Document Detail


The determination of organophosphonate nerve agent metabolites in human urine by hydrophilic interaction liquid chromatography tandem mass spectrometry.
MedLine Citation:
PMID:  17289448     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
A sensitive, robust isotope dilution LC/MS/MS method is presented for the quantitative analysis of human urine for the alkyl methylphosphonic acid metabolites of five organophosphorus nerve agents (VX, rVX or VR, GB or Sarin, GD or Soman, and GF or Cyclosarin). The selective sample preparation method employs non-bonded silica solid-phase extraction and is partially automated. While working with a mobile phase composition that enhances the electrospray ionization process, the hydrophilic interaction chromatography method results in a 5-min injection-to-injection cycle time, excellent peak shapes and adequate retention (k'=3.1). These factors lead to limits of detection for these metabolites as low as 30 pg/mL in a 1-mL sample of human urine. The quality control data (15 and 75 ng/mL) demonstrate accurate (-0.5 to +3.4%) and precise (coefficients of variation of 2.1-3.6%) quantitative results over the clinically relevant urine concentration range of 1-200 ng/mL for a validation set of 20 standard and quality control sets prepared by five analysts over 54 days. The selectivity of the method is demonstrated for a 100-individual reference range study, as well as the analysis of relevant biological samples. The combined sample preparation and analysis portions of this method have a throughput of 288 samples per day.
Authors:
Douglas B Mawhinney; Elizabeth I Hamelin; Rheaclare Fraser; Sathya S Silva; Antonis J Pavlopoulos; Robert J Kobelski
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Publication Detail:
Type:  Journal Article; Validation Studies     Date:  2007-01-26
Journal Detail:
Title:  Journal of chromatography. B, Analytical technologies in the biomedical and life sciences     Volume:  852     ISSN:  1570-0232     ISO Abbreviation:  J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.     Publication Date:  2007 Jun 
Date Detail:
Created Date:  2007-06-04     Completed Date:  2007-08-01     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101139554     Medline TA:  J Chromatogr B Analyt Technol Biomed Life Sci     Country:  Netherlands    
Other Details:
Languages:  eng     Pagination:  235-43     Citation Subset:  IM    
Affiliation:
National Center for Environmental Health, Division of Laboratory Sciences, Emergency Response and Air Toxicants, U.S. Centers for Disease Control and Prevention, 4770 Buford Highway NE, Mailstop F-44, Atlanta, GA 30341, USA. dmawhinney@cdc.gov
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MeSH Terms
Descriptor/Qualifier:
Chemical Warfare Agents / analysis*
Chromatography, High Pressure Liquid / methods*
Humans
Organophosphorus Compounds / urine*
Sensitivity and Specificity
Spectrometry, Mass, Electrospray Ionization / methods
Tandem Mass Spectrometry / methods*
Urine / chemistry*
Chemical
Reg. No./Substance:
0/Chemical Warfare Agents; 0/Organophosphorus Compounds

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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