Dubey D K, Pardasani Deepak, Gupta A K, Palit Meehir, Kanaujia Pankaj K, Tak Vijay
Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior 474002, India.
J Chromatogr A. 2006 Feb 24;1107(1-2):29-35. doi: 10.1016/j.chroma.2005.12.095. Epub 2006 Jan 19.
Unambiguous detection and identification of chemical warfare agents (CWAs) and related compounds are of paramount importance from verification point of view of Chemical Weapons Convention (CWC). It requires development of fast, reliable, simple and reproducible sample preparation of CWAs from water which is likely to be contaminated during deliberate or inadvertent spread of CWAs. This work describes development of hollow fiber liquid-phase microextraction (HF-LPME) method for efficient extraction of CWAs (such as sarin, sulfur mustard and their analogues) from water followed by gas chromatography-mass spectrometric analysis. Extraction parameters, such as organic solvent, agitation, extraction time, and salt concentration were optimized. Best recoveries of target analytes were achieved using 1 microL trichloroethylene as extracting solvent, 1000 rpm stirring rate, 15 min extraction time, and 30% NaCl. Excellent precision was observed with less than 7.6% RSD. The limit of detection by HF-LPME was achieved up to 0.1 microg/L at 30% salt concentration.
从《化学武器公约》（CWC）的核查角度来看，明确检测和识别化学战剂（CWA）及其相关化合物至关重要。这需要开发快速、可靠、简单且可重现的方法，用于从可能在化学战剂蓄意或意外扩散过程中受到污染的水中制备CWA样本。本文描述了中空纤维液相微萃取（HF-LPME）方法的开发，该方法用于从水中高效萃取CWA（如沙林、芥子气及其类似物），随后进行气相色谱-质谱分析。对萃取参数，如有机溶剂、搅拌、萃取时间和盐浓度进行了优化。使用1微升三氯乙烯作为萃取溶剂、1000转/分钟的搅拌速度、15分钟的萃取时间和30%的氯化钠，可实现目标分析物的最佳回收率。观察到精密度极佳，相对标准偏差（RSD）小于7.6%。在30%的盐浓度下，HF-LPME的检测限可达0.1微克/升。
