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采用 HPLC 柱切换在线样品制备结合 ESI-MS/MS 同时定量测定人血清和母乳中的全氟烷基酸。

Simultaneous quantitation of perfluoroalkyl acids in human serum and breast milk using on-line sample preparation by HPLC column switching coupled to ESI-MS/MS.

机构信息

Bavarian Health and Food Safety Authority, Environmental Medicine/Biomonitoring, Pfarrstrasse 3, D-80538 Munich, Germany.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 1;878(27):2652-8. doi: 10.1016/j.jchromb.2010.01.015. Epub 2010 Jan 18.

DOI:10.1016/j.jchromb.2010.01.015
PMID:20172766
Abstract

A high throughput analytical method using a column switching high-performance liquid chromatography combined with isotope dilution tandem mass spectrometry (column switching-HPLC-MS/MS) was developed to simultaneously quantitate the concentrations of 7 perfluoroalkyl acids (PFAAs) in serum and 3 PFAAs in breast milk samples. The sample preparation includes addition of the isotope-labelled internal standard solution to breast milk and serum, enzymatic hydrolysis and filtration of milk samples, precipitation of proteins and analysis by column switching-HPLC-MS/MS. The limits of quantitation ranged from 0.1 to 0.4 μg/l for serum and 0.02 to 0.15 μg/l for breast milk samples. The method accuracies ranged between 73.2% and 100.2% for the different analytes at two concentrations in PFAAs spiked samples. The validity of the method was confirmed by analysing 20 serum and 20 breast milk samples.

摘要

建立了一种基于柱切换高效液相色谱-串联质谱(column switching-HPLC-MS/MS)的高通量分析方法,用于同时定量血清中 7 种全氟烷基酸(PFAAs)和乳样中 3 种 PFAAs 的浓度。样品制备包括向乳样和血清中加入同位素标记的内标溶液,对乳样进行酶解和过滤,沉淀蛋白质,然后通过柱切换-HPLC-MS/MS 进行分析。血清中各物质的定量下限为 0.1-0.4μg/L,乳样中各物质的定量下限为 0.02-0.15μg/L。在不同浓度加标 PFAAs 样品中,不同物质的方法准确度在 73.2%-100.2%之间。通过分析 20 份血清和 20 份乳样验证了该方法的有效性。

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