Direct derivatization and trace determination of nerve agent biomarkers in urine samples
(English)Manuscript (preprint) (Other (popular science, discussion, etc.))
A rapid direct derivatization and gas chromatography mass spectrometry (GC-MS) method has been developed for the determination of alkylphosphonic acids (APAs) in urine, which act as biomarkers of organophosphorus nerve agents. The method involves rapid (5 min) and direct derivatization of acidified urine samples (25 μL) using the highly fluorinated phenyldiazomethane reagent [1-(diazomethyl)-3,5-bis(trifluoromethyl)benzene]. The APA derivatives are then trapped on reversed-phase C18 bonded silica to remove any underivatized APAs and HCl in the sample solution. After elution, the APA derivatives are then determined by low resolution mass spectrometry using negative ion chemical ionization single ion monitoring.The selectivity of the method was further improved by using high resolution negative ion chemical ionization selected ion monitoring on a double focusing magnetic sector mass spectrometer. High sensitivity was obtained with limits of detection ranging from 0.1 to 10 ng/mL of the APAs (in urine) for both techniques. The conditions for the derivatization were optimized using statistical experimental design and multivariate data analysis. Based on the current results and earlier work on APAs in water using the direct derivatization approach, we conclude that the method offers excellent performance and is viable for the simultaneous trace determination of a wide range of nerve agent markers.
Biomarkers, nerve agents
Research subject Analytical Chemistry
IdentifiersURN: urn:nbn:se:umu:diva-54641OAI: oai:DiVA.org:umu-54641DiVA: diva2:524692