Advances in Sample Preparation最新文献

Microwave-assisted extraction of isoangustone A from Derris scandens (Roxb.) Benth. using a hydrophobic deep eutectic solvents-based microemulsion 微波辅助提取黄芪中等angustone A的研究Benth。采用疏水深共晶溶剂型微乳液

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2026-02-22 DOI: 10.1016/j.sampre.2026.100232

Benyatip Buajan , Mudtorlep Nisoa , Fonthip Makkliang , Waraporn Putalun , Geoffrey A. Cordell , Rawiwan Charoensup , Gorawit Yusakul

The aim of this research was to develop a new extraction method combining hydrophobic deep eutectic solvent (HDES)-based microemulsion systems with microwave-assisted extraction (MAE) technology to enhance the extraction efficiency of isoangustone A (IsoA) from the leaves of the Thai medicinal plant Derris scandens (Roxb.) Benth. (Fabaceae). The research optimized the extraction parameters, characterized the microemulsion formulations, and evaluated the anti-inflammatory potential of the preparations in vitro. The HDES (menthol:lactic acid, 1:2 mol ratio)-microemulsion formulation demonstrated enhanced extraction efficiency over conventional ethanol-based methods. This formulation achieved a yield of IsoA of 6.52 μg/mg, surpassing the 5.76 μg/mg yield obtained through ethanol extraction. Response Surface Methodology (RSM) modeling enabled precise optimization of the extraction parameters, reaching 91.2 % predictive accuracy. Physicochemical characterization revealed that HDES-based microemulsions maintained 23.1–50.7 nm size, facilitating an enhanced bioavailability profile. The incorporation of D. scandens leaf extracts into the HDES (menthol:lactic acid, 2:1 mol ratio)-based microemulsion provided optimal inhibition of LPS-induced NO production in RAW264.7 macrophages, with IC₅₀ values (9.07±2.26 μg/mL) substantially lower than the DMSO-solubilized counterparts (53.7±3.8 μg/mL) demonstrating enhanced cell penetration resulting in improved extraction. This integrated approach represents a significant advancement in sustainable extraction technology, offering enhanced recovery of bioactive compounds while preserving their biological properties for further assessment.

本研究旨在建立一种基于疏水深共晶溶剂（HDES）微乳液体系与微波辅助萃取（MAE）技术相结合的提取方法，以提高泰国药用植物Derris scandens （Roxb）叶片中异angustone a （IsoA）的提取效率。Benth。(蝶形花科)。本研究优化了提取工艺，对微乳制剂进行了表征，并对其体外抗炎活性进行了评价。与传统的乙醇提取方法相比，HDES（薄荷醇：乳酸，1:2摩尔比）微乳液配方的提取效率更高。该配方的IsoA得率为6.52 μg/mg，优于乙醇提取法的5.76 μg/mg。响应面法（RSM）建模能够精确优化提取参数，预测准确率达到91.2%。物理化学表征表明，基于hdes的微乳液保持23.1-50.7 nm的尺寸，有助于提高生物利用度。将香丹参叶提取物掺入以HDES（薄荷醇：乳酸，物质比2:1）为基础的微乳液中，对lps诱导的RAW264.7巨噬细胞产生NO的抑制效果最佳，IC50值（9.07±2.26 μg/mL）显著低于dmso溶解的IC50值（53.7±3.8 μg/mL），表明细胞穿透能力增强，提取效果改善。这种综合方法代表了可持续提取技术的重大进步，在保留生物活性化合物的生物学特性以供进一步评估的同时，提高了生物活性化合物的回收率。

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引用次数: 0

Innovative ultrasound-assisted and vacuum manifold-assisted pipette tip solid-phase extraction using MSU-2-C18 sorbent for the extraction and purification of glycoalkaloids in potato-based snacks prior to UHPLC-MS/MS analysis 在UHPLC-MS/MS分析之前，使用MSU-2-C18吸附剂，采用创新的超声辅助和真空歧管辅助移液尖端固相萃取法提取和纯化马铃薯零食中的糖生物碱

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2025-11-25 DOI: 10.1016/j.sampre.2025.100228

Isabel Martínez-García , Damián Pérez-Quintanilla , Sonia Morante-Zarcero , Isabel Sierra

A miniaturized and environmentally conscious analytical workflow was developed and validated for the extraction, purification, and quantification of major glycoalkaloids (α-solanine, α-chaconine), the degradation product γ-chaconine, and the aglycone solanidine in potato-based snack products. The method combines ultrasound-assisted extraction (UAE) with pipette-tip solid-phase extraction (PT-SPE), followed by UHPLC-MS/MS analysis. UAE conditions were optimized using a Box-Behnken statistical design, which evaluated the extraction time, ultrasound amplitude, and solid:liquid (SL) ratio. Optimal conditions were determined to be 5 min, 100 % amplitude, and a 1:9 w/v of SL ratio, with methanol as the most effective extraction solvent. MSU-2-C18 mesostructured silica sorbent, packed into pipette tips (5 mg) connected to a SPE vacuum manifold (VMA-PT-SPE), was employed under the optimized conditions to simultaneously purify up to 12 extracts. The method's greenness was evaluated using the AGREEprep metric, yielding a score of 0.65, indicating good environmental performance. Limits of detection (LOD) and quantification (LOQ), ranging from 0.55–4.40 µg/kg and 1.82–14.67 µg/kg, respectively, were achieved for the target analytes. Application to four commercial potato-based snacks revealed major (α-solanine and α-chaconine) and minor glycoalkaloids (γ-chaconine and solanidine) levels, ranging from 2.0 to 16.0 mg/kg fresh weight, highlighting substantial variability among products and providing a more comprehensive characterization of the glycoalkaloid profile. Compared to conventional SPE formats, this UAE-VMA-PT-SPE strategy offers superior reproducibility while reducing sample and solvent consumption. The method represents a powerful tool for routine monitoring of glycoalkaloids in potato snacks, supporting food safety assessments and addressing analytical priorities established by the European Food Safety Authority.

开发并验证了一种小型化、环保的分析流程，用于提取、纯化和定量马铃薯零食产品中主要的糖生物碱（α-龙葵碱、α-恰康碱）、降解产物γ-恰康碱和茄碱苷元。该方法将超声辅助提取（UAE）与移液头固相萃取（PT-SPE）相结合，然后进行UHPLC-MS/MS分析。采用Box-Behnken统计设计优化UAE条件，评估提取时间、超声振幅和固液比。以甲醇为最佳提取溶剂，提取时间为5 min，提取幅度为100%，SL比为1:9 w/v。MSU-2-C18介结构二氧化硅吸附剂装在连接到SPE真空歧管（VMA-PT-SPE）的移液头（5mg）中，在优化的条件下同时纯化多达12个提取物。该方法的绿色度使用AGREEprep指标进行评估，得分为0.65，表明环境性能良好。目标分析物的检出限（LOD）和定量限（LOQ）分别为0.55 ~ 4.40µg/kg和1.82 ~ 14.67µg/kg。对四种商业马铃薯零食的研究显示，主要的（α-龙葵碱和α-恰康碱）和次要的糖生物碱（γ-恰康碱和茄碱）含量在2.0到16.0 mg/kg新鲜重量之间，突出了产品之间的巨大差异，并提供了更全面的糖生物碱谱表征。与传统的SPE格式相比，这种UAE-VMA-PT-SPE策略在减少样品和溶剂消耗的同时提供了卓越的重现性。该方法是马铃薯零食中糖生物碱常规监测的有力工具，支持食品安全评估和解决欧洲食品安全局确定的分析重点。

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引用次数: 0

Corrigendum to “A Novel Automated Micro Solid Phase Extraction (µSPE) Method to Quantify 21 Per- and Polyfluoroalkyl Substances Compounds in Biological Samples” [Advances in Sample Preparation, Volume 17 (2026) 1-13/100230] “一种新型自动微固相萃取（µSPE）方法定量生物样品中的21个全氟和多氟烷基物质化合物”的勘误表[样品制备进展，第17卷（2026）1-13/100230]

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2026-02-26 DOI: 10.1016/j.sampre.2026.100231

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

引用次数: 0

Electromembrane extraction of tetracyclines in foods and human plasma prior to LC-MS/MS analysis: Impact of sample matrix on extraction performance LC-MS/MS分析前食品和人血浆中四环素的电膜提取：样品基质对提取性能的影响

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2026-02-01 Epub Date: 2025-11-21 DOI: 10.1016/j.sampre.2025.100227

Anne Oldeide Hay, Frederik André Hansen

Tetracyclines are widely used antibiotics in animal farming, raising concerns over their residues in food and associated health risks. Current methods for residue determination are complex, time-consuming, and produce substantial solvent waste. Electromembrane extraction (EME) offers high clean-up efficiency, minimal solvent use, and direct LC-MS/MS compatibility. This study evaluates EME for extraction of four tetracyclines (oxytetracycline, tetracycline, chlorotetracycline, doxycycline) from complex matrices including milk, egg white, honey, and human plasma. Optimal parameters varied across matrices, underscoring the need for matrix-specific optimization. Optimized methods achieved recoveries of 66–101 %, excellent linearity (R² = 0.9929–0.9998), and minimal matrix effects (-14 % to 1 %). LLOQs ranged from 0.5 to 2.1 ng/g, with calibration curves extending to 1000 ng/g, covering concentrations relevant for residue monitoring. These results demonstrate EME’s potential for reliable analysis of challenging polar and zwitterionic compounds in food and biological samples. Finally, the greenness was evaluated by the AGREEprep metric tool, gaining a total score of 0.64.

四环素是动物养殖中广泛使用的抗生素，引起了人们对其在食品中的残留和相关健康风险的担忧。目前的残留测定方法复杂，耗时，并且产生大量的溶剂浪费。电膜萃取（EME）具有清洁效率高、溶剂用量少、LC-MS/MS直接兼容等优点。本研究评估了EME从复杂基质（包括牛奶、蛋清、蜂蜜和人血浆）中提取四种四环素（土霉素、四环素、氯四环素、强力霉素）的效果。最优参数因矩阵而异，强调了对矩阵特定优化的需求。优化后的方法回收率为66% ~ 101%，线性良好（R²= 0.9929 ~ 0.9998），基质效应最小（- 14% ~ 1%）。LLOQs范围为0.5 ~ 2.1 ng/g，校准曲线延伸至1000 ng/g，涵盖了与残留监测相关的浓度。这些结果证明了EME在食品和生物样品中具有挑战性的极性和两性离子化合物的可靠分析方面的潜力。最后，采用AGREEprep指标工具对绿度进行评价，得到总分0.64分。

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引用次数: 0

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。

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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。

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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。

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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。

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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。

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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%。

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