title: 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-microECD). 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.
authors.affiliation: Department of Toxic Organic Pollutants, Research Base of the SMU--Institute of Preventive and Clinical Medicine, Slovak Medical University, Limbová 12, 83303 Bratislava, Slovak Republic. kamil.conka@szu.sk
authors.forename: K
authors.initials: K
authors.lastname: Conka
authors.forename: B
authors.initials: B
authors.lastname: Drobná
authors.forename: A
authors.initials: A
authors.lastname: Kocan
authors.forename: J
authors.initials: J
authors.lastname: Petrík
mesh_terms: D000818:Animals; D005591:Chemical Fractionation / Q000379:methods; D002849:Chromatography, Gas / Q000379:methods; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000097:blood*; D010575:Pesticides / Q000097:blood*; D011078:Polychlorinated Biphenyls / Q000097:blood*; D011786:Quality Control; D015203:Reproducibility of Results; D013552:Swine
chemical_list: D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D011078:Polychlorinated Biphenyls