High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry
High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry
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DOI：
10.5012/bkcs.2012.33.11.3727
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发表时间：
2012-11
影响因子：
1.7
通讯作者：
Wonwoong Lee;Sun Young Lee;S. Yu;Jongki Hong
中科院分区：
文献类型：
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作者：
Wonwoong Lee;Sun Young Lee;S. Yu;Jongki Hong
建立了一种快速测定人血清中全氟化合物的分析方法。采用改进的方法从人血清中提取和纯化PFCs。采用C18整体柱液相色谱（LC）在3.3 min内快速分离了10种PFCs，电喷雾串联质谱（MS/MS）在负离子模式下进行检测。整体柱LC上PFC的运行时间比传统柱LC快4倍。研究了三乙胺（TEA）对移动的相的影响，考察了TEA对全氟碳化物电喷雾电离质谱检测灵敏度的影响。采用13 C标记的内标物，通过LC-MS/MS以多离子反应监测（MRM）模式进行定量。进行方法验证以确定回收率、线性、精密度和定量限，然后分析标准参比物质（NIST的SRM 1957）。整个方法的总回收率范围为81.5 - 106.3%，RSD为3.4 - 16.2%。方法的线性范围为0.33 ~ 50 ng·mL-1，相关系数（R2）大于0.995，定量限为0.08 ~ 0.46 ng·mL-1 .该方法可用于人血清中10种PFCs的快速、灵敏、准确的定量分析。
An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using 13 C-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 ng mL �1 , with a correlation coefficient (R 2 ) greater than 0.995 and the limits of quantification with 0.08 to 0.46 ng mL �1 . This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.