluation of pesticides and antibiotics in food matrices 利用填料吸附剂进行微萃取:采用新型壳聚糖-氧化石墨烯混合硅基生物吸附剂评估食品基质中的农药和抗生素
IF 5.2
Advances in Sample Preparation Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100134
Rafael O. Martins, Fernando M. Lanças
{"title":"Microextraction by packed sorbent: Introducing a novel hybrid silica-based chitosan-graphene oxide biosorbent for the evaluation of pesticides and antibiotics in food matrices","authors":"Rafael O. Martins,&nbsp;Fernando M. Lanças","doi":"10.1016/j.sampre.2024.100134","DOIUrl":"10.1016/j.sampre.2024.100134","url":null,"abstract":"<div><div>This study introduces a novel silica-graphene oxide@chitosan (SiGO@CS) material as a packed biosorbent for microextraction by packed sorbent (MEPS), followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of pesticides (atrazine and thiamethoxam) and antibiotics (ceftiofur and sulfonamide) in food samples. The graphene-based aerogel was modified with varying percentages of silica-graphene oxide/chitosan (w/w) and characterized to confirm successful chitosan incorporation. Optimization of the MEPS protocol, using 2<sup>4–1</sup> and 2<sup>3</sup> experimental designs, identified draw/eject and washing cycles as the most influential parameters for extraction efficiency. The SiGO@CS biosorbent with 80 % CS/SiGO (w/w) exhibited superior extraction efficiency compared to other ratios and commercial sorbents. The method demonstrated excellent linearity for all analytes (R² &gt; 0.9900), with low limits of detection (LOD) and quantification (LOQ) ranging from 0.020 to 0.045 µg <span>l</span><sup>-1</sup> and 0.045 to 1.0 µg <span>l</span><sup>-1</sup> for pesticides, respectively, and 5 to 15 µg <span>l</span><sup>-1</sup> and 15 to 20 µg <span>l</span><sup>-1</sup> for antibiotics, respectively. Trueness values were within 82 % to 109 %. The method's green credentials were confirmed using AGREEprep and the Green Analytical Procedure Index (GAPI) approach, highlighting sorbent reusability (over 15 times) and rapid analytical throughput (5 min per sample) with low use of pre-treated sample extract volume (500 µL). The application to local corn, tomato, and milk samples confirmed the detection and quantification of thiamethoxam and atrazine at concentrations above the recommended ingestion per day for one sample of tomato and corn out of the three samples analyzed. Furthermore, using the novel SiGO@CS biosorbent in the MEPS protocol offers a green, high-performance analytical alternative to traditional sorbent phases, with the potential for evaluating trace levels of pesticides and antibiotics in food matrices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100134"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142593277","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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