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Simultaneous quantitation of seven pyrethroid metabolites in human urine by capillary gas chromatography–mass spectrometry
Author(s) -
Tao Lin,
Chen Mei,
Collins Erin,
Lu Chensheng
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200655
Subject(s) - chromatography , chemistry , urine , derivatization , pyrethroid , gas chromatography–mass spectrometry , coefficient of variation , mass spectrometry , gas chromatography , detection limit , biochemistry , pesticide , biology , agronomy
Pyrethroid insecticides are applied in the residential environment, as well as in agricultural crops, for insect control purpose. We developed and validated an accurate, sensitive, and reproducible analytical method to simultaneously detect seven pyrethroid metabolites, namely, 3‐(2,2‐dichlorovinyl)‐2,2‐dimethyl‐(1‐cyclopropane) carboxylic acid, 3‐(2,2‐dibromovinyl)‐2,2‐dimethyl‐(1‐cyclopropane) carboxylic acid, 3‐phenoxybenzoic acid, 4‐fluoro‐3‐phenoxybenzoic acid, 2‐methyl‐3‐phenylbenzoic acid, 4‐chloro‐α‐isoproply benzeneacetic acid, and 3‐(2‐chloro‐3,3,3‐trifluoroprop‐1‐enyl)‐2,2‐dimethylcyclopropanecarboxylic acid, in human urine. This method employs deconjugation with enzyme, SPE using A gilent C 18 cartridges on a R apid T race SPE workstation, derivatization using hexafluoro isopropanol and N , N ′‐diisopropylcarbodiimide, and compounds separation and identification on GC – MS . The detection limits of seven metabolites were 0.02–0.08 ng/m L in urine. The recoveries of seven metabolites were 81–104%, 85–99%, and 83–99% in urine specimens fortified at 0.1, 0.4, and 3.2 ng/m L concentrations, respectively. The overall coefficient of variation was 4.3–10.8% in two quality control specimens which were repeatedly measured during a period of 2 months. This method was applied to urine samples collected from children living in B oston, MA . The median concentrations of six detected pyrethroid metabolites ranged from 0.06 to 0.86 ng/m L in urine.