title: Magnetic hydrophilic-lipophilic balance sorbent for efficient extraction of chemical warfare agents from water samples.
abstract: Magnetic hydrophilic-lipophilic balance (MHLB) hybrid resin was prepared by precipitation polymerization using N-vinylpyrrolidone (PVP) and divinylbenzene (DVB) as monomers and Fe2O3 nanoparticles as magnetic material. These resins were successfully applied for the extraction of chemical warfare agents (CWAs) and their markers from water samples through magnetic dispersive solid-phase extraction (MDSPE). By varying the ratios of monomers, resin with desired hydrophilic-lipophilic balance was prepared for the extraction of CWAs and related esters of varying polarities. Amongst different composites Fe2O3 nanoparticles coated with 10% PVP+90% DVB exhibited the best recoveries varying between 70.32 and 97.67%. Parameters affecting the extraction efficiencies, such as extraction time, desorption time, nature and volume of desorption solvent, amount of extraction sorbent and the effect of salts on extraction were investigated. Under the optimized conditions, linearity was obtained in the range of 0.5-500 ng mL(-1) with correlation ranging from 0.9911-0.9980. Limits of detection and limits of quantification were 0.5-1.0 and 3.0-5.0 ng mL(-1) respectively with RSDs varying from 4.88-11.32% for markers of CWAs. Finally, the developed MDSPE method was employed for extraction of analytes from water samples of various sources and the OPCW proficiency test samples.
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Varoon
authors.initials: V
authors.lastname: Singh
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Ajay Kumar
authors.initials: AK
authors.lastname: Purohit
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Sridhar
authors.initials: S
authors.lastname: Chinthakindi
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Raghavender
authors.initials: R
authors.lastname: Goud D
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Vijay
authors.initials: V
authors.lastname: Tak
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Deepak
authors.initials: D
authors.lastname: Pardasani
authors.affiliation: Electron Microscopy Division, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India.
authors.forename: Anchal Roy
authors.initials: AR
authors.lastname: Shrivastava
authors.affiliation: Vertox Laboratory, Defence Research and Development Establishment, Jhansi road, Gwalior 474002, India. Electronic address: dkdubey@rediffmail.com.
authors.forename: Devendra Kumar
authors.initials: DK
authors.lastname: Dubey
mesh_terms: D002619:Chemical Warfare Agents / Q000032:analysis / Q000302:isolation & purification*; D005290:Ferric Compounds / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D057927:Hydrophobic and Hydrophilic Interactions; D057230:Limit of Detection; D060328:Magnetic Phenomena; D011760:Pyrrolidinones / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D002619:Chemical Warfare Agents; D005290:Ferric Compounds; D011760:Pyrrolidinones; D014874:Water Pollutants, Chemical; C042670:N-vinyl-2-pyrrolidinone
keywords: Chemical warfare agents; GC–MS; Hydrophilic–lipophilic balance resin; Magnetic nanoparticles; Sample preparation