Solid supported in situ derivatization extraction of acidic degradation products of nerve agents from aqueous samples

被引:8
作者
Chinthakindi, Sridhar [1 ]
Purohit, Ajay [1 ]
Singh, Varoon [1 ]
Tak, Vijay [1 ]
Dubey, D. K. [1 ]
Pardasani, Deepak [1 ]
机构
[1] Def Res & Dev Estab, Vertox Lab, Gwalior 474002, India
关键词
Chemical Warfare Agents; Alkylphosphonic acids; Silylation; Supported liquid extraction; In situ derivatization; CHEMICAL-WARFARE AGENTS; LIQUID-PHASE MICROEXTRACTION; GAS-CHROMATOGRAPHY; MASS-SPECTROMETRY; ALKYLPHOSPHONIC ACIDS; WATER; SILYLATION;
D O I
10.1016/j.chroma.2014.07.046
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
This study deals with the solid supported in situ derivatization extraction. of acidic degradation products of nerve agents present in aqueous samples. Target analytes were alkyl alkylphosphonic acids and alkylphosphonic acids, which are important environmental signatures of nerve agents. The method involved tert-butyldimethylchlorosilane mediated in situ silylation of analytes on commercially available diatomaceous solid phase extraction cartridges. Various parameters such as derivatizing reagent, its concentration, reaction time, temperature and eluting solvent were optimized. Recoveries of the analytes were determined by GC-MS which ranged from 60% to 86%. The limits of detection (LOD) and limit of quantification (LOQ) with selected analytes were achieved down to 78 and 213 ng mL(-1) respectively, in selected ion monitoring mode. The successful applicability of method was also demonstrated on samples of biological origin such as plasma and to the samples received in 34th official proficiency test conducted by the Organization for Prohibition the of Chemical Weapons. (C) 2014 Elsevier B.V. All rights reserved.
引用
收藏
页码:325 / 329
页数:5
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