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An integrated method for simultaneously determining 10 classes of per- and polyfluoroalkyl substances in one drop of human serum
Analytica Chimica Acta ( IF 6.2 ) Pub Date : 2018-01-01 , DOI: 10.1016/j.aca.2017.10.038
Ke Gao , Jianjie Fu , Qiao Xue , Yili Li , Yong Liang , Yuanyuan Pan , Aiqian Zhang , Guibin Jiang

Per- and polyfluoroalkyl substances (PFASs) represent a group of synthetic chemicals, and they have quite different physicochemical properties, which result in difficulties of their simultaneous determination in a single injection. A sensitive, reliable, and fully automated method was developed for simultaneously detecting 10 classes of PFASs (total of 43) in human serum using online Turboflow SPE-UHPLC-MS/MS. This method provided high linearity of matrix-matched calibration standards (R > 0.99), excellent method limits of detection (MLODs) (0.013-0.089 ng mL-1), satisfactory matrix spiked recoveries (84.3-109%) and relative standard deviations (RSDs) (intra-day RSDs: 1.3-12.6%, inter-day RSDs: 1.7-13.8%, inter-week RSDs: 1.8-13.5%, inter-month RSDs: 3.1-12.4%), short analysis time (19 min per sample) and small sample amount requirement (25 μL), which were suitable for large-scale epidemiologic studies. Moreover, the method provided the feasibility of real-time monitoring for the degradation kinetics of PFASs precursors both in vitro and in vivo. The quality of the present method was further verified by repetitive analysis of a standard reference material (SRM 1957), with the deviations of the targeted PFAS concentrations ranging from 1.9% to 14.2% (n = 5) between the detected and reference values. The present study also determined values for several PFASs in SRM 1957 other than those on the certificate, for the first time, such as N-EtFOSA, 6:2 Cl-PFESA, and PFBA. Finally, the established method was applied to detect PFASs in serum samples of 15 ordinary people and 15 occupational workers, and 6:2 FTSA was found as the dominant precursor.

中文翻译:

一种同时测定一滴人血清中 10 类全氟和多氟烷基物质的综合方法

全氟烷基物质和多氟烷基物质 (PFAS) 是一组合成化学品,它们的理化性质差异很大,因此难以在一次进样中同时测定。开发了一种灵敏、可靠且全自动的方法,可使用在线 Turboflow SPE-UHPLC-MS/MS 同时检测人血清中的 10 类 PFAS(共 43 种)。该方法提供了基质匹配校准标准品的高线性度 (R > 0.99)、出色的方法检测限 (MLOD) (0.013-0.089 ng mL-1)、令人满意的基质加标回收率 (84.3-109%) 和相对标准偏差 ( RSD)(日内 RSD:1.3-12.6%,日间 RSD:1.7-13.8%,周间 RSD:1.8-13.5%,月间 RSD:3.1-12.4%),分析时间短(19 分钟)每个样品)和小样品量要求(25 μL),适合大规模流行病学研究。此外,该方法为实时监测全氟和多氟烷基物质前体的体外和体内降解动力学提供了可行性。本方法的质量通过对标准参考物质 (SRM 1957) 的重复分析得到进一步验证,目标 PFAS 浓度在检测值和参考值之间的偏差范围为 1.9% 至 14.2% (n = 5)。本研究还首次确定了 SRM 1957 中除证书之外的几种 PFAS 的值,例如 N-EtFOSA、6:2 Cl-PFESA 和 PFBA。最后,将建立的方法应用于15名普通人和15名职业工人血清样本中PFASs的检测,发现6:2 FTSA为显性前体。
更新日期:2018-01-01
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