title: Determination of organochlorine pesticides and polychlorinated biphenyls in human serum using headspace solid-phase microextraction and gas chromatography-electron capture detection.
abstract: A simple procedure for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in human serum using headspace solid-phase microextraction (HS-SPME) was developed. The analysis was carried out by gas chromatography (GC) equipped with electron capture detector (ECD). A 2(7-4) Plackett-Burman reduced factorial design for screening and a central composite design for optimizing the significant variables were applied. A 100 microm PDMS fiber, 3/5 headspace ratio (3 ml in 5 ml vial), 85 degrees C extraction temperature, 50 min extraction time, and 1 ml of acidic solution (pH 3) added to 1 ml of diluted serum (1:1) were chosen for the best response in HS extraction mode. The detection limits found were from 1 pg/ml (PCB 167) to 52 pg/ml (beta-HCH), the relative standard deviation for the procedure varied from 3% (PCB 52) to 12% (PCB 189) and the accuracy was checked by using validated solid-phase extraction (SPE) procedure. The method that avoids the use of clean-up steps and the hazardous solvents enabled reliable determinations of the OCPs and the PCBs except beta-HCH. The method was applied to the analysis of 33 human serum samples. The most abundant target compound was p-p'-DDE (range, 0.3-8.0 ng/ml; median value, 2.1 ng/ml). Among the PCBs the prevalent congeners were 138, 153 and 180.
authors.affiliation: Departamento de Química Aplicada, Universidad del País Vasco, Facultad de Química, Apdo. 1072, 20080-San Sebastián, Spain.
authors.forename: Raul
authors.initials: R
authors.lastname: López
authors.forename: Fernando
authors.initials: F
authors.lastname: Goñi
authors.forename: Arsenio
authors.initials: A
authors.lastname: Etxandia
authors.forename: Esmeralda
authors.initials: E
authors.lastname: Millán
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000097:blood*; D010575:Pesticides / Q000032:analysis*; D011078:Polychlorinated Biphenyls / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results
chemical_list: D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D011078:Polychlorinated Biphenyls