Palit Meehir, Pardasani Deepak, Gupta A K, Dubey D K
Vertox Laboratory, Defence Research and Development Establishment, Gwalior, India.
Anal Chem. 2005 Jan 15;77(2):711-7. doi: 10.1021/ac0486948.
Retrospective detection and identification of chemical warfare agents (CWAs) is important from the verification point of view of the Chemical Weapons Convention. In the present work, a novel method for determination of CWAs and their markers in water has been described. It is based on a single drop micro extraction (SDME) of analytes and gas chromatography/mass spectrometric identification. Extraction conditions, such as solvent selection, agitation, extraction time, and salt content, were found to have significant influence on SDME. The conditions optimized for extraction of CWAs were 1 microL CH2Cl2/CCl4 (3:1 v/v), 30-min extraction time, 300-rpm stirring rate, and with or without NaCl addition. Under optimized conditions, comparison of SDME, solid-phase microextraction, and liquid-liquid extraction was also made. The limit of detection by SDME ranged from 75 to 10 microg L(-1) at a signal-to-noise ratio of 10:1.
从《化学武器公约》核查的角度来看,化学战剂(CWAs)的回顾性检测与识别十分重要。在当前工作中,已描述了一种测定水中化学战剂及其标志物的新方法。该方法基于分析物的单滴微萃取(SDME)以及气相色谱/质谱鉴定。发现萃取条件,如溶剂选择、搅拌、萃取时间和盐含量,对单滴微萃取有显著影响。针对化学战剂萃取优化的条件为1微升二氯甲烷/四氯化碳(3:1 v/v)、30分钟萃取时间、300转/分钟搅拌速率,以及添加或不添加氯化钠。在优化条件下,还对单滴微萃取、固相微萃取和液 - 液萃取进行了比较。在信噪比为10:1时,单滴微萃取的检测限范围为75至10微克/升。