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Endogenous HiBiT-tagging combined with affinity complementation: A new strategy for small open reading frame-encoded polypeptide detection in bacteria
IF 5.2 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100143
Laure Simoens, Veronique Jonckheere, Dominiek Catteeuw, Petra Van Damme
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 Salmonella enterica (serovar) Typhimurium (S. 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 S. 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.
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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 Q1 CHEMISTRY, ANALYTICAL 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
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(Fe)) 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-1, 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 %).
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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 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100157
Zinar Pinar Gumus , Mustafa Soylak
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-NH2-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-NH2-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.
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引用次数: 0
Biodiesel as a green alternative solvent in dispersive liquid-liquid microextraction 生物柴油作为分散液-液微萃取的绿色替代溶剂
IF 5.2 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100163
Samara Soares, Fábio R.P. Rocha
Biodiesel, a fuel derived from renewable sources, is a nonpolar liquid, composed of alkyl esters derived from long-chain carboxylic acids. Because of its environmental friendliness, large-scale production, and cost-effectiveness, biodiesel is herein proposed as a green solvent for liquid-liquid microextraction. Its potential has been demonstrated through the extraction of model analytes, with varying polarities through analytical measurements performed by smartphone-based digital images. Partition coefficients biodiesel/water (log P) were –0.45 (pH 2.0) for crystal violet, –1.3 (pH 7.0) for bromocresol green, 1.05 for PAN, 3.48 for Cu(II)-PAN complex, and 2.14 for quercetin. Biodiesel was effective in extracting nonpolar species, with extraction efficiencies of 90 % for PAN, 99 % for quercetin and Cu(II)-PAN complex. Efficiency of extraction of the Cu(II)-PAN complex increased in the following order: chloroform, ethyl acetate, and biodiesel, and the highest recoveries were achieved with biodiesel as solvent. Only slightly variations in the extraction efficiency was observed from biodiesel produced from different feedstock. Biodiesel was also efficient for extraction of the ion-pairs from anionic surfactants and methylene blue, with the perspective of replacing chloroform in this classical method. The results showed that biodiesel is an efficient alternative solvent to replace typical toxic solvents, with greenness demonstrated through the Green Star and AGREE metrics.
{"title":"Biodiesel as a green alternative solvent in dispersive liquid-liquid microextraction","authors":"Samara Soares,&nbsp;Fábio R.P. Rocha","doi":"10.1016/j.sampre.2025.100163","DOIUrl":"10.1016/j.sampre.2025.100163","url":null,"abstract":"<div><div>Biodiesel, a fuel derived from renewable sources, is a nonpolar liquid, composed of alkyl esters derived from long-chain carboxylic acids. Because of its environmental friendliness, large-scale production, and cost-effectiveness, biodiesel is herein proposed as a green solvent for liquid-liquid microextraction. Its potential has been demonstrated through the extraction of model analytes, with varying polarities through analytical measurements performed by smartphone-based digital images. Partition coefficients biodiesel/water (log P) were –0.45 (pH 2.0) for crystal violet, –1.3 (pH 7.0) for bromocresol green, 1.05 for PAN, 3.48 for Cu(II)-PAN complex, and 2.14 for quercetin. Biodiesel was effective in extracting nonpolar species, with extraction efficiencies of 90 % for PAN, 99 % for quercetin and Cu(II)-PAN complex. Efficiency of extraction of the Cu(II)-PAN complex increased in the following order: chloroform, ethyl acetate, and biodiesel, and the highest recoveries were achieved with biodiesel as solvent. Only slightly variations in the extraction efficiency was observed from biodiesel produced from different feedstock. Biodiesel was also efficient for extraction of the ion-pairs from anionic surfactants and methylene blue, with the perspective of replacing chloroform in this classical method. The results showed that biodiesel is an efficient alternative solvent to replace typical toxic solvents, with greenness demonstrated through the Green Star and AGREE metrics.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100163"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143518978","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 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100133
Mengjie Gu, Shutong Xue, Menghan Hou, Xiantao Shen
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.
近年来,对含有合成卡西酮的生物样本进行分析已成为研究人员关注的一个重要领域,因为合成卡西酮可导致妄想和幻觉等不良反应。一般来说,生物样本中复杂的样本基质和极低的药物浓度给目标物质的测定带来了巨大挑战。因此,科学家们致力于开发有效的样品制备技术来解决这些难题。然而,目前有关合成卡西酮的综述都集中在检测方法上。目前仍缺乏针对合成卡西酮定量的样品制备的系统综述。有鉴于此,本文综述了合成卡西酮最常用的样品制备技术。讨论了不同生物样本(如血液、尿液、口腔液和毛发样本)中合成卡西酮的样本制备技术的最新进展。此外,我们还展望了用于合成卡西酮测定的生物样品制备技术所面临的挑战和未来前景。
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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 Q1 CHEMISTRY, ANALYTICAL 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
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.
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 (>39 %) and matrix effect (<±29 %) and was applied successfully to the determination of basic pharmaceuticals in environmental water samples (river water, effluent wastewater and influent wastewater).
将核壳材料用作液相色谱柱的填料在分析化学中很常见,但将其用作固相萃取(SPE)中的吸附剂却鲜有人问津。本研究设计并合成了具有强阳离子交换特性的核壳聚合物微球。这些新材料具有超交联和相对较薄的功能性外壳,从而提高了吸附剂的比表面积和吸附能力,并使分析物的扩散路径长度相对较短。在优化了上样溶液的 pH 值和体积以及上样步骤后,从表观和相对回收率、基质效应、检出限、定量限和精密度等方面对 SPE 方法进行了验证。该方法在表观回收率(39%)和基质效应(±29%)方面都取得了很好的结果,并成功应用于环境水样(河水、废水和进水)中基本药物的测定。
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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 Q1 CHEMISTRY, ANALYTICAL 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
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.
The µ-QuEChERS-DLLME method was validated according to FDA guidelines, demonstrating high selectivity, specificity, and excellent linearity (r² ≥ 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.
婴儿配方奶粉是唯一适合婴儿在出生后最初几个月食用的食品。因此,评估食品污染物对确保婴儿食品安全至关重要。我们开发了一种微型 QuEChERS(µ-QuEChERS)与分散液-液微萃取(DLLME)相结合的方法,可同时检测 IF 中的丙烯酰胺、缩水甘油酰胺和乙酰胺。采用非对称因子设计优化了多个参数,包括样品量、萃取溶剂、净化吸附剂类型和用量等。μ-QuEChERS-DLLME方法根据美国食品药品管理局(FDA)指南进行了验证,结果表明该方法具有高选择性、特异性和良好的线性关系(r² ≥ 0.9995)。回收率在 91.0 % 到 110.1 % 之间,精确度(RSD ≤ 9.1 %)高。使用 AGREEprep 工具对该方法的可持续性进行了评估。该方法用于分析 8 个婴儿配方奶粉样品中的丙烯酰胺、缩水甘油胺和乙酰胺。其中一个样品中的乙酰胺可以定量(230 纳克/克),而丙烯酰胺的含量从低于定量限到 50 纳克/克不等,与之前的研究结果一致。这表明该方法对婴儿配方奶粉中的酰胺分析具有良好的稳定性。
{"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 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100134
Rafael O. Martins, Fernando M. Lanças
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 24–1 and 23 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 > 0.9900), with low limits of detection (LOD) and quantification (LOQ) ranging from 0.020 to 0.045 µg l-1 and 0.045 to 1.0 µg l-1 for pesticides, respectively, and 5 to 15 µg l-1 and 15 to 20 µg l-1 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.
本研究介绍了一种新型二氧化硅-氧化石墨烯@壳聚糖(SiGO@CS)材料,它是一种填料生物吸附剂,可用于填料吸附剂微萃取(MEPS),然后通过液相色谱-串联质谱(LC-MS/MS)分析食品样品中的农药(阿特拉津和噻虫嗪)和抗生素(头孢噻呋和磺酰胺)。用不同比例的二氧化硅-氧化石墨烯/壳聚糖(重量比)对石墨烯基气凝胶进行了改性,并对其进行了表征,以确认壳聚糖的成功加入。采用 24-1 和 23 实验设计对 MEPS 方案进行了优化,确定抽吸/喷射和洗涤周期是对萃取效率影响最大的参数。与其他比例和商用吸附剂相比,SiGO@CS 生物吸附剂(CS/SiGO(重量比)为 80%)的萃取效率更高。该方法对所有分析物均表现出良好的线性关系(R² > 0.9900),检出限(LOD)和定量限(LOQ)较低,农药的检出限(LOD)和定量限(LOQ)分别为 0.020 至 0.045 µg l-1 和 0.045 至 1.0 µg l-1,抗生素的检出限(LOD)和定量限(LOQ)分别为 5 至 15 µg l-1 和 15 至 20 µg l-1。真实值在 82 % 至 109 % 之间。使用 AGREEprep 和绿色分析程序指数 (GAPI) 方法确认了该方法的绿色证书,突出了吸附剂的可重复使用性(超过 15 次)和快速分析吞吐量(每个样品 5 分钟),且预处理样品提取物用量少(500 µL)。对当地玉米、番茄和牛奶样品的应用证实,在分析的三个样品中,有一个番茄和一个玉米样品的噻虫嗪和阿特拉津的检测和定量浓度超过了建议的每日摄入量。此外,在 MEPS 方案中使用新型 SiGO@CS 生物吸附剂为传统吸附剂相提供了一种绿色、高性能的分析替代品,有望评估食品基质中痕量农药和抗生素的含量。
{"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
Determination of steroid hormones in sea urchins by microwave-assisted extraction and ultrahigh-performance liquid chromatography tandem mass spectrometry 微波辅助萃取和超高效液相色谱串联质谱法测定海胆中的类固醇激素
IF 5.2 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100132
Irene Rodríguez-de Cos , Raibel Núñez-González , Rayco Guedes-Alonso , Sarah Piaugeard , María Esther Torres-Padrón , José Juan Castro-Hernández , Zoraida Sosa-Ferrera , José Juan Santana-Rodríguez
Marine pollution poses significant threats to ecosystems by contaminating habitats and degrading marine life. This involves the need to develop efficient methodologies to evaluate the compounds that affect marine organisms, such as steroid hormones. The study of the presence of these compounds in marine organisms like sea urchins is very interesting given their role as bioindicators because they feed on algae and are constantly in contact with sediments. Given the low concentrations of steroid hormones in marine environments, it is necessary to develop extraction procedures that allow these pollutants to be extracted and preconcentrated before chemical analyses. Of all the extraction methods, microwave-assisted extraction (MAE) has been used for its many advantages compared to traditional extraction techniques, such as easy sample handling or scarce organic solvents use, and for providing very selective extractions. This study presents the novel MAE optimisation for the extraction of 15 hormones, including five oestrogens, three androgens, four progestogens and three glucocorticoids from sea urchin tissues. The extracted hormones were subsequently determined by high-performance liquid chromatography tandem mass spectrometry. To the best of the authors' knowledge, this approach has not been previously developed. To perform extraction optimisation, different variables were studied following factorial experimental designs. The optimised extraction method showed very appropriate analytical parameters, with limits of detection between 0.21 and 20.4 ng·g-1 for the four families of studied steroid hormones, and recovery extractions over 60 % for most target compounds. After optimisation, the analytical methodology was applied to samples of three different sea urchins species (Arbacia lixula, Paracentrotus lividus, Sphaerechinus granularis) caught in different locations around the Gran Canaria island (Canary Islands, Spain). The results showed the great applicability of the optimised methodology and two target hormones, boldenone and prednisolone, which were quantified in different samples and locations. This indicates the potential of sea urchins as bioindicators of the health of marine ecosystems and of anthropogenic contamination.
海洋污染会污染栖息地并使海洋生物退化,从而对生态系统构成重大威胁。这就需要开发有效的方法来评估影响海洋生物的化合物,如类固醇激素。由于海胆以藻类为食,并经常与沉积物接触,因此作为生物指示剂,研究这些化合物在海胆等海洋生物体内的存在非常有意义。由于海洋环境中的类固醇激素浓度较低,因此有必要开发萃取程序,以便在进行化学分析之前对这些污染物进行萃取和预浓缩。在所有萃取方法中,微波辅助萃取(MAE)因其与传统萃取技术相比的诸多优势而得到了广泛应用,如样品处理简便、有机溶剂用量少、萃取选择性强等。本研究介绍了从海胆组织中提取 15 种激素(包括 5 种雌激素、3 种雄激素、4 种孕激素和 3 种糖皮质激素)的新型 MAE 优化方法。提取的激素随后通过高效液相色谱串联质谱法进行测定。据作者所知,这种方法以前从未开发过。为了对萃取进行优化,采用因子实验设计对不同的变量进行了研究。优化后的萃取方法显示出非常合适的分析参数,对所研究的四个甾体激素家族的检测限在 0.21 至 20.4 纳克-克-1 之间,对大多数目标化合物的萃取回收率超过 60%。经过优化后,该分析方法被应用于在大加那利岛(西班牙加那利群岛)附近不同地点捕获的三种不同海胆(Arbacia lixula、Paracentrotus lividus、Sphaerechinus granularis)样本。结果表明,优化方法和两种目标荷尔蒙(勃地酮和泼尼松龙)的适用性很强,可在不同的样本和地点进行定量分析。这表明海胆具有作为海洋生态系统健康和人为污染的生物指标的潜力。
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引用次数: 0
One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD 通过 HPLC-FLD 一步衍生化和可切换亲水性溶剂微萃取法测定人体尿液中的金刚烷类似物
IF 5.2 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-01 DOI: 10.1016/j.sampre.2024.100135
Marianna Ntorkou , Paraskevas D. Tzanavaras , Constantinos K. Zacharis
The present study describes an “one-step” derivatization and microextraction using a pH-switchable hydrophilicity solvent for the determination of amantadine and memantine in human urine by liquid chromatography and fluorescence detection. The procedure is based on the derivatization of the analytes with o-phthalaldehyde/N-acetyl cysteine at alkaline conditions in the presence of sodium salicylate as extractant in a homogeneous solution. The liquid-solid transition of salicylic acid was achieved by adding an aliquot of concentrated phosphoric acid that enables efficient dispersion and phase separation in a single step. Due to the moderate melting point of salicylic acid, its solidification is carried out at room temperature without the need for sample cooling. Critical parameters affecting the efficiency of the derivatization reaction and the microextraction performance were investigated and optimized. The fluorescent analyte derivatives were monitored at λex/λem = 340/450 nm. The proposed method was validated in terms of specificity, linearity, precision and trueness. The method was linear in the range of 50–2000 ng mL−1 while the intraday and between days precision was less than 13.7% in all cases. The trueness of the method ranged between 87.9 and 113%. The green character and the applicability of the method were assessed using ComplexMoGAPI and BAGI tools. The developed analytical scheme presented satisfactory performance, and it could be applied in the analysis of selected drugs in human urine samples.
本研究介绍了一种 "一步法 "衍生化和微萃取方法,使用一种 pH 值可调的亲水性溶剂,通过液相色谱法和荧光检测法测定人体尿液中的金刚烷胺和美金刚。该方法是在碱性条件下,以水杨酸钠为萃取剂,在均匀溶液中用邻苯二甲醛/N-乙酰半胱氨酸对被分析物进行衍生。水杨酸的液固转换是通过加入等量的浓磷酸实现的,这样就能在一个步骤中实现高效的分散和相分离。由于水杨酸的熔点适中,其凝固过程可在室温下进行,无需冷却样品。对影响衍生反应效率和微萃取性能的关键参数进行了研究和优化。在 λex/λem = 340/450 纳米波长下监测荧光分析衍生物。所提议的方法在特异性、线性、精密度和真实性方面都得到了验证。该方法在 50-2000 ng mL-1 范围内线性良好,日内和日间精密度均小于 13.7%。该方法的准确度在 87.9%和 113%之间。使用ComplexMoGAPI和BAGI工具对该方法的绿色特性和适用性进行了评估。所开发的分析方案性能令人满意,可用于人体尿样中特定药物的分析。
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引用次数: 0
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