Determination of Perfluorinated Compounds in Human Blood Samples by High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry
Determination of Perfluorinated Compounds in Human Blood Samples by High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry
复制标题
DOI：
10.1016/s1872-2040(08)60072-9
复制
发表时间：
2008-10-01
影响因子：
1.2
通讯作者：
Cai Ya-Qi
中科院分区：
文献类型：
--
作者：
Pan Yuan-Yuan;Shi Ya-Li;Cai Ya-Qi
建立了分离测定血液样品中9种全氟化合物的灵敏方法。采用高效液相色谱/电喷雾串联质谱(HPLC - ESI MS/MS) - C-18反相柱，在15 min内检测全氟己烷磺酸（PFHxS）、全氟乙烷酸（PFHpA）、全氟辛酸（PFOA）、全氟辛烷磺酸（PFOS）、全氟壬烷酸（PFNA）、全氟癸酸（PFDA）、全氟癸酸（PFUnDA）、全氟十二烷酸（PFDoDA）和全氟十四烷酸（PFTA）。使用C-13(4)标记的全氟辛烷磺酸（MPFOS）作为内部标准。在传统的注射前MTBE提取后，用固相萃取筒进一步提取血液样品中的PFCs。对RP、P、C-18、HLB四种吸附剂进行了测试，最终选择HLB为高效吸附剂。对两种C-18色谱柱，Acclaim 120（50毫米× 4.6毫米，3亩）和Acclaim 120（250毫米× 4.6毫米，5亩）也进行了比较研究。两种色谱柱灵敏度相近，对真实血液样品的检出限为0.03 ~ 0.8 μ g/L。加样回收率的相对标准偏差为3% ~ 11%。最后，由于柱容量的优势，选择了Acclaim公司的120柱（250 mm x 4.6 mm, 5 μ m）。在最佳条件下，除PFTA的回收率仅为60%左右外，血液样品中PFCs的回收率为74.2% ~ 118.1%
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 C-13(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%