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Determination of Perfluorinated Compounds in Human Blood Samples by High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

机译:高效液相色谱-电喷雾串联质谱法测定人血中的全氟化合物

摘要

A sensitive method was established for the separation and determination of nine perfluorinated compounds (PFCs) in blood samples. Perfluorohexane sulfonate (PFHxS), perfluorohetanoic acid (PFHpA), perfluorooctanoate (PFOA), perfluorooctane sulfonat (PFOS), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecnaoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA) and perflouorotetradodecanoic acid(PFTA) were detected by high performance liquid chromatography/electrospray tandem mass spectrometry (HPLC ESI MS/MS) with C(18) reversed phase column in 15 min, using (13)C(4) labeled PFOS (MPFOS) as the internal standard. PFCs in the blood samples were further extracted with solid phase extraction cartridges after traditional MTBE extraction before injection. Four kinds of cartridges were tested, including RP, P, C(18) and HLB, then HLB cartridge was selected as the efficient adsorbent. A comparative study of two C(18) columns, Acclaim 120 (50 mm x 4.6 min, 3 mu m) and Acclaim 120 (250 mm x 4.6 mm, 5 mu m) column, were also performed. Both columns provided similar sensitivities, with the detection limits of 0.03 -0.8 mu g/L for real blood samples. The relative standard deviation of recoveries ranged from 3% to 11%. Finally, Acclaim 120 (250 mm x 4.6 mm, 5 mu m) column was chosen for its superiority of column capacity. With the optimal conditions, the recoveries of PFCs in blood samples ranged from 74.2% to 118.1%, with the exception of PFTA, which was only about 60%
机译:建立了一种灵敏的方法来分离和测定血液样品中的九种全氟化合物(PFC)。全氟己烷磺酸盐(PFHxS),全氟己酸(PFHpA),全氟辛酸(PFOA),全氟辛烷磺酸(PFOS),全氟壬酸(PFNA),全氟癸酸(PFDA),全氟十一烷酸(PFUnDA),全氟十二烷四酸(loudo)使用(13)C(4)标记的PFOS(MPFOS)作为内标,通过高效液相色谱/电喷雾串联质谱(HPLC ESI MS / MS)在15分钟内使用C(18)反相柱进行检测。传统MTBE萃取后,在进样前用固相萃取柱进一步萃取血样中的PFC。测试了四种滤芯,包括RP,P,C(18)和HLB,然后选择HLB滤芯作为有效吸附剂。还进行了两个C(18)色谱柱的比较研究,Acclaim 120(50 mm x 4.6 min,3μm)和Acclaim 120(250 mm x 4.6 mm,5μm)色谱柱。两种色谱柱都提供了相似的灵敏度,对真实血液样品的检出限为0.03 -0.8μg / L。回收率的相对标准偏差为3%至11%。最后,选择Acclaim 120(250 mm x 4.6 mm,5μm)色谱柱,因为它具有出色的色谱柱容量。在最佳条件下,血液样品中PFC的回收率范围为74.2%至118.1%,但PFTA除外,后者仅为60%左右。

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