PMID- 27113675 OWN - NLM STAT- MEDLINE DCOM- 20161226 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1448 DP - 2016 May 27 TI - Analysis of chemical warfare agents in organic liquid samples with magnetic dispersive solid phase extraction and gas chromatography mass spectrometry for verification of the chemical weapons convention. PG - 32-41 LID - S0021-9673(16)30498-8 [pii] LID - 10.1016/j.chroma.2016.04.058 [doi] AB - A simple, sensitive and low temperature sample preparation method is developed for detection and identification of Chemical Warfare Agents (CWAs) and scheduled esters in organic liquid using magnetic dispersive solid phase extraction (MDSPE) followed by gas chromatography-mass spectrometry analysis. The method utilizes Iron oxide@Poly(methacrylic acid-co-ethylene glycol dimethacrylate) resin (Fe2O3@Poly(MAA-co-EGDMA)) as sorbent. Variants of these sorbents were prepared by precipitation polymerization of methacrylic acid-co-ethylene glycol dimethacrylate (MAA-co-EGDMA) onto Fe2O3 nanoparticles. Fe2O3@poly(MAA-co-EGDMA) with 20% MAA showed highest recovery of analytes. Extractions were performed with magnetic microspheres by MDSPE. Parameters affecting the extraction efficiency were studied and optimized. Under the optimized conditions, method showed linearity in the range of 0.1-3.0mugmL(-1) (r(2)=0.9966-0.9987). The repeatability and reproducibility (relative standard deviations (RSDs) %) were in the range of 4.5-7.6% and 3.4-6.2% respectively for organophosphorous esters in dodecane. Limits of detection (S/N=3/1) and limit of quantification (S/N=10/1) were found to be in the range of 0.05-0.1mugmL(-1) and 0.1-0.12mugmL(-1) respectively in SIM mode for selected analytes. The method was successfully validated and applied to the extraction and identification of targeted analytes from three different organic liquids i.e. n-hexane, dodecane and silicon oil. Recoveries ranged from 58.7 to 97.3% and 53.8 to 95.5% at 3mugmL(-1) and 1mugmL(-1) spiking concentrations. Detection of diethyl methylphosphonate (DEMP) and O-Ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX) in samples provided by the Organization for Prohibition of Chemical Weapons Proficiency Test (OPCW-PT) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. CI - Copyright (c) 2016 Elsevier B.V. All rights reserved. FAU - Singh, Varoon AU - Singh V AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Purohit, Ajay Kumar AU - Purohit AK AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Chinthakindi, Sridhar AU - Chinthakindi S AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Goud, Raghavender D AU - Goud RD AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Tak, Vijay AU - Tak V AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Pardasani, Deepak AU - Pardasani D AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Shrivastava, Anchal Roy AU - Shrivastava AR AD - Electron Microscopy Division, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. FAU - Dubey, Devendra Kumar AU - Dubey DK AD - Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. Electronic address: dkdubey@rediffmail.com. LA - eng PT - Journal Article DEP - 20160420 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Alkanes) RN - 0 (Chemical Warfare Agents) RN - 0 (Ferric Compounds) RN - 0 (Hexanes) RN - 0 (Organophosphonates) RN - 0 (Organothiophosphorus Compounds) RN - 0 (Polymethacrylic Acids) RN - 0 (Silicone Oils) RN - 0 (poly((ethylene glycol dimethacrylate)-co-(methacrylic acid))) RN - 11A386X1QH (n-dodecane) RN - 1K09F3G675 (ferric oxide) RN - 2DDG612ED8 (n-hexane) SB - IM MH - Alkanes/*chemistry MH - Chemical Warfare Agents/*analysis MH - Ferric Compounds/chemistry MH - Gas Chromatography-Mass Spectrometry/instrumentation/methods MH - Hexanes/*chemistry MH - Magnetics MH - Organophosphonates/*analysis MH - Organothiophosphorus Compounds/*analysis MH - Polymethacrylic Acids/chemistry MH - Reproducibility of Results MH - Silicone Oils/*chemistry MH - Solid Phase Extraction/methods OTO - NOTNLM OT - Chemical warfare agents OT - Chemical weapons convention OT - GC-MS OT - Magnetic dispersive solid phase extraction OT - Magnetic nanoparticles OT - Sample preparation EDAT- 2016/04/27 06:00 MHDA- 2016/12/27 06:00 CRDT- 2016/04/27 06:00 PHST- 2016/02/10 00:00 [received] PHST- 2016/04/05 00:00 [revised] PHST- 2016/04/19 00:00 [accepted] PHST- 2016/04/27 06:00 [entrez] PHST- 2016/04/27 06:00 [pubmed] PHST- 2016/12/27 06:00 [medline] AID - S0021-9673(16)30498-8 [pii] AID - 10.1016/j.chroma.2016.04.058 [doi] PST - ppublish SO - J Chromatogr A. 2016 May 27;1448:32-41. doi: 10.1016/j.chroma.2016.04.058. Epub 2016 Apr 20.