Simultaneous determination of perfluorooctane sulfonate and perfluorooctanoic acid isomers by HPLC-MS/MS
Simultaneous determination of perfluorooctane sulfonate and perfluorooctanoic acid isomers by HPLC-MS/MS
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DOI：
10.7524/j.issn.0254-6108.2015.08.2015011801
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发表时间：
2015-08-01
期刊：
影响因子：
--
通讯作者：
Cai Yaqi
中科院分区：
文献类型：
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作者：
Niu Xiameng;Shi Yali;Cai Yaqi
建立了固相萃取-高效液相色谱-串联质谱（SPE-HPLC-MS/MS）同时测定环境样品中全氟辛烷磺酸和全氟辛酸异构体的方法。样品经WAX固相萃取柱富集净化后，采用负离子电喷雾多反应监测（MRM）模式进行HPLC-MS/MS测定。用Ascentis（R）Express F5 PFP柱实现分离，其中移动的相为A，甲醇和B，60 mmol。L-1 NH4OH/20 mmol . L-1甲酸水溶液。建立的方法用于分析水，沉积物和贝类样品。方法检出限（S/N = 3）在0.05-1.1 ng之间。L ~（-1），0.025-0.56 ng . g（-1）和0.025- 0.56ng. g（-1）。PFASs异构体的回收率在90。8%-127%，74. 0%-124%和76.相对标准偏差（RSD，n = 5）分别为5.9%~ 17.2%、2.5%~ 17.0%和3.30%~ 11.5%。
A method was established for simultaneous determination of perfluorooctane sulfonate and perfluorooctanoic acid isomers in environmental sample by using high performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction (SPE-HPLC-MS/MS). The WAX SPE cartridge was used for samples' enrichment and clean-up, then followed by determination by HPLC-MS/MS in negative electrospray ionization and multiple reaction monitoring (MRM) mode. The separation was achieved with an Ascentis (R) Express F5 PFP column with mobile phases of A, methanol and B, 60 mmol . L-1 NH4OH/20 mmol . L-1 formic acid aqueous solution. The established method was used for the analyses of water, sediment and shellfish samples. The method detection limits(S/N = 3) were in the range of 0.05-1.1 ng . L-1, 0.025-0.56 ng . g(-1) and 0.025-0.56 ng . g(-1), respectively. Satisfactory results were obtained with the recoveries of PFASs isomers in the range of 90. 8%-127%, 74. 0%-124% and 76. 7%-113%, and the relative standard deviations (RSD, n = 5) in the range of 5.9%-17.2%, 2.5%-17.0% and 3.30%-11.5%, respectively.