title: Single vial sample preparation of markers of nerve agents by dispersive solid-phase extraction using magnetic strong anion exchange resins.
abstract: A sample preparation method involving extraction, enrichment and derivatization of acidic degradation products of nerve agents was developed using magnetic strong anion exchange resins (MSAX). The method was performed in a single vial involving magnetic dispersive solid phase extraction (MDSPE). Analytes were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) in the presence of resins. MSAX were custom synthesized using Fe3O4 nanoparticles as core, 4-vinylpyridine-co-divinylbenzene as polymer shell and quaternary pyridinium function as anion-exchanger. Hydroxide ions were the counter-anions of MSAX to effectively capture the acidic alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs). Quantitative measurements of analytes were performed in the selected ion monitoring mode of GC-MS. Full scan mode of analysis was followed for identifications. Under the optimized conditions analytes were recovered in the range of 39.7-98.8% (n=3, relative standard deviations (RSD) from 0.3 to 6.5%). Limits of detection (LODs) were in the range of 0.1-1.1ngmL(-1); and the linear dynamic range was 5-1000ngmL(-1) with r(2) of 0.9977-0.9769. Applicability of the method was tested with rain-, tap-, muddy-water and Organization for Prohibition of Chemical Weapons (OPCW) Proficiency Test samples.
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India.
authors: Varoon
authors: V
authors: Singh
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India.
authors: Sridhar
authors: S
authors: Chinthakindi
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India.
authors: Ajay Kumar
authors: AK
authors: Purohit
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India.
authors: Deepak
authors: D
authors: Pardasani
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India.
authors: Vijay
authors: V
authors: Tak
authors: Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior - 474002, India. Electronic address: dkdubey@rediffmail.com.
authors: Devendra Kumar
authors: DK
authors: Dubey
mesh_terms: D000837:Anion Exchange Resins / Q000737:chemistry*; D002619:Chemical Warfare Agents / Q000032:analysis*; D004784:Environmental Monitoring / Q000379:methods*; D005290:Ferric Compounds / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D060328:Magnetic Phenomena; D053768:Metal Nanoparticles / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D014867:Water / Q000737:chemistry
chemical_list: D000837:Anion Exchange Resins; D002619:Chemical Warfare Agents; D005290:Ferric Compounds; D014867:Water; C000499:ferric oxide
keywords: Alkylalkyl phosphonic acids; Alkylphosphonic acids; Chemical warfare agents; Chemical weapons convention; Derivatization; GC–MS; Magnetic strong anion-exchange resins; Verification