A rapid and fully automatic method for the accurate determination of a wide carbon-chain range of per- and polyfluoroalkyl substances (C4-C18) in human serum
A rapid and fully automatic method for the accurate determination of a wide carbon-chain range of per- and polyfluoroalkyl substances (C4-C18) in human serum
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一种快速全自动方法，用于准确测定人血清中宽碳链范围的全氟烷基物质和多氟烷基物质 (C4-C18)
DOI：
10.1016/j.chroma.2016.09.050
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发表时间：
2016-11-04
影响因子：
4.1
通讯作者：
Zhang, Aiqian
中科院分区：
文献类型：
--
作者：
Gao, Ke;Gao, Yan;Zhang, Aiqian
建立了一种快速、全自动测定人血清中21种全氟烷基和多氟烷基物质(碳链范围从C4到C18，包括13个全氟烷基化合物、5个全氟烷基化合物、2个氯-全氟烷基化合物和PFOSA)的方法。对高效液相色谱参数、Turboflow柱、流动相、进样量、上样流速、样品清理和洗脱时间进行了优化。将25亩L血清样品稀释后直接进样到在线Turboflow固相萃取液相色谱质谱联用系统进行分析。由于Turboflow色谱柱的基质去除效率和所使用的足够类型的内部同位素标准，对基质效应进行了校正。建立的方法具有良好的线性关系(r(2)>；0.99)、快速处理时间(每个样品20min)、满意的回收率(基质加标回收率为84.6%~114%)和精密度(日内和日间RSD分别为1.5%~9.2%和1.1%~7.0%)。21种分析的全氟辛烷磺酸的检出限在0.008~0.19ngmL(-1)之间。短链和长链全氟辛烷磺酸的检出限分别为0.008、0.022、0.15和0.19ngmL(-1)，加标回收率分别为101.05、87.1和85.8%。精密度和回收率均好于以往的研究。此外，在线固相萃取方法与传统的离线固相萃取方法测定的血清PFASs浓度一致(r：0.98~0.99)，验证了本方法的准确性和适用性。该方法在人血清中痕量全氟烷基物质和多氟烷基物质的分析中具有良好的应用前景。(C)2016爱思唯尔B.V.保留所有权利。
A rapid and fully automatic method for determining 21 per- and polyfluoroalkyl substances (with carbon chains ranging from C4 to C18, including 13 PFCAs, 5 PFCAs, 2 Cl-PFESAs, and PFOSA) in human serum samples was developed. The HPLC parameters, Turboflow column, mobile phase, sample injection volume, loading flow rate, and sample cleanup and elution time were optimized. 25 mu L serum sample was directly injected into the developed on-line Turboflow SPE HPLC-MS/MS system for analysis after dilution. Matrix effects were corrected due to the matrix removal efficiency of the Turboflow column and sufficient types of internal isotope standards that were used. The established method showed a good linearity (r(2)>0.99), rapid processing time (20 min per sample), satisfactory recoveries (matrix spiked recoveries range from 84.6% to 114%) and precision (intra-day and inter-day RSDs ranged from 1.5% to 9.2% and from 1.1% to 7.0%, respectively). The limits of detection (LODs) of the 21 analyzed PFASs were between 0.008 and 0.19 ngmL(-1). The LODs of short- and long-chain PFASs, such as PFBA, PFPeA, PFHxDA, and PFODA, were 0.008, 0.022, 0.15 and 0.19 ngmL(-1), respectively; the spiked recoveries of these PFASs were 101, 105, 87.1, and 85.8%, respectively. Both the LODs and recoveries were better than previous studies. Further, serum PFASs concentrations detected by the presented on-line SPE method were consistent with the traditional off-line SPE method (r: 0.98-0.99), which verified the accuracy and applicability of the present method. The method shows good practical prospects in the analysis of trace per- and polyfluoroalkyl substances in human serum. (C) 2016 Elsevier B.V. All rights reserved.