title: Extraction and derivatization of chemical weapons convention relevant aminoalcohols on magnetic cation-exchange resins.
abstract: Analysis and identification of nitrogen containing aminoalcohols is an integral part of the verification analysis of chemical weapons convention (CWC). This study was aimed to develop extraction and derivatization of aminoalcohols of CWC relevance by using magnetic dispersive solid-phase extraction (MDSPE) in combination with on-resin derivatization (ORD). For this purpose, sulfonated magnetic cation-exchange resins (SMRs) were prepared using magnetite nanoparticles as core, styrene and divinylbenzene as polymer coat and sulfonic acid as acidic cation exchanger. SMRs were successfully employed as extractant for targeted basic analytes. Adsorbed analytes were derivatized with hexamethyldisilazane (HMDS) on the surface of extractant. Derivatized (silylated) compounds were analyzed by GC-MS in SIM and full scan mode. The linearity of the method ranged from 5 to 200ngmL(-1). The LOD and LOQ ranged from 2 to 6ngmL(-1) and 5 to 19ngmL(-1) respectively. The relative standard deviation for intra-day repeatability and inter-day intermediate precision ranged from 5.1% to 6.6% and 0.2% to 7.6% respectively. Recoveries of analytes from spiked water samples from different sources varied from 28.4% to 89.3%.
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: Prabhat
authors.initials: P
authors.lastname: Garg
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: Vijay
authors.initials: V
authors.lastname: Tak
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India. Electronic address: dkdubey@rediffmail.com.
authors.forename: Devendra Kumar
authors.initials: DK
authors.lastname: Dubey
mesh_terms: D000327:Adsorption; D000605:Amino Alcohols / Q000302:isolation & purification*; D002411:Cation Exchange Resins / Q000737:chemistry; D002412:Cations / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D008280:Magnetics; D008855:Microscopy, Electron, Scanning; D052616:Solid Phase Extraction / Q000379:methods; D017550:Spectroscopy, Fourier Transform Infrared
chemical_list: D000605:Amino Alcohols; D002411:Cation Exchange Resins; D002412:Cations
keywords: Aminoalcohols; Chemical weapons convention; Derivatization; GC–MS; Magnetic cation-exchange resins