title: High throughput method for the determination of organochlorine pesticides and polychlorinated biphenyls in human serum.
abstract: An improved method for the determination of selected organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in human serum was developed. The method requires low volume of serum (500 microl) and 48-96 samples per day can be prepared by one analyst without special automatic equipment. Initial extraction was performed using 96-well solid-phase extraction disk plates and was followed by a clean-up with silica gel/sulfuric acid. Different denaturation, elution and clean-up conditions were tested. Quantification was carried out by gas chromatography equipped with electron capture detector (GC-ECD) or mass spectrometer (GC-MS). Recoveries of PCB congeners 28, 52, 101, 118, 138, 153 and 180 and OCPs HCB, beta-HCH, p,p'-DDE and p,p'-DDT at two spiking levels (n=8) varied from 57 to 120%, and intra-day relative standard deviation from 1 to 11%, both depending on spiking level and compound. Inter-day relative standard deviation was <15% in all cases. Limit of quantification (LOQ) for these PCBs ranged from 0.08 to 0.13 ng/ml and for these OCPs from 0.16 to 0.40 ng/ml. The optimized method was applied to the analysis of 1000 serum samples from different places of Spain.
authors.affiliation: Laboratorio de Salud Pública de Guipúzcoa, Avenida Navarra 4, 20013-San Sebastián, Spain. labora2-san@ej-gv.es
authors.forename: Fernando
authors.initials: F
authors.lastname: Goñi
authors.forename: Raul
authors.initials: R
authors.lastname: López
authors.forename: Arsenio
authors.initials: A
authors.lastname: Etxeandia
authors.forename: Esmeralda
authors.initials: E
authors.lastname: Millán
authors.forename: Pilar
authors.initials: P
authors.lastname: Amiano
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006843:Hydrocarbons, Chlorinated / Q000097:blood*; D010575:Pesticides / Q000097:blood*; D011078:Polychlorinated Biphenyls / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D011078:Polychlorinated Biphenyls