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《化学分析计量》 2022年第06期
DOI:10.3969/j.issn.1008-6145.2022.06.010
超分子溶剂萃取-气相色谱-质谱法测定水中神经性毒剂及其模拟剂
唐慧,陈博,黄永鹏,陈茜,孟祥燕
国民核生化灾害防护国家重点实验室,北京 102205 
Determination of nerve agents and stimulant in water by supramolecular solvent extraction and gas chromatography-mass spectrometry
TANG Hui, CHEN Bo, HUANG Yongpeng, CHEN Xi, MENG Xiangyan
State Key Laboratory of NBC Protection for Civilian, Bejing 102205, China 
摘要:建立了水中神经性毒剂沙林、梭曼及其模拟剂甲基磷酸二甲酯的超分子溶剂萃取-气相色谱-质谱分析方法。以聚氧乙烯单叔辛苯基醚在水中自组装形成水相胶束的超分子溶剂为萃取剂,对水样中的沙林、梭曼及其模拟剂甲基磷酸二甲酯进行液液微萃取,再通过异辛烷进行微波萃取分析。采用单因素试验考察了超分子溶液组成、用量、涡旋时间、离子强度等参数对萃取率的影响。实验结果表明:沙林、梭曼、甲基磷酸二甲酯的质量浓度在0.040~50μg/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.999,检出限为0.2~0.8 ng/mL,定量限为0.4~2.0 ng/mL,样品加标回收率为80.7%~89.3%,测定结果的相对标准偏差为5.87%~9.26%(n=6)。该方法有机溶剂用量少、环境友好、准确可靠、快速稳定,可用于水中神经性毒剂的测定。 
Abstract:A method for the determination of nerve agents sarin, soman and their simulant called dimethyl methylphosponate (DMMP) in water by gas chromatography-mass spectrometry with supramolecular solvent extraction was developed. Liquid-liquid microextraction of sarin, soman and their simulant DMMP from water samples was carried out with a supramolecular solvent, which was self-assembled into an aqueous micelle by polyethylene glycol octylphenyl ether, then microwave extraction was carried out by isooctane. The effects of composition, dosage of supramolecular solution, vortex time and ionic strength on the extraction rate were investigated by single factor experiment. The mass concentration of sarin, soman and DMMP had a good linear relationship with the chromatographic peak area in the range of 0.040-50μg/mL, the correlation coefficient were all more than 0.999, the limit of detection and quantitation were 0.2-0.8 ng/mL and 0.4-2.0 ng/mL, respectively. The recovery rate ranged from 80.7% to 89.3%, the relative standard deviations of n determination results were 5.87%-9.26%( =6). The method is accurate, rapid and environmentally friendly, which used less extractant, reliable, and it can be used for the determination of nerve agent in water. 
关键词:神经性毒剂;超分子溶剂;气相色谱-质谱法 
Keywords:nerve agents; supramolecular solvent; gas chromatography-mass spectrometry 
本文引用格式:
唐慧,陈博,黄永鹏,等.超分子溶剂萃取-气相色谱-质谱法测定水中神经性毒剂及其模拟剂[J].化学分析计量,2022,31(6):41.
TANG Hui,CHEN Bo,HUANG Yongpeng,et al. Determination of nerve agents and stimulant in water by supramolecular solvent extraction and gas chromatography-mass spectrometry[J]. Chemical Analysis and Meterage,2022,31(6):41. 

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