PMID- 19481219 OWN - NLM STAT- MEDLINE DCOM- 20090806 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1216 IP - 27 DP - 2009 Jul 3 TI - On-line high-performance liquid chromatography-ultraviolet-nuclear magnetic resonance method of the markers of nerve agents for verification of the Chemical Weapons Convention. PG - 5228-34 LID - 10.1016/j.chroma.2009.05.005 [doi] AB - This paper details an on-flow liquid chromatography-ultraviolet-nuclear magnetic resonance (LC-UV-NMR) method for the retrospective detection and identification of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the markers of the toxic nerve agents for verification of the Chemical Weapons Convention (CWC). Initially, the LC-UV-NMR parameters were optimized for benzyl derivatives of the APAs and AAPAs. The optimized parameters include stationary phase C(18), mobile phase methanol:water 78:22 (v/v), UV detection at 268nm and (1)H NMR acquisition conditions. The protocol described herein allowed the detection of analytes through acquisition of high quality NMR spectra from the aqueous solution of the APAs and AAPAs with high concentrations of interfering background chemicals which have been removed by preceding sample preparation. The reported standard deviation for the quantification is related to the UV detector which showed relative standard deviations (RSDs) for quantification within +/-1.1%, while lower limit of detection upto 16mug (in mug absolute) for the NMR detector. Finally the developed LC-UV-NMR method was applied to identify the APAs and AAPAs in real water samples, consequent to solid phase extraction and derivatization. The method is fast (total experiment time approximately 2h), sensitive, rugged and efficient. FAU - Mazumder, Avik AU - Mazumder A AD - Vertox Laboratory, Defence Research and Development Establishment, Gwalior 474002, India. FAU - Gupta, Hemendra K AU - Gupta HK FAU - Garg, Prabhat AU - Garg P FAU - Jain, Rajeev AU - Jain R FAU - Dubey, Devendra K AU - Dubey DK LA - eng PT - Evaluation Study PT - Journal Article DEP - 20090513 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Chemical Warfare Agents) SB - IM MH - Chemical Warfare Agents/*chemistry MH - Chromatography, High Pressure Liquid/instrumentation/*methods MH - Magnetic Resonance Spectroscopy/*methods MH - Online Systems/instrumentation MH - Sensitivity and Specificity EDAT- 2009/06/02 09:00 MHDA- 2009/08/07 09:00 CRDT- 2009/06/02 09:00 PHST- 2009/02/23 00:00 [received] PHST- 2009/04/16 00:00 [revised] PHST- 2009/05/07 00:00 [accepted] PHST- 2009/06/02 09:00 [entrez] PHST- 2009/06/02 09:00 [pubmed] PHST- 2009/08/07 09:00 [medline] AID - S0021-9673(09)00708-0 [pii] AID - 10.1016/j.chroma.2009.05.005 [doi] PST - ppublish SO - J Chromatogr A. 2009 Jul 3;1216(27):5228-34. doi: 10.1016/j.chroma.2009.05.005. Epub 2009 May 13.