title: Determination of selected perfluorinated alkyl acids and persistent organic pollutants from a small volume human serum sample relevant for epidemiological studies.
abstract: A simple and fast method is presented for the determination of selected persistent organic pollutants (POPs) and perfluorinated alkyl acids (PFAAs), a subgroup of per- and polyfluorinated alkyl substances (PFAS) from a single 200μl aliquot of serum. Sample pretreatment starts with dispersive solid phase extraction of POPs to dichloromethane-hexane, which is immediately poured to cleanup column. POPs are eluted from column and concentrated for GC-MS/MS analysis. PFAAs are trapped to dispersant and are then extracted with ammonium acetate in methanol, concentrated and analysed with LC-MS/MS. For POPs, the limit of detection (LOD) ranged from 1.6 to 17pg/ml. Oxychlordane and dichlorodiphenyltrichloroethane had LODs in the upper end of this range as they were more labile and prone for interferences in the GC-MS/MS. For PFAAs, the LOD range from 0.027 to 0.068ng/ml. For POPs, the accuracy from Standard Reference Materials SRM 1589a and Arctic Monitoring and Assessment Programme (AMAP) intercalibration samples range from 74 to 127% and the repeatability (relative standard deviation, RSD%) from 2.0 to 15%. For PFAAs, the accuracy from AMAP samples ranged from 90 to 110% and from LOQ level spiked serum samples from 72 to 133%. Repeatability from AMAP and LOQ samples ranged from 1.6 to 7.3% and 5.5 to 15%, respectively. The presented method is useful in epidemiological studies where only limited amount of serum is available.
authors: National Institute for Health and Welfare, Department of Environmental Health, P.O. Box 95, FI-70701 Kuopio, Finland. ani.koponen@thl.fi
authors: Jani
authors: J
authors: Koponen
authors: Panu
authors: P
authors: Rantakokko
authors: Riikka
authors: R
authors: Airaksinen
authors: Hannu
authors: H
authors: Kiviranta
mesh_terms: D004781:Environmental Exposure / Q000032:analysis; D004785:Environmental Pollutants / Q000097:blood* / Q000302:isolation & purification; D016021:Epidemiologic Studies; D005466:Fluorocarbons / Q000097:blood* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D009930:Organic Chemicals / Q000097:blood* / Q000302:isolation & purification; D052616:Solid Phase Extraction
chemical_list: D004785:Environmental Pollutants; D005466:Fluorocarbons; D009930:Organic Chemicals; C018959:hexadecafluoro-nonanoic acid
keywords: Cardiovascular disease; Dispersive solid phase extraction; Human serum; Perfluorinated alkyl substances; Persistent organic pollutants; Type 2 diabetes