title: Solid supported in situ derivatization extraction of acidic degradation products of nerve agents from aqueous samples.
abstract: This study deals with the solid supported in situ derivatization extraction of acidic degradation products of nerve agents present in aqueous samples. Target analytes were alkyl alkylphosphonic acids and alkylphosphonic acids, which are important environmental signatures of nerve agents. The method involved tert-butyldimethylchlorosilane mediated in situ silylation of analytes on commercially available diatomaceous solid phase extraction cartridges. Various parameters such as derivatizing reagent, its concentration, reaction time, temperature and eluting solvent were optimized. Recoveries of the analytes were determined by GC-MS which ranged from 60% to 86%. The limits of detection (LOD) and limit of quantification (LOQ) with selected analytes were achieved down to 78 and 213ngmL(-1) respectively, in selected ion monitoring mode. The successful applicability of method was also demonstrated on samples of biological origin such as plasma and to the samples received in 34th official proficiency test conducted by the Organization for Prohibition the of Chemical Weapons.
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
authors.forename: Sridhar
authors.initials: S
authors.lastname: Chinthakindi
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
authors.forename: Ajay
authors.initials: A
authors.lastname: Purohit
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
authors.forename: Varoon
authors.initials: V
authors.lastname: Singh
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
authors.forename: Vijay
authors.initials: V
authors.lastname: Tak
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
authors.forename: D K
authors.initials: DK
authors.lastname: Dubey
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India. Electronic address: dkpardasani@drde.drdo.in.
authors.forename: Deepak
authors.initials: D
authors.lastname: Pardasani
mesh_terms: D000818:Animals; D002619:Chemical Warfare Agents / Q000032:analysis* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D051379:Mice; D010949:Plasma / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification*
chemical_list: D002619:Chemical Warfare Agents; D014874:Water Pollutants, Chemical
keywords: Alkylphosphonic acids; Chemical Warfare Agents; In situ derivatization; Silylation; Supported liquid extraction