Kanaujia Pankaj K, Tak Vijay, Pardasani Deepak, Gupta A K, Dubey D K
Vertox Laboratory, Defence Research & Development Establishment, Jhansi Road, Gwalior 474002, India.
J Chromatogr A. 2008 Mar 28;1185(2):167-77. doi: 10.1016/j.chroma.2008.01.080. Epub 2008 Feb 8.
The analysis of nitrogen containing amino alcohols, which are the precursors and degradation products of nitrogen mustards and nerve agent VX, constitutes an important aspect for verifying the compliance to the CWC (Chemical Weapons Convention). This work devotes on the development of solid-phase extraction method using silica- and polymer-based SCX (strong cation-exchange) and MCX (mixed-mode strong cation-exchange) cartridges for N,N-dialkylaminoethane-2-ols and alkyl N,N-diethanolamines, from water. The extracted analytes were analyzed by GC-MS (gas chromatography-mass spectrometry) in the full scan and selected ion monitoring modes. The extraction efficiencies of SCX and MCX cartridges were compared, and results revealed that SCX performed better. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 2 mL methanol containing 10% NH(4)OH and limits of detection could be achieved up to 5 x 10(-3) microg mL(-1) in the selected ion monitoring mode and 0.01 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of amino alcohol present in water sample sent by Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests. The method was also applied to extract the analytes from human plasma. The SCX cartridge showed good recoveries of amino alcohols from human plasma after protein precipitation.
对含氮氨基醇的分析是核查是否符合《化学武器公约》（CWC）的一个重要方面，含氮氨基醇是氮芥和神经性毒剂VX的前体及降解产物。本研究致力于开发一种固相萃取方法，该方法使用基于硅胶和聚合物的强阳离子交换（SCX）柱和混合模式强阳离子交换（MCX）柱，从水中萃取N,N -二烷基氨基乙烷 - 2 -醇和烷基N,N -二乙醇胺。萃取的分析物通过气相色谱 - 质谱联用仪（GC - MS）在全扫描和选择离子监测模式下进行分析。比较了SCX柱和MCX柱的萃取效率，结果表明SCX柱表现更佳。对萃取参数，如负载量、萃取溶剂及其体积、洗涤溶剂等进行了优化。使用含10% NH₄OH的2 mL甲醇可获得最佳回收率，在选择离子监测模式下检测限可达5×10⁻³ μg mL⁻¹，在全扫描模式下为0.01 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来的水样中存在的氨基醇。该方法还应用于从人血浆中萃取分析物。在蛋白沉淀后，SCX柱对人血浆中的氨基醇显示出良好的回收率。
