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New gas chromatographic-mass spectrometric method for the determination of urinary pyrethroid metabolites in environmental medicine.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Oct 05; 778(1-2):121-30.JC

Abstract

We have developed and validated a new, reliable and very sensitive method for the determination of the urinary metabolites of the most common pyrethroids in one analytical run. After acidic hydrolysis for the cleavage of conjugates, the analytes cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (cis-Cl(2)CA), trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (trans-Cl(2)CA), cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (Br(2)CA), 4-fluoro-3-phenoxybenzoic acid (F-PBA) and 3-phenoxybenzoic acid (3-PBA) were extracted from the matrix with a liquid-liquid extraction procedure using n-hexane under acidic conditions. For further clean-up, NaOH was added to the organic phase and the carboxylic acids were re-extracted into the aqueous phase. After acidification and extraction into n-hexane again, the metabolites were then derivatised to volatile esters using N-tert.-butyldimethylsilyl-N-methyltrifluoroacetamid (MTBSTFA). Separation and detection were carried out using capillary gas chromatography with mass-selective detection (GC-MS). 2-Phenoxybenzoic acid (2-PBA) served as internal standard for the quantification of the pyrethroid metabolites. The limit of detection for all analytes was 0.05 microg/l urine. The RSD of the within-series imprecision was between 2.0 and 5.4% at a spiked concentration of 0.4 microg/l and the relative recovery was between 79.3 and 93.4%, depending on the analyte. This method was used for the analysis of urine samples of 46 persons from the general population without known exposure to pyrethroids. The metabolites cis-Cl(2)CA, trans-Cl(2)CA and 3-PBA could be found in 52, 72 and 70% of all samples with median values of 0.06, 0.11 and 0.16 microg/l, respectively. Br(2)CA and F-PBA could also be detected in 13 and 4% of the urine samples.

Authors+Show Affiliations

Schettgen T
Institute and Outpatient Clinic of Occupational, Social and Environmental Medicine, Friedrich-Alexander-University of Erlangen-Nürnberg, Schillerstrasse 25/29, D-91054 Erlangen, Germany.
Koch HM
No affiliation info available
Drexler H
No affiliation info available
Angerer J
No affiliation info available

MeSH

AdolescentAdultCalibrationEnvironmental MedicineFemaleGas Chromatography-Mass SpectrometryHumansInsecticidesMaleMiddle AgedPyrethrinsReference StandardsReproducibility of ResultsSensitivity and Specificity

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

12376120

Citation

Schettgen, T, et al. "New Gas Chromatographic-mass Spectrometric Method for the Determination of Urinary Pyrethroid Metabolites in Environmental Medicine." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 778, no. 1-2, 2002, pp. 121-30.
Schettgen T, Koch HM, Drexler H, et al. New gas chromatographic-mass spectrometric method for the determination of urinary pyrethroid metabolites in environmental medicine. J Chromatogr B Analyt Technol Biomed Life Sci. 2002;778(1-2):121-30.
Schettgen, T., Koch, H. M., Drexler, H., & Angerer, J. (2002). New gas chromatographic-mass spectrometric method for the determination of urinary pyrethroid metabolites in environmental medicine. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 778(1-2), 121-30.
Schettgen T, et al. New Gas Chromatographic-mass Spectrometric Method for the Determination of Urinary Pyrethroid Metabolites in Environmental Medicine. J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Oct 5;778(1-2):121-30. PubMed PMID: 12376120.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - New gas chromatographic-mass spectrometric method for the determination of urinary pyrethroid metabolites in environmental medicine. AU - Schettgen,T, AU - Koch,H M, AU - Drexler,H, AU - Angerer,J, PY - 2002/10/12/pubmed PY - 2003/4/9/medline PY - 2002/10/12/entrez SP - 121 EP - 30 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 778 IS - 1-2 N2 - We have developed and validated a new, reliable and very sensitive method for the determination of the urinary metabolites of the most common pyrethroids in one analytical run. After acidic hydrolysis for the cleavage of conjugates, the analytes cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (cis-Cl(2)CA), trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (trans-Cl(2)CA), cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (Br(2)CA), 4-fluoro-3-phenoxybenzoic acid (F-PBA) and 3-phenoxybenzoic acid (3-PBA) were extracted from the matrix with a liquid-liquid extraction procedure using n-hexane under acidic conditions. For further clean-up, NaOH was added to the organic phase and the carboxylic acids were re-extracted into the aqueous phase. After acidification and extraction into n-hexane again, the metabolites were then derivatised to volatile esters using N-tert.-butyldimethylsilyl-N-methyltrifluoroacetamid (MTBSTFA). Separation and detection were carried out using capillary gas chromatography with mass-selective detection (GC-MS). 2-Phenoxybenzoic acid (2-PBA) served as internal standard for the quantification of the pyrethroid metabolites. The limit of detection for all analytes was 0.05 microg/l urine. The RSD of the within-series imprecision was between 2.0 and 5.4% at a spiked concentration of 0.4 microg/l and the relative recovery was between 79.3 and 93.4%, depending on the analyte. This method was used for the analysis of urine samples of 46 persons from the general population without known exposure to pyrethroids. The metabolites cis-Cl(2)CA, trans-Cl(2)CA and 3-PBA could be found in 52, 72 and 70% of all samples with median values of 0.06, 0.11 and 0.16 microg/l, respectively. Br(2)CA and F-PBA could also be detected in 13 and 4% of the urine samples. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/12376120/New_gas_chromatographic_mass_spectrometric_method_for_the_determination_of_urinary_pyrethroid_metabolites_in_environmental_medicine_ DB - PRIME DP - Unbound Medicine ER -