Determination of trace levels of pyrethroid metabolites in human urine by capillary gas chromatography-high resolution mass spectrometry with negative chemical ionization |
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Authors: | G Leng K -H Kühn A Leng W Gries J Lewalter H Idel |
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Institution: | 1. Institute of Hygiene, University of Düsseldorf, Moorenstra?e 5, 40225, Düsseldorf, Germany 2. Department of Medicine, Bayer AG, Building L9, 51368, Leverkusen, Germany
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Abstract: | Summary Applications of high-resolution gas chromatography and high-resolution mass spectrometry (GC-MS) for identification and quantitation
of trace amounts of pyrethroid metabolites in human urine samples are demonstrated. The method covers the pyrethroid metabolitescis- andtrans-3-(2,2-dichlorovinyl)-2,2-dimethyl-cyclopropane carboxylic acid (cis- andtrans-DCCA),cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane carboxylic acid (cis-DBCA), 4-fluoro-3-phenoxybenzoic acid (FPBA), and 3-phenoxybenzoic acid (3-PBA). After acid-induced hydrolysis of urine samples
and exhaustive solvent extraction, a carbodiimide-coupled esterification of the free carboxylic acids with hexafluoroisopropanol
(HFIP) is applied. Identification of the derivatives formed is achieved by low-resolution electron-impact mass spectrometry
(EIMS) using an ion-trap detector. Quantitation was by capillary gas chromatography—high-resolution mass spectrometry using
negative chemical ionization (GC-NCIMS). 2-Phenoxybenzoic acid (2-PBA) served as internal standard. The limits of detection
forcis- andtrans-DCCA,cis-DBCA, FPBA and 3-PBA were 0.03 μg L−1 or below. The applicability of the presented method was tested on urine samples of persons exposed to low levels of pyrethroids. |
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Keywords: | Capillary gas chromatography Pyrethroid metabolites in urine High-resolution mass spectrometry Negative chemical ionization (NCI) Electron-impact ionization (EI) Hexafluoroisopropyl (HFIP) ester |
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