Direct derivatization and rapid GC-MS screening of nerve agent markers in aqueous samples

Subramaniam, RajaUmeå universitet,Kemiska institutionen,The Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden (författare)

A rapid screening and identification method based on derivatization and gas chromatography mass spectrometry (GC-MS) has been developed for the detection of alkylphosphonic acids (APAs), the degradation products of organophosphorus nerve agents. The novel method described involves rapid (5 min) and direct derivatization of 25 muL aqueous sample using highly fluorinated phenyldiazomethane reagents (e.g., 1-(diazomethyl)-3,5-bis(trifluoromethyl)benzene). The APA derivatives are then screened by GC-MS negative ion chemical ionization (NICI) and identified by electron ionization (EI) mode. The conditions for the derivatization were optimized using statistical experimental design and multivariate data analysis. Method robustness was evaluated using aqueous samples from an official OPCW Proficiency Test and all APAs present in the sample were conclusively identified. Limits of detection for rapid screening using SIM NICI were between 5 and 10 ng/mL APA in aqueous sample, and for identification using full scan EI 100 ng/mL.

Åstot, CristerThe Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden (författare)
Juhlin, LarsThe Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden (författare)
Nilsson, CalleThe Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden (författare)
Östin, AndersThe Swedish Defence Research Agency, FOI CBRN Defence and Security, SE-901 82 Umeå, Sweden,Swedish Armed Forces, National CBRN-Defence Centre, SE-901 76 Umeå, Sweden (författare)
Umeå universitetKemiska institutionen (creator_code:org_t)

Ingår i:Analytical Chemistry: American Chemical Society (ACS)82:17, s. 7452-74590003-27001520-6882

Av författaren/redakt...: Subramaniam, Raj ...; Åstot, Crister; Juhlin, Lars; Nilsson, Calle; Östin, Anders

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