title: On-line solid phase extraction-liquid chromatography-mass spectrometry for trace determination of nerve agent degradation products in water samples.
abstract: Three primary nerve agent degradation products (ethyl-, isopropyl- and pinacolyl methylphosphonic acid) have been determined in water samples using on-line solid phase extraction-liquid chromatography and mass spectrometry (SPE-LC-MS) with electrospray ionisation. Porous graphitic carbon was employed for analyte enrichment followed by hydrophilic interaction chromatography. Diethylphosphate was applied as internal standard for quantitative determination of the alkyl methylphosphonic acids (AMPAs). By treating the samples with strong cation-exhange columns on Ba, Ag and H form, the major inorganic anions in water were removed by precipitation prior to the SPE-LC-MS determination. The AMPAs could be determined in tap water with limits of detection of 0.01-0.07 μg L(-1) with the [M-H](-) ions extracted at an accuracy of ±5 mDa. The within and between assay precisions at analyte concentrations of 5 μg L(-1) were 2-3%, and 5-9% relative standard deviation, respectively. The developed method was employed for determination of the AMPAs in three natural waters and a simulated waste water sample, spiked at 5 μg L(-1). Recoveries of ethyl-, isopropyl- and pinacolyl methylphosphonic acid were 80-91%, 92-103% and 99-106%, respectively, proving the applicability of the technique for natural waters of various origins.
authors: Norwegian Defence Research Establishment (FFI), P.O. Box 25, NO-2027 Kjeller, Norway. Bent-Tore.Roen@ffi.no
authors: Bent T
authors: BT
authors: Røen
authors: Stig R
authors: SR
authors: Sellevåg
authors: Elsa
authors: E
authors: Lundanes
mesh_terms: D002619:Chemical Warfare Agents / Q000032:analysis* / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods; D004867:Equipment Design; D005618:Fresh Water / Q000032:analysis; D006108:Graphite / Q000737:chemistry; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000295:instrumentation / Q000379:methods; D063065:Organophosphonates / Q000032:analysis* / Q000302:isolation & purification; D009943:Organophosphorus Compounds / Q000032:analysis* / Q000302:isolation & purification; D016062:Porosity; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D012999:Soman / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification; D014867:Water / Q000032:analysis; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D002619:Chemical Warfare Agents; D063065:Organophosphonates; D009943:Organophosphorus Compounds; D014874:Water Pollutants, Chemical; D014867:Water; C108318:ethyl methylphosphonic acid; C048760:isopropyl methylphosphonic acid; C046573:pinacolyl methylphosphonic acid; D006108:Graphite; D012999:Soman