A novel automated micro solid phase extraction (µSPE) method to quantify 21 per- and polyfluoroalkyl substances compounds in biological samples

IF 6.6 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

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Abstract

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.

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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

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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来源期刊

Advances in Sample Preparation

CiteScore

3.50

自引率

0.00%

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