Kanaujia Pankaj K, Pardasani Deepak, Gupta A K, Kumar Rajesh, Srivastava R K, Dubey D K
Vertox Laboratory, Defence Research & Development Establishment, Jhansi Road, Gwalior 474002, India.
J Chromatogr A. 2007 Aug 17;1161(1-2):98-104. doi: 10.1016/j.chroma.2007.05.076. Epub 2007 May 31.
The analysis of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the hydrolyzed products of nerve agents, constitutes an important aspect for verifying the compliance to the Chemical weapons convention (CWC). This work devotes on the development of solid-phase extraction method using polymeric mixed-mode strong anion-exchange (Oasis MAX) cartridges for extraction of AAPAs and APAs from water. The extracted analytes were analyzed by GC-MS under full scan and selected ion monitoring mode. The extraction efficiencies of MAX and silica-based anion-exchange cartridges were compared, and results revealed that MAX sorbents yielded better recoveries. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 1 mL of acidic methanol (0.1 M), and limits of detection could be achieved up to 5 x 10(-4) microg mL(-1) (in SIM) and 0.05 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of alkylphosphonic acids present in soil sample sent by the Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests.
神经毒剂的水解产物烷基烷基膦酸（AAPAs）和烷基膦酸（APAs）的分析是核查《化学武器公约》（CWC）履约情况的一个重要方面。本工作致力于开发一种固相萃取方法，该方法使用聚合物混合模式强阴离子交换（Oasis MAX）柱从水中萃取AAPAs和APAs。萃取得到的分析物通过气相色谱 - 质谱联用仪在全扫描和选择离子监测模式下进行分析。比较了MAX柱和硅胶基阴离子交换柱的萃取效率，结果表明MAX吸附剂具有更好的回收率。对诸如负载量、萃取溶剂及其体积以及洗涤溶剂等萃取参数进行了优化。使用1 mL酸性甲醇（0.1 M）可获得最佳回收率，在选择离子监测模式下检测限可达5×10⁻⁴ μg mL⁻¹，在全扫描模式下为0.05 μg mL⁻¹。该方法成功用于检测和鉴定在禁止化学武器组织（OPCW）官方能力验证测试中送检的土壤样品中存在的烷基膦酸。
