Advances in Sample Preparation最新文献_第2页

Hydrophobic and aromatic polymer nanofibers for a spin-filter micro solid phase extraction of polycyclic aromatic hydrocarbons in river water 疏水和芳香族聚合物纳米纤维用于自旋过滤微固相萃取河水中的多环芳烃

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2026-01-27 DOI: 10.1016/j.sampre.2026.100229

Ewelina Czyz , Marie Štorková , Jakub Erben , Pavel Holec , František Švec , Dalibor Šatínský

The use of hydrophobic and aromatic polymer nanofibers as novel sorbents for extracting polycyclic aromatic hydrocarbons (PAHs) from river water has been evaluated. Of the materials tested, the biodegradable aliphatic polymer polycaprolactone (PCL) exhibited strong retention of all analytes via hydrophobic interactions. In contrast, the aromatic polymer polyphenylene sulfide (PPS) demonstrated superior performance with higher-ring PAHs due to a combination of hydrophobic and π–π stacking interactions. The porous, permeable structure of the fibrous sorbents enabled rapid extraction. The spin-filter µSPE format required only 10 s for sorbent activation, extraction, and elution, resulting in a total processing time of 30 s per sample. Up to 48 samples could be processed simultaneously, reducing manual handling and simplifying the workflow. Analytical performance was evaluated using river water spiked at different concentration levels. The method showed good linearity (R² ≥ 0.98) across concentration ranges of 0.1–5 µg L⁻¹ for most analytes, with limits of detection of 0.009–0.14 µg L⁻¹ for PCL and 0.012–0.27 µg L⁻¹ for PPS. Recoveries ranged from 57 to 102 % for PCL and 88–139 % for PPS, with relative standard deviations below 15 %, and preconcentration factors of approximately twofold. These results demonstrate that meltblown PCL and PPS nanofibers combined with spin-filter µSPE provide a rapid and practical approach to extracting PAHs from environmental water samples.

研究了疏水性和芳香族聚合物纳米纤维作为新型吸附剂对水中多环芳烃（PAHs）的吸附性能。在所测试的材料中，可生物降解的脂肪族聚合物聚己内酯（PCL）通过疏水相互作用表现出对所有分析物的强保留。相比之下，芳香族聚合物聚苯硫醚（PPS）由于疏水和π -π堆叠相互作用的结合，在高环多环芳烃中表现出优越的性能。纤维吸附剂的多孔、可渗透结构使其能够快速提取。自旋过滤器µSPE格式只需要10秒的吸附剂活化，提取和洗脱，导致每个样品的总处理时间为30秒。最多可同时处理48个样品，减少人工处理，简化工作流程。使用不同浓度水平的河水对分析性能进行了评估。该方法对大多数分析物在0.1-5µg L⁻¹的浓度范围内表现出良好的线性（R²≥0.98），PCL的检测限为0.009-0.14µg L⁻¹，PPS的检测限为0.012-0.27µg L⁻¹。PCL加样回收率为57 ~ 102%，PPS加样回收率为88 ~ 139%，相对标准偏差小于15%，富集系数约为2倍。这些结果表明，熔喷PCL和PPS纳米纤维结合自旋过滤器µSPE可以快速实用地从环境水样中提取多环芳烃。

{"title":"Hydrophobic and aromatic polymer nanofibers for a spin-filter micro solid phase extraction of polycyclic aromatic hydrocarbons in river water","authors":"Ewelina Czyz , Marie Štorková , Jakub Erben , Pavel Holec , František Švec , Dalibor Šatínský","doi":"10.1016/j.sampre.2026.100229","DOIUrl":"10.1016/j.sampre.2026.100229","url":null,"abstract":"<div><div>The use of hydrophobic and aromatic polymer nanofibers as novel sorbents for extracting polycyclic aromatic hydrocarbons (PAHs) from river water has been evaluated. Of the materials tested, the biodegradable aliphatic polymer polycaprolactone (PCL) exhibited strong retention of all analytes via hydrophobic interactions. In contrast, the aromatic polymer polyphenylene sulfide (PPS) demonstrated superior performance with higher-ring PAHs due to a combination of hydrophobic and π–π stacking interactions. The porous, permeable structure of the fibrous sorbents enabled rapid extraction. The spin-filter µSPE format required only 10 s for sorbent activation, extraction, and elution, resulting in a total processing time of 30 s per sample. Up to 48 samples could be processed simultaneously, reducing manual handling and simplifying the workflow. Analytical performance was evaluated using river water spiked at different concentration levels. The method showed good linearity (R² ≥ 0.98) across concentration ranges of 0.1–5 µg L⁻¹ for most analytes, with limits of detection of 0.009–0.14 µg L⁻¹ for PCL and 0.012–0.27 µg L⁻¹ for PPS. Recoveries ranged from 57 to 102 % for PCL and 88–139 % for PPS, with relative standard deviations below 15 %, and preconcentration factors of approximately twofold. These results demonstrate that meltblown PCL and PPS nanofibers combined with spin-filter µSPE provide a rapid and practical approach to extracting PAHs from environmental water samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100229"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146077374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A novel automated micro solid phase extraction (µSPE) method to quantify 21 per- and polyfluoroalkyl substances compounds in biological samples 一种新型的自动化微固相萃取（µSPE）方法，用于定量生物样品中的21个单氟烷基和多氟烷基物质化合物

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2026-01-30 DOI: 10.1016/j.sampre.2026.100230

Gong Zhang , Adam Wawrzynczak , Grace Tseng , Amélie Blais , Andy Nong , Azam F. Tayabali , Guillaume Pelletier , Allison Loan , David Prescott , Kristin M. Eccles , Rocio Aranda-Rodriguez

A semi-automated micro solid-phase extraction (μSPE) method has been developed and optimized for the quantification of 21 per- and polyfluoroalkyl substances (PFAS) across various biological matrices, including plasma, serum, urine, and liver tissue. This method employed μSPE cartridges integrated with a PAL-RTC robotic system, which enabled precise flow control and high-throughput procedures while ensuring exceptional extraction efficiency and reproducibility. Sample homogenization of liver tissues was achieved by bead-mill technology which eliminated sample cross-contamination and significantly reduced processing time. The extraction efficiency was influenced by the concentration of methanol in the sample, especially for longer-chain PFAS (C9–14). Extraction efficiencies of over 90% extraction were achieved with loading solutions containing 50–60% methanol in plasma and serum, and up to 80% methanol in water samples. The μSPE protocol included two sequential wash steps that provided excellent matrix clean-up, and reduced background signals by over 95% compared to traditional protein precipitation (PP) methods. The µSPE-LC-MS/MS method offers high sensitivity (method detection limits between 0.008 ng/mL and 0.048 ng/mL), along with good recoveries (90.3 to 105.1%), and precision (RSD <10%). It also demonstrated strong agreement with non-certified values of NIST Standard Reference Materials (SRM 1957/1958). The method was successfully used in the analysis of PFAS in human urine and plasma, as well as in mouse liver samples from an in vivo study. The μSPE approach provides a sensitive, reproducible, and automated solution that requires limited biological sample volumes, making it suitable for the analysis of PFAS in biomonitoring and toxicokinetic studies.

建立了一种半自动化微固相萃取（μSPE）方法，并对其进行了优化，该方法可用于测定血浆、血清、尿液和肝组织等多种生物基质中的21种全氟烷基和多氟烷基物质（PFAS）。该方法采用集成了PAL-RTC机器人系统的μSPE萃取管，在保证萃取效率和重现性的同时，实现了精确的流量控制和高通量程序。肝脏组织的样品均质是通过球磨技术实现的，消除了样品的交叉污染，大大缩短了处理时间。萃取效率受样品中甲醇浓度的影响，特别是对长链PFAS （C9-14）。在血浆和血清中含有50-60%的甲醇，在水样中含有高达80%的甲醇时，萃取效率达到90%以上。μSPE协议包括两个顺序洗涤步骤，提供了出色的基质清理，与传统的蛋白质沉淀（PP）方法相比，减少了95%以上的背景信号。该方法灵敏度高（检测限为0.008 ~ 0.048 ng/mL），加样回收率（90.3 ~ 105.1%），精密度（RSD <10%）。它还显示了与NIST标准参考物质（SRM 1957/1958）的非认证值的强烈一致性。该方法已成功地用于分析人类尿液和血浆中的PFAS，以及小鼠肝脏样本的体内研究。μSPE方法提供了一种敏感、可重复和自动化的解决方案，需要有限的生物样本量，使其适用于生物监测和毒物动力学研究中的PFAS分析。

{"title":"A novel automated micro solid phase extraction (µSPE) method to quantify 21 per- and polyfluoroalkyl substances compounds in biological samples","authors":"Gong Zhang , Adam Wawrzynczak , Grace Tseng , Amélie Blais , Andy Nong , Azam F. Tayabali , Guillaume Pelletier , Allison Loan , David Prescott , Kristin M. Eccles , Rocio Aranda-Rodriguez","doi":"10.1016/j.sampre.2026.100230","DOIUrl":"10.1016/j.sampre.2026.100230","url":null,"abstract":"<div><div>A semi-automated micro solid-phase extraction (μSPE) method has been developed and optimized for the quantification of 21 per- and polyfluoroalkyl substances (PFAS) across various biological matrices, including plasma, serum, urine, and liver tissue. This method employed μSPE cartridges integrated with a PAL-RTC robotic system, which enabled precise flow control and high-throughput procedures while ensuring exceptional extraction efficiency and reproducibility. Sample homogenization of liver tissues was achieved by bead-mill technology which eliminated sample cross-contamination and significantly reduced processing time. The extraction efficiency was influenced by the concentration of methanol in the sample, especially for longer-chain PFAS (C9–14). Extraction efficiencies of over 90% extraction were achieved with loading solutions containing 50–60% methanol in plasma and serum, and up to 80% methanol in water samples. The μSPE protocol included two sequential wash steps that provided excellent matrix clean-up, and reduced background signals by over 95% compared to traditional protein precipitation (PP) methods. The µSPE-LC-MS/MS method offers high sensitivity (method detection limits between 0.008 ng/mL and 0.048 ng/mL), along with good recoveries (90.3 to 105.1%), and precision (RSD <10%). It also demonstrated strong agreement with non-certified values of NIST Standard Reference Materials (SRM 1957/1958). The method was successfully used in the analysis of PFAS in human urine and plasma, as well as in mouse liver samples from an <em>in vivo</em> study. The μSPE approach provides a sensitive, reproducible, and automated solution that requires limited biological sample volumes, making it suitable for the analysis of PFAS in biomonitoring and toxicokinetic studies.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100230"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147394986","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Green hydrophobic deep eutectic solvent-based rapid synergistic cloud point extraction and quantification of ultra-trace lead 绿色疏水深共晶溶剂基快速协同云点萃取及超痕量铅定量

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-11-19 DOI: 10.1016/j.sampre.2025.100225

Ingrid Hagarová , Vasil Andruch , Alina Kalyniukova

In this study, a novel and environmentally friendly analytical procedure was developed for the fast separation and preconcentration of ultra-trace levels of lead from water samples at room temperature. The method is based on a hydrophobic deep eutectic solvent–assisted rapid synergistic cloud point extraction (HDES-RS-CPE), followed by electrothermal atomic absorption spectrometry (ETAAS) for quantification. The selected HDES was composed of l-menthol and 1-octanol in a 1:1 molar ratio, while ammonium pyrrolidine dithiocarbamate (APDC) and Triton X-114 were employed as the chelating agent and nonionic surfactant, respectively. Key experimental parameters influencing extraction efficiency were systematically investigated and optimized. Under optimal conditions, the method achieved a limit of detection (LOD) of 0.04 µg/L, a limit of quantification (LOQ) of 0.12 µg/L, and an enrichment factor (EF) of 38, with spike recoveries ranging from 94 % to 104 %. The method’s greenness, practicality and robustness were confirmed using various metrics demonstrated compliance with the principles of Green Analytical Chemistry, highlighting the method’s potential as a sustainable and efficient approach for ultra-trace lead quantification in environmental samples.

在本研究中，开发了一种新的环境友好的分析方法，用于在室温下快速分离和富集水样中的超痕量铅。该方法基于疏水深共晶溶剂辅助快速协同云点萃取（HDES-RS-CPE），然后采用电热原子吸收光谱法（ETAAS）进行定量。选用l-薄荷醇和1-辛醇以1:1的摩尔比组成HDES，吡咯烷二硫代氨基甲酸铵（APDC）和Triton X-114分别作为螯合剂和非离子表面活性剂。对影响萃取效率的关键实验参数进行了系统研究和优化。在最佳条件下，该方法的检出限为0.04µg/L，定量限为0.12µg/L，富集因子为38，峰回收率为94% ~ 104%。该方法的绿色、实用性和稳健性得到了各种指标的证实，这些指标符合绿色分析化学的原则，突出了该方法作为环境样品中超痕量铅定量的可持续和有效方法的潜力。

{"title":"Green hydrophobic deep eutectic solvent-based rapid synergistic cloud point extraction and quantification of ultra-trace lead","authors":"Ingrid Hagarová , Vasil Andruch , Alina Kalyniukova","doi":"10.1016/j.sampre.2025.100225","DOIUrl":"10.1016/j.sampre.2025.100225","url":null,"abstract":"<div><div>In this study, a novel and environmentally friendly analytical procedure was developed for the fast separation and preconcentration of ultra-trace levels of lead from water samples at room temperature. The method is based on a hydrophobic deep eutectic solvent–assisted rapid synergistic cloud point extraction (HDES-RS-CPE), followed by electrothermal atomic absorption spectrometry (ETAAS) for quantification. The selected HDES was composed of <span>l</span>-menthol and 1-octanol in a 1:1 molar ratio, while ammonium pyrrolidine dithiocarbamate (APDC) and Triton X-114 were employed as the chelating agent and nonionic surfactant, respectively. Key experimental parameters influencing extraction efficiency were systematically investigated and optimized. Under optimal conditions, the method achieved a limit of detection (LOD) of 0.04 µg/L, a limit of quantification (LOQ) of 0.12 µg/L, and an enrichment factor (EF) of 38, with spike recoveries ranging from 94 % to 104 %. The method’s greenness, practicality and robustness were confirmed using various metrics demonstrated compliance with the principles of Green Analytical Chemistry, highlighting the method’s potential as a sustainable and efficient approach for ultra-trace lead quantification in environmental samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100225"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145623498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Recovery of proteins and bioactive compounds from turmeric (Curcuma longa) and ginger (Zingibber officinale) wastes using sustainable extraction techniques. Tentative identification of main extracted compounds by UHPLC-Q-TOF-MS/MS 利用可持续提取技术从姜黄（Curcuma longa）和姜（Zingibber officinale）废料中回收蛋白质和生物活性化合物。UHPLC-Q-TOF-MS/MS对主要提取物进行初步鉴定

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-09-13 DOI: 10.1016/j.sampre.2025.100213

Rubio-Marín Carlos , María Luisa Marina , María Concepción García

Ginger and turmeric are spices increasingly employed in juice production due to their outstanding composition and health benefits. This practice results in wastes that, like whole spices, likely constitute a cheap and sustainable source of proteins, as well as antioxidant and antimicrobial compounds, whose recovery has not yet been proposed. This work aims to evaluate low environmental impact techniques to make the most of these wastes: high-intensity focused ultrasounds (HIFU), subcritical water extraction (SWE), and enzyme-assisted extraction (EAE). In all cases, water was used as extracting solvent and experimental design chemometric tools (Box-Behnken and factorial 3² design) were employed to maximize the recovery of proteins, antioxidants, and antimicrobial compounds, while minimizing the formation of potentially harmful Maillard products during extraction. HIFU demonstrated a greater capability for extracting proteins, which increased significantly when combined with EAE using a polysaccharidase enzyme. The largest protein extraction was achieved from the ginger extract using HIFU for 18 min, at 60 ºC and 80 % amplitude, combined with EAE using Celluclast enzyme. The extracts obtained using SWE showed significant antioxidant activity, with a slight improvement observed when using 2 cycles instead of one. The highest antioxidant activity was observed in the extract obtained from the turmeric waste using SWE at 175 ºC for 15 min. The extracts also exhibited antimicrobial activity, especially against Staphylococcus aureus, highlighting the minimum inhibitory concentration obtained from the turmeric waste extract using SWE at 155 ºC for 9 min (0.15 mg/mL). The extracts showing the highest antioxidant or antimicrobial activity were analyzed by ultrahigh-performance liquid chromatography coupled to high-resolution tandem mass spectrometry for the tentative identification of main compounds responsible for the observed activities. Phenolic compounds, such as 6-gingerol and its derivatives in ginger waste extracts, and curcuminoids in turmeric waste extracts, were tentatively identified as the predominant constituents.

生姜和姜黄由于其出色的成分和健康益处而越来越多地用于果汁生产。这种做法产生的废物，就像整个香料一样，可能构成廉价和可持续的蛋白质来源，以及抗氧化和抗菌化合物，其回收尚未提出。这项工作旨在评估低环境影响技术，以充分利用这些废物：高强度聚焦超声（HIFU）、亚临界水提取（SWE）和酶辅助提取（EAE）。在所有情况下，均使用水作为提取溶剂，并采用实验设计化学测量工具（Box-Behnken和析因32设计）来最大限度地回收蛋白质、抗氧化剂和抗菌化合物，同时最大限度地减少提取过程中潜在有害美拉德产物的形成。HIFU显示出更大的蛋白质提取能力，当使用多糖酶与EAE联合使用时，蛋白质提取能力显著提高。在60ºC和80%振幅下，HIFU作用18 min，结合使用Celluclast酶的EAE，从姜提取物中提取的蛋白质最多。SWE提取的提取物具有显著的抗氧化活性，当使用2个周期而不是1个周期时，其抗氧化活性略有提高。从姜黄废料中提取的抗氧化活性最高，SWE在175℃下加热15 min。该提取物还显示出抗菌活性，特别是对金黄色葡萄球菌，突出显示姜黄废物提取物在155ºC下使用SWE处理9分钟（0.15 mg/mL）获得的最低抑制浓度。采用高效液相色谱联用高分辨率串联质谱法对抗氧化或抗菌活性最高的提取物进行了分析，初步确定了主要活性成分。初步确定了生姜提取物中的6-姜辣素及其衍生物和姜黄素等酚类化合物为主要成分。

{"title":"Recovery of proteins and bioactive compounds from turmeric (Curcuma longa) and ginger (Zingibber officinale) wastes using sustainable extraction techniques. Tentative identification of main extracted compounds by UHPLC-Q-TOF-MS/MS","authors":"Rubio-Marín Carlos , María Luisa Marina , María Concepción García","doi":"10.1016/j.sampre.2025.100213","DOIUrl":"10.1016/j.sampre.2025.100213","url":null,"abstract":"<div><div>Ginger and turmeric are spices increasingly employed in juice production due to their outstanding composition and health benefits. This practice results in wastes that, like whole spices, likely constitute a cheap and sustainable source of proteins, as well as antioxidant and antimicrobial compounds, whose recovery has not yet been proposed. This work aims to evaluate low environmental impact techniques to make the most of these wastes: high-intensity focused ultrasounds (HIFU), subcritical water extraction (SWE), and enzyme-assisted extraction (EAE). In all cases, water was used as extracting solvent and experimental design chemometric tools (Box-Behnken and factorial 3<sup>2</sup> design) were employed to maximize the recovery of proteins, antioxidants, and antimicrobial compounds, while minimizing the formation of potentially harmful Maillard products during extraction. HIFU demonstrated a greater capability for extracting proteins, which increased significantly when combined with EAE using a polysaccharidase enzyme. The largest protein extraction was achieved from the ginger extract using HIFU for 18 min, at 60 ºC and 80 % amplitude, combined with EAE using Celluclast enzyme. The extracts obtained using SWE showed significant antioxidant activity, with a slight improvement observed when using 2 cycles instead of one. The highest antioxidant activity was observed in the extract obtained from the turmeric waste using SWE at 175 ºC for 15 min. The extracts also exhibited antimicrobial activity, especially against <em>Staphylococcus aureus</em>, highlighting the minimum inhibitory concentration obtained from the turmeric waste extract using SWE at 155 ºC for 9 min (0.15 mg/mL). The extracts showing the highest antioxidant or antimicrobial activity were analyzed by ultrahigh-performance liquid chromatography coupled to high-resolution tandem mass spectrometry for the tentative identification of main compounds responsible for the observed activities. Phenolic compounds, such as 6-gingerol and its derivatives in ginger waste extracts, and curcuminoids in turmeric waste extracts, were tentatively identified as the predominant constituents.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100213"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145106276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Compatibility of NADES and ABS with CE-SDS analysis of bovine milk proteins NADES和ABS与牛乳蛋白CE-SDS分析的相容性

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-10-31 DOI: 10.1016/j.sampre.2025.100222

Cristian Gonzalez-Jimenez, Paula Tejedor-Matellanes, Mercedes de Frutos, Angel Puerta

The rising interest in studying milk proteins is due to several factors such as the food supplement consumption based on them and the circular economy of the whey obtained as a byproduct in the dairy industry. Modifications of the milk proteins, such as fragmentation, aggregation and denaturation happening during manufacturing need to be tightly controlled. In this work the use of an aqueous biphasic system (ABS) consisting of a natural deep eutectic solvent (NADES) and a salt to recover proteins from milk that could be applied to the extraction of milk proteins from byproducts in the dairy industry, was evaluated. As NADES betaine:urea:water (1:2:1 molar ratio) was employed. Back-extraction of milk proteins into water was evaluated by UV spectroscopy and by capillary electrophoresis with sodium dodecyl sulfate (CE-SDS). This study included the prior assessment of the usefulness of non-reducing CE-SDS method with laboratory-made gel-buffers for analyzing bovine caseins and whey proteins. Afterwards the compatibility of this CE method with the use of this NADES as protein solvent was established. The study allowed demonstrating that caseins as well as whey proteins mainly partition in the NADES-rich phase of the ABS, with recovery yield values higher than 77 %, extraction efficiencies higher than 97 % and back-extraction into water using centrifugal filter devices higher than 28 %. This work supports a procedure for recovering milk proteins from dairy industry byproducts using chemicals considered environmentally friendly. Sustainability of the ABS and back-extraction method was assessed using the AGREEprep tool. Besides the green characteristics of the sample preparation, the CE-SDS method established consumes a very low volume of sample and reagents and allows analyzing the individual caseins and whey proteins in less than 6 min as well as measuring the back-extraction recovery in water.

人们对研究牛奶蛋白的兴趣日益浓厚，这是由于几个因素，比如以牛奶蛋白为基础的食品补充剂消费，以及乳清作为乳制品工业副产品的循环经济。牛奶蛋白的修饰，如在生产过程中发生的破碎、聚集和变性，需要严格控制。在这项工作中，评估了由天然深共熔溶剂（NADES）和盐组成的双水相体系（ABS）从牛奶中回收蛋白质的应用，该体系可用于从乳制品工业的副产品中提取牛奶蛋白质。NADES采用甜菜碱：尿素：水（1:2:1）的摩尔比。采用紫外光谱法和毛细管电泳法对乳蛋白反提进行了评价。这项研究包括预先评估非还原CE-SDS方法与实验室自制的凝胶缓冲液分析牛酪蛋白和乳清蛋白的有效性。然后建立了该方法与NADES作为蛋白质溶剂的相容性。该研究表明，酪蛋白和乳清蛋白主要在ABS的富nades相分离，回收率高于77%，提取效率高于97%，使用离心过滤装置反提取到水中的效率高于28%。这项工作支持了一种使用环保化学品从乳制品工业副产品中回收牛奶蛋白的方法。使用AGREEprep工具评估ABS和反拔方法的可持续性。除了样品制备的绿色特性外，建立的CE-SDS方法消耗的样品和试剂体积非常小，可以在不到6分钟的时间内分析单个酪蛋白和乳清蛋白，并测量水中反萃取回收率。

{"title":"Compatibility of NADES and ABS with CE-SDS analysis of bovine milk proteins","authors":"Cristian Gonzalez-Jimenez, Paula Tejedor-Matellanes, Mercedes de Frutos, Angel Puerta","doi":"10.1016/j.sampre.2025.100222","DOIUrl":"10.1016/j.sampre.2025.100222","url":null,"abstract":"<div><div>The rising interest in studying milk proteins is due to several factors such as the food supplement consumption based on them and the circular economy of the whey obtained as a byproduct in the dairy industry. Modifications of the milk proteins, such as fragmentation, aggregation and denaturation happening during manufacturing need to be tightly controlled. In this work the use of an aqueous biphasic system (ABS) consisting of a natural deep eutectic solvent (NADES) and a salt to recover proteins from milk that could be applied to the extraction of milk proteins from byproducts in the dairy industry, was evaluated. As NADES betaine:urea:water (1:2:1 molar ratio) was employed. Back-extraction of milk proteins into water was evaluated by UV spectroscopy and by capillary electrophoresis with sodium dodecyl sulfate (CE-SDS). This study included the prior assessment of the usefulness of non-reducing CE-SDS method with laboratory-made gel-buffers for analyzing bovine caseins and whey proteins. Afterwards the compatibility of this CE method with the use of this NADES as protein solvent was established. The study allowed demonstrating that caseins as well as whey proteins mainly partition in the NADES-rich phase of the ABS, with recovery yield values higher than 77 %, extraction efficiencies higher than 97 % and back-extraction into water using centrifugal filter devices higher than 28 %. This work supports a procedure for recovering milk proteins from dairy industry byproducts using chemicals considered environmentally friendly. Sustainability of the ABS and back-extraction method was assessed using the AGREEprep tool. Besides the green characteristics of the sample preparation, the CE-SDS method established consumes a very low volume of sample and reagents and allows analyzing the individual caseins and whey proteins in less than 6 min as well as measuring the back-extraction recovery in water.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100222"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473711","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Ionic liquid-grafted aminosilica-graphene oxide sorbent for efficient microextraction by packed sorbent of multiclass pesticides in wine 离子液体接枝氨基硅-氧化石墨烯吸附剂对葡萄酒中多类农药的高效微萃取

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-10-13 DOI: 10.1016/j.sampre.2025.100217

Alessandra Timóteo Cardoso , Gloria Domínguez-Rodríguez , Alejandro Cifuentes , Fernando Mauro Lanças

Monitoring pesticide residues in wine is essential for ensuring food safety, as these compounds and their metabolites can persist in the final product and pose potential health risks. This study reports the development of a hybrid sorbent based on graphene oxide anchored to aminosilica particles (GO@Si), functionalized with ionic liquids (ILs) via direct anion-exchange. Among the tested combinations, GO@Si-[VHIm]⁺PF₆⁻ exhibited the best extraction performance due to its multiple interaction mechanisms with analytes. This sorbent was integrated into a microextraction by packed sorbent (MEPS) system for the extraction of six multiclass pesticides from wine, followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. After optimizing extraction conditions using univariate and multivariate approaches, the method demonstrated excellent linearity (r² ≥ 0.9958), satisfactory precision (RSDs < 15 %), and recoveries ranging from 49 % to 112 %. Limits of quantification were from 0.030 to 0.130 ng mL⁻¹, with negligible matrix effects in white, red, and rosé wines. The method also presented notable green advantages, including device reusability (up to six cycles) and low solvent consumption (0.7 mL per extraction). Sustainability assessments using AGREEprep and BAGI yielded favourable scores (0.52 and 57.5, respectively). This pilot study provides a promising and environmentally conscious analytical approach for multiclass pesticide monitoring in wines, with potential for further development into routine analysis.

监测葡萄酒中的农药残留对确保食品安全至关重要，因为这些化合物及其代谢物可能持续存在于最终产品中，并构成潜在的健康风险。本研究报告了一种基于氧化石墨烯锚定到氨基二氧化硅颗粒（GO@Si）的混合吸附剂的开发，通过直接阴离子交换与离子液体（ILs）功能化。在测试的组合中，GO@Si-[VHIm]⁺PF₆⁻由于与被测物的多重作用机制，表现出最好的萃取性能。将该吸附剂集成到包装吸附剂（MEPS）微萃取系统中，用于从葡萄酒中提取6种多类农药，并进行高效液相色谱-串联质谱（HPLC-MS/MS）分析。采用单因素和多因素优化提取条件，结果表明，该方法线性度高（r²≥0.9958），精密度高（rsd = 15%），加样回收率为49% ~ 112%。定量限为0.030 ~ 0.130 ng mL（毒血症），在白、红、红葡萄酒中基质效应可以忽略不计。该方法还具有显著的绿色优势，包括设备可重复使用（多达6次循环）和低溶剂消耗（每次提取0.7 mL）。使用AGREEprep和BAGI的可持续性评估获得了有利的分数（分别为0.52和57.5）。本初步研究为葡萄酒中多种农药的监测提供了一种有前景的、环保的分析方法，并有进一步发展为常规分析的潜力。

{"title":"Ionic liquid-grafted aminosilica-graphene oxide sorbent for efficient microextraction by packed sorbent of multiclass pesticides in wine","authors":"Alessandra Timóteo Cardoso , Gloria Domínguez-Rodríguez , Alejandro Cifuentes , Fernando Mauro Lanças","doi":"10.1016/j.sampre.2025.100217","DOIUrl":"10.1016/j.sampre.2025.100217","url":null,"abstract":"<div><div>Monitoring pesticide residues in wine is essential for ensuring food safety, as these compounds and their metabolites can persist in the final product and pose potential health risks. This study reports the development of a hybrid sorbent based on graphene oxide anchored to aminosilica particles (GO@Si), functionalized with ionic liquids (ILs) via direct anion-exchange. Among the tested combinations, GO@Si-[VHIm]⁺PF₆⁻ exhibited the best extraction performance due to its multiple interaction mechanisms with analytes. This sorbent was integrated into a microextraction by packed sorbent (MEPS) system for the extraction of six multiclass pesticides from wine, followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. After optimizing extraction conditions using univariate and multivariate approaches, the method demonstrated excellent linearity (r² ≥ 0.9958), satisfactory precision (RSDs < 15 %), and recoveries ranging from 49 % to 112 %. Limits of quantification were from 0.030 to 0.130 ng mL⁻¹, with negligible matrix effects in white, red, and rosé wines. The method also presented notable green advantages, including device reusability (up to six cycles) and low solvent consumption (0.7 mL per extraction). Sustainability assessments using AGREEprep and BAGI yielded favourable scores (0.52 and 57.5, respectively). This pilot study provides a promising and environmentally conscious analytical approach for multiclass pesticide monitoring in wines, with potential for further development into routine analysis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100217"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145362225","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Introducing a modified sample preparation and straightforward elemental ratio determination strategy with LA-ICP-MS to expand the nanoparticle probing toolkit 引入改进的样品制备和直接元素比测定策略与LA-ICP-MS扩展纳米颗粒探测工具箱

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-11-02 DOI: 10.1016/j.sampre.2025.100223

Olga Lanaridi , Yan Chen , Jakob Nils Blaschke , Pablo Ayala , Bernhard C. Bayer , Dominik Eder , Andreas Limbeck

Nanoparticles (NPs) are employed in a wide range of applications due to some of their unique characteristics. Since their properties are partly determined by their composition, accurate determination of their stoichiometry is of paramount importance for optimization and fine tuning of their properties.

We propose a laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) procedure which enables determination of NP composition. Small NP quantities (approx. 1 mg) are dispersed in a polymeric solution which is then spin coated onto a Si wafer, thereby ensuring uniform distribution of the NPs within the thin polymer film deposited on the Si substrate. Matrix-matched standards are similarly prepared by mixing elemental aqueous stock solutions with the same polymer solution, followed by spin coating.

After thorough optimization of the sample preparation, and the parameters used for laser-ablation and subsequent ICP-MS analysis, the content of the analytes could be determined with a relative standard deviation (RSD) of < 2 % for standards and < 3–8 % for the NP samples, depending on the NP type, with detection limits lower than 0.2000 µg/g for all elements. Based on the results determined for the individual NP constituents, prevailing elemental ratios have been assessed.

Yttria-doped zirconia of known stoichiometry, i.e., (ZrO₂)_0.98(Y₂O₃)_0.08, was used as a reference material to validate the fit of the developed approach for the stoichiometric determination of NPs. The experimentally determined stoichiometry is in agreement with the one provided by the manufacturer. The applicability of the method is further demonstrated by assessment of the loading of CdS rods with medium-entropy (CoNiMoW)S NPs, which are interesting as novel catalysts and stoichiometric determination of Zr-based metal organic frameworks (MOFs), which function as catalysts in CO₂ reduction.

纳米粒子（NPs）由于其一些独特的特性而被广泛应用。由于它们的性质部分是由它们的组成决定的，因此准确测定它们的化学计量对于优化和微调它们的性质至关重要。我们提出了一种激光烧蚀-电感耦合等离子体质谱（LA-ICP-MS）程序，可以确定NP组成。小的NP数量(大约。1毫克)分散在聚合物溶液中，然后自旋涂覆在硅晶片上，从而确保NPs在沉积在硅衬底上的薄聚合物薄膜内均匀分布。基质匹配的标准品同样是通过将元素水原液与相同的聚合物溶液混合，然后进行旋转涂层来制备的。经过对样品制备、激光烧蚀及后续ICP-MS分析参数的全面优化，根据NP类型，标准样品的相对标准偏差（RSD）为2%，NP样品的相对标准偏差（RSD）为3 - 8%，所有元素的检出限均低于0.2000µg/g。根据对单个NP成分确定的结果，评估了普遍的元素比率。以已知化学计量的氧化锆（ZrO2）0.98(Y2O3)0.08作为对照物质，验证了该方法测定NPs化学计量的拟合性。实验测定的化学计量与厂家提供的一致。该方法的适用性通过评估具有中熵（CoNiMoW）S NPs的CdS棒的负载以及化学计量学测定作为CO2还原催化剂的zr基金属有机框架（mof）进一步得到验证。

{"title":"Introducing a modified sample preparation and straightforward elemental ratio determination strategy with LA-ICP-MS to expand the nanoparticle probing toolkit","authors":"Olga Lanaridi , Yan Chen , Jakob Nils Blaschke , Pablo Ayala , Bernhard C. Bayer , Dominik Eder , Andreas Limbeck","doi":"10.1016/j.sampre.2025.100223","DOIUrl":"10.1016/j.sampre.2025.100223","url":null,"abstract":"<div><div>Nanoparticles (NPs) are employed in a wide range of applications due to some of their unique characteristics. Since their properties are partly determined by their composition, accurate determination of their stoichiometry is of paramount importance for optimization and fine tuning of their properties.</div><div>We propose a laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) procedure which enables determination of NP composition. Small NP quantities (approx. 1 mg) are dispersed in a polymeric solution which is then spin coated onto a Si wafer, thereby ensuring uniform distribution of the NPs within the thin polymer film deposited on the Si substrate. Matrix-matched standards are similarly prepared by mixing elemental aqueous stock solutions with the same polymer solution, followed by spin coating.</div><div>After thorough optimization of the sample preparation, and the parameters used for laser-ablation and subsequent ICP-MS analysis, the content of the analytes could be determined with a relative standard deviation (RSD) of < 2 % for standards and < 3–8 % for the NP samples, depending on the NP type, with detection limits lower than 0.2000 µg/g for all elements. Based on the results determined for the individual NP constituents, prevailing elemental ratios have been assessed.</div><div>Yttria-doped zirconia of known stoichiometry, i.e., (ZrO<sub>2</sub>)<sub>0.98</sub>(Y<sub>2</sub>O<sub>3</sub>)<sub>0.08</sub>, was used as a reference material to validate the fit of the developed approach for the stoichiometric determination of NPs. The experimentally determined stoichiometry is in agreement with the one provided by the manufacturer. The applicability of the method is further demonstrated by assessment of the loading of CdS rods with medium-entropy (CoNiMoW)S NPs, which are interesting as novel catalysts and stoichiometric determination of Zr-based metal organic frameworks (MOFs), which function as catalysts in CO<sub>2</sub> reduction.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100223"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145528670","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Sorbent-less dried blood spot microsampling 无吸附剂干血斑显微取样

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-10-29 DOI: 10.1016/j.sampre.2025.100221

Miloš Dvořák , Sylvie Profousová , Pavel Kubáň

Dried blood spots (DBSs) are typically sampled on porous sorbents, which may retain analytes in their structure during DBS rehydration but also release various species into the eluates and contaminate them. To eliminate the eluate contamination, a novel concept for sorbent-less DBS microsampling was suggested, and a comprehensive study was carried out investigating the effect of the novel and the standard DBS sampling procedures on the contamination. In the novel concept, a small drop of capillary blood with a known volume was quantitatively pipetted into a non-porous polypropylene vial (compatible with capillary electrophoresis (CE) instruments for subsequent analysis) without being absorbed by any sorbent. All procedures, including DBS sampling, drying, rehydration, and homogenization, were done directly in-vial, and the blood drying time was < 3 h. By neglecting the porous sorbent, contamination of the resulting DBS eluates by sorbent-borne species was eliminated, which was demonstrated by the CE determination of inorganic cations/anions and organic anions. The ionic composition of the rehydrated sorbent-less DBSs showed no statistical difference from the original liquid capillary blood. On the contrary, all commercial sorbents released considerable levels of ions into the eluates (Ca²⁺, Mg²⁺, Na⁺ and Cl^-, NO₃^-, SO₄^2-, HCOO^- being the major cationic and anionic contaminants, respectively), resulting in up to 3.5-fold higher concentrations in standard vs. sorbent-less DBS samples and having a detrimental effect on quantitative DBS analyses. Moreover, additional ionic contamination was observed for DBSs sampled on pre-impregnated sorbents and/or by volumetric devices treated with anticoagulants. Consequently, a simple, precise, and accurate procedure was presented for sorbent-less DBS microsampling in medical as well as patient-centric conditions. The most convenient and economical DBS sampling was achieved by a low-cost micropipette with adjustable volume, resulting in precision and accuracy of ≤ 1.7 and 1.4%, respectively, for quantitative blood transfers, and CE analyses repeatability of ≤ 7.2%, after the whole DBS processing.

干血斑（DBS）通常在多孔吸附剂上取样，在DBS再水化过程中，这种吸附剂可能保留分析物的结构，但也会释放各种物质到洗脱液中并污染它们。为了消除洗脱液污染，提出了一种无吸附剂DBS微采样的新概念，并对新型DBS采样程序和标准DBS采样程序对污染的影响进行了全面研究。在这个新概念中，一小滴已知体积的毛细管血被定量地移液到一个无孔聚丙烯小瓶中（与毛细管电泳（CE）仪器兼容，用于后续分析），而不被任何吸附剂吸收。所有步骤，包括DBS取样、干燥、复水化和均质，都是直接在瓶中完成的，血液干燥时间为3小时。通过忽略多孔吸附剂，消除了吸收剂携带的物质对所得DBS洗脱物的污染，无机阳离子/阴离子和有机阴离子的CE测定证明了这一点。再水合无吸附剂DBSs的离子组成与原始液体毛细血管血无统计学差异。相反，所有商业吸附剂释放相当水平的离子到洗脱物中（Ca2+, Mg2+， Na+和Cl-， NO3-, SO42-， HCOO-分别是主要的阳离子和阴离子污染物），导致标准DBS样品中的浓度比无吸附剂的高3.5倍，并对DBS定量分析产生不利影响。此外，在预浸渍吸附剂和/或经抗凝剂处理的体积装置上取样的DBSs观察到额外的离子污染。因此，提出了一种简单、精确和准确的程序，用于医疗和以患者为中心的条件下的无吸附剂DBS微采样。DBS取样最方便、最经济的方法是使用低成本、可调节体积的微移管，定量输血的精密度和准确度分别≤1.7和1.4%，整个DBS处理后CE分析的重复性≤7.2%。

{"title":"Sorbent-less dried blood spot microsampling","authors":"Miloš Dvořák , Sylvie Profousová , Pavel Kubáň","doi":"10.1016/j.sampre.2025.100221","DOIUrl":"10.1016/j.sampre.2025.100221","url":null,"abstract":"<div><div>Dried blood spots (DBSs) are typically sampled on porous sorbents, which may retain analytes in their structure during DBS rehydration but also release various species into the eluates and contaminate them. To eliminate the eluate contamination, a novel concept for sorbent-less DBS microsampling was suggested, and a comprehensive study was carried out investigating the effect of the novel and the standard DBS sampling procedures on the contamination. In the novel concept, a small drop of capillary blood with a known volume was quantitatively pipetted into a non-porous polypropylene vial (compatible with capillary electrophoresis (CE) instruments for subsequent analysis) without being absorbed by any sorbent. All procedures, including DBS sampling, drying, rehydration, and homogenization, were done directly in-vial, and the blood drying time was < 3 h. By neglecting the porous sorbent, contamination of the resulting DBS eluates by sorbent-borne species was eliminated, which was demonstrated by the CE determination of inorganic cations/anions and organic anions. The ionic composition of the rehydrated sorbent-less DBSs showed no statistical difference from the original liquid capillary blood. On the contrary, all commercial sorbents released considerable levels of ions into the eluates (Ca<sup>2+</sup>, Mg<sup>2+</sup>, Na<sup>+</sup> and Cl<sup>-</sup>, NO<sub>3</sub><sup>-</sup>, SO<sub>4</sub><sup>2-</sup>, HCOO<sup>-</sup> being the major cationic and anionic contaminants, respectively), resulting in up to 3.5-fold higher concentrations in standard vs. sorbent-less DBS samples and having a detrimental effect on quantitative DBS analyses. Moreover, additional ionic contamination was observed for DBSs sampled on pre-impregnated sorbents and/or by volumetric devices treated with anticoagulants. Consequently, a simple, precise, and accurate procedure was presented for sorbent-less DBS microsampling in medical as well as patient-centric conditions. The most convenient and economical DBS sampling was achieved by a low-cost micropipette with adjustable volume, resulting in precision and accuracy of ≤ 1.7 and 1.4%, respectively, for quantitative blood transfers, and CE analyses repeatability of ≤ 7.2%, after the whole DBS processing.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100221"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473710","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Versatile sorbent materials in sample preparation: Where do we go next? 样品制备中的多功能吸附材料：我们下一步要做什么？

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-09-04 DOI: 10.1016/j.sampre.2025.100211

Rafael Oliveira Martins, Maria Flávia Assunção Magalhães, Winnie Evelyn Valeria Perez Vite, Jussara da Silva Alves, Camila Will, Fernando Mauro Lanças

Continuous advances in sample preparation methods have led to the development of enhanced strategies to address the complexity of diverse matrices in both qualitative and quantitative analyses. These methods are designed to facilitate sample clean-up and preconcentration of target analytes before analysis by different analytical instruments. In both conventional and miniaturized solid-based approaches, the analytical performance of the extraction is primarily influenced by the sorbent phase. As the sorbent is responsible for mediating the interaction between the target analytes and the extraction material, careful selection is essential. In this context, a wide range of sorbent materials has been introduced to ensure efficient and selective interactions, supporting their application in sample preparation protocols. Nevertheless, the literature still lacks comprehensive and up-to-date reviews that highlight recent advances in sorbent development, including both conventional and bio-based alternatives. Therefore, this review aims to provide a current overview of sorbent innovations, discuss emerging trends, and outline potential future directions in the field.

样品制备方法的不断进步导致了增强策略的发展，以解决定性和定量分析中不同矩阵的复杂性。这些方法的目的是在不同的分析仪器分析之前，方便样品的清理和目标分析物的预浓缩。在传统和小型固体基方法中，萃取的分析性能主要受吸附相的影响。由于吸附剂负责调节目标分析物和萃取物质之间的相互作用，因此仔细选择是必不可少的。在这种情况下，广泛的吸附剂材料已经被引入，以确保有效和选择性的相互作用，支持它们在样品制备方案中的应用。然而，文献仍然缺乏全面和最新的评论，强调吸附剂发展的最新进展，包括传统和生物基替代品。因此，本综述旨在提供吸附剂创新的当前概述，讨论新兴趋势，并概述该领域潜在的未来方向。

{"title":"Versatile sorbent materials in sample preparation: Where do we go next?","authors":"Rafael Oliveira Martins, Maria Flávia Assunção Magalhães, Winnie Evelyn Valeria Perez Vite, Jussara da Silva Alves, Camila Will, Fernando Mauro Lanças","doi":"10.1016/j.sampre.2025.100211","DOIUrl":"10.1016/j.sampre.2025.100211","url":null,"abstract":"<div><div>Continuous advances in sample preparation methods have led to the development of enhanced strategies to address the complexity of diverse matrices in both qualitative and quantitative analyses. These methods are designed to facilitate sample clean-up and preconcentration of target analytes before analysis by different analytical instruments. In both conventional and miniaturized solid-based approaches, the analytical performance of the extraction is primarily influenced by the sorbent phase. As the sorbent is responsible for mediating the interaction between the target analytes and the extraction material, careful selection is essential. In this context, a wide range of sorbent materials has been introduced to ensure efficient and selective interactions, supporting their application in sample preparation protocols. Nevertheless, the literature still lacks comprehensive and up-to-date reviews that highlight recent advances in sorbent development, including both conventional and bio-based alternatives. Therefore, this review aims to provide a current overview of sorbent innovations, discuss emerging trends, and outline potential future directions in the field.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100211"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145010830","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

In-situ simultaneous extraction of non-steroidal anti-inflammatory drugs from wastewater using 3D-printed device and UHPLC-DAD/FLD analysis 利用3d打印装置和UHPLC-DAD/FLD分析同时提取废水中非甾体类抗炎药

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 Epub Date: 2025-09-01 DOI: 10.1016/j.sampre.2025.100210

César Castro-García , Arianna Palermo , Edwin Palacio , Luz O. Leal , Laura Ferrer

Non-steroidal anti-inflammatory drugs (NSAIDs) are widely employed in medicine for their anti-inflammatory and antipyretic properties. Their occurrence has been documented in effluents from wastewater treatment plants (WWTPs), as well as in aquatic ecosystems. NSAIDs are classified as emerging contaminants, thereby underscoring the importance of their environmental monitoring. This study presents a novel approach for the simultaneous on-site extraction of six NSAIDs –acetylsalicylic acid (ASP), celecoxib (CEL), diclofenac (DIC), ibuprofen (IBU), ketoprofen (KET), and naproxen (NAP)– from wastewater, followed by ultra-high performance liquid chromatography coupled with photodiode array and fluorescence detection (UHPLC-DAD/FLD). A 3D-printed device, coated with a highly selective solid-phase extraction (SPE) resin (Oasis HLB®), enabled on-site extraction and preconcentration of the analytes, avoiding to handle large sample volumes. A peristaltic pump helps both retention and elution steps. Method detection limits were 0.12 µg L^-1 for ASP, 0.16 µg L^-1 for CEL and IBU, 1.5 µg L^-1 for DIC, 0.09 µg L^-1 for KET and 0.19 µg L^-1 for NAP. The analytical performance of the 3D-printed device was demonstrated by precision below 5 % and the possibility of reusing up to 24 times without significant loss of extraction efficiency. An AGREEprep score of 0.53 classifies this methodology as moderately green. On-site analysis was conducted at the Calvià WWTP (Mallorca, Spain), where five NSAIDs were detected at various stages, demonstrating the feasibility of the on-site extraction across a broad concentration range. Except for ASP, which exhibited a recovery rate below 47 %, the remaining analytes showed satisfactory recoveries, ranging from 90 to 98 %.

非甾体抗炎药（NSAIDs）因其抗炎和解热的特性而被广泛应用于医学领域。它们在废水处理厂（WWTPs）的流出物以及水生生态系统中都有记录。非甾体抗炎药被归类为新兴污染物，因此强调了其环境监测的重要性。本研究建立了一种从废水中同时现场提取乙酰水杨酸（ASP）、塞来昔布（CEL）、双氯芬酸（DIC）、布洛芬（IBU）、酮洛芬（KET）和萘普生（NAP） 6种非甾体抗炎药的新方法，并采用超高效液相色谱-光电二极管阵列和荧光检测（UHPLC-DAD/FLD）。3d打印设备，涂有高选择性固相萃取（SPE）树脂（Oasis HLB®），可以现场提取和预浓缩分析物，避免处理大样本量。蠕动泵有助于保留和洗脱步骤。方法检出限分别为ASP 0.12µg L-1、CEL和IBU 0.16µg L-1、DIC 1.5µg L-1、KET 0.09µg L-1、NAP 0.19µg L-1。3d打印设备的分析性能被证明精度低于5%，并且可以重复使用多达24次，而不会显著降低提取效率。AGREEprep得分为0.53，将这种方法归类为中度绿色。在calvio污水处理厂（西班牙Mallorca）进行了现场分析，在不同阶段检测到五种非甾体抗炎药，证明了在广泛浓度范围内现场提取的可行性。除ASP回收率低于47%外，其余分析物的回收率均在90% ~ 98%之间，令人满意。

{"title":"In-situ simultaneous extraction of non-steroidal anti-inflammatory drugs from wastewater using 3D-printed device and UHPLC-DAD/FLD analysis","authors":"César Castro-García , Arianna Palermo , Edwin Palacio , Luz O. Leal , Laura Ferrer","doi":"10.1016/j.sampre.2025.100210","DOIUrl":"10.1016/j.sampre.2025.100210","url":null,"abstract":"<div><div>Non-steroidal anti-inflammatory drugs (NSAIDs) are widely employed in medicine for their anti-inflammatory and antipyretic properties. Their occurrence has been documented in effluents from wastewater treatment plants (WWTPs), as well as in aquatic ecosystems. NSAIDs are classified as emerging contaminants, thereby underscoring the importance of their environmental monitoring. This study presents a novel approach for the simultaneous on-site extraction of six NSAIDs –acetylsalicylic acid (ASP), celecoxib (CEL), diclofenac (DIC), ibuprofen (IBU), ketoprofen (KET), and naproxen (NAP)– from wastewater, followed by ultra-high performance liquid chromatography coupled with photodiode array and fluorescence detection (UHPLC-DAD/FLD). A 3D-printed device, coated with a highly selective solid-phase extraction (SPE) resin (Oasis HLB®), enabled on-site extraction and preconcentration of the analytes, avoiding to handle large sample volumes. A peristaltic pump helps both retention and elution steps. Method detection limits were 0.12 µg L<sup>-1</sup> for ASP, 0.16 µg L<sup>-1</sup> for CEL and IBU, 1.5 µg L<sup>-1</sup> for DIC, 0.09 µg L<sup>-1</sup> for KET and 0.19 µg L<sup>-1</sup> for NAP. The analytical performance of the 3D-printed device was demonstrated by precision below 5 % and the possibility of reusing up to 24 times without significant loss of extraction efficiency. An AGREEprep score of 0.53 classifies this methodology as moderately green. On-site analysis was conducted at the Calvià WWTP (Mallorca, Spain), where five NSAIDs were detected at various stages, demonstrating the feasibility of the on-site extraction across a broad concentration range. Except for ASP, which exhibited a recovery rate below 47 %, the remaining analytes showed satisfactory recoveries, ranging from 90 to 98 %.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100210"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989916","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0