Determination of hydroxy-PCBs in urine by gas chromatography/mass spectrometry with solid-phase extraction and derivatization

Abstract

A sensitive derivatization and extraction method is proposed for the determination of hydroxy-PCBs in urine. Phenolic hydroxyl groups of PCBs were allowed to react with five different reagents such as iodomethane, iodoethane, iodopropane, BSTFA and MTBSTFA. Propylated products at 100degreesC for 30 min showed the best sensitivity with mass selective detector. Extraction recoveries and relative standard deviations of hydroxy-PCBs by SPE using C2 column were in the range of 78.0-112.3% and 2.5-9.6%, respectively. Instrumental detection limits for derivatized hydroxy-PCBs were in the range of 1-2 pg and were 10-1000 times more sensitive than those of non-derivatized hydroxy-PCBs. The correlation coefficients of the linear regression curves exceed 0.99, and the intra- and inter-day precisions were evaluated by RSDs within 10% at the concentrations of 0.4 and 4.0 ng/mL. (C) 2004 Elsevier B.V. All rights reserved.