Simple solid-phase extraction method for determination of polychlorinated biphenyls and selected organochlorine pesticides in human serum

Abstract

A simple off-line solid-phase extraction (SPE) method for isolation of polychlorinated biphenyls (PCBs) and selected organochlorine pesticides (OCPs) from human serum has been developed. The procedure includes denaturation of serum proteins by a mixture of water–1-propanol, application of the sample by aspiration twice repeatedly through the SPE column and elution with a mixture of n-hexane–dichlormethane. After final clean-up the compounds of interest were analysed by gas chromatography with micro-electron capture detection (GC–μECD). The recoveries achieved for PCB congeners using spiked porcine serum samples were 99–120% and for OCPs 88–115%. Relative standard deviations (RSD) ranged from 3 to 7%. The method was applied to real human serum samples and the recoveries of analytes in the serum were proportionally recalculated considering the recovery of the internal standard PCB-174. PCB-103 served as a syringe standard to correct volume of samples analysed. The aim of this study was to develop an effective off-line SPE procedure by optimization of existing SPE methods to supply laborious, solvent- and time-consuming liquid–liquid extraction (LLE) in routine analytical process.