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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 33, Number 11
BKCSDE 33(11)
November 20, 2012 
 
Title
 High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry
Author
 Won-Woong Lee, Sun-Young Lee, Se Mi Yu, Jongki Hong*
Keywords
 Perfluorinated compounds, Serum, Monolithic column, LC-MS/MS, Method validation
Abstract
 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 13C-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 (R2) 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.
Page
 3727 - 3734
Full Text
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