用于《化学武器公约》核查的氮芥和硫芥前体三氟乙酰衍生物的气相色谱-质谱分析

Gas chromatography-mass spectrometry analysis of trifluoroacetyl derivatives of precursors of nitrogen and sulfur mustards for verification of chemical weapons convention.

作者信息

Pardasani Deepak, Palit Meehir, Gupta A K, Kanaujia Pankaj K, Dubey D K

机构信息

Vertox Laboratory, Defence Research and Development Establishment, Jhansi Road, Gwalior 474002, India.

出版信息

J Chromatogr A. 2004 Dec 3;1059(1-2):157-64. doi: 10.1016/j.chroma.2004.10.039.

DOI:10.1016/j.chroma.2004.10.039

PMID:15628136

Abstract

Trifluoroacetylation reactions were optimized for gas chromatography-mass spectrometric (GC-MS) analysis of precursors of nitrogen and sulfur mustards using newly developed N-trifluoroacetylbenzimidazole (TFABI) and known N-trifluoroacetylimidazole (TFAI) and N-trifluoroacetylbenzotriazole (TFABT) reagents. TFAI and TFABI gave the best results in terms of yields and reaction time. Trifluoroacetyl derivatives showed clean total ion chromatograms in GC-MS analysis than trimethylsilyl (TMS) derivatives. The negative ion chemical ionization analysis of these derivatives gave pseudo molecular weight information, with low limit of detection.

摘要

利用新开发的N-三氟乙酰苯并咪唑（TFABI）以及已知的N-三氟乙酰咪唑（TFAI）和N-三氟乙酰苯并三唑（TFABT）试剂，对用于氮芥和硫芥前体的气相色谱-质谱（GC-MS）分析的三氟乙酰化反应进行了优化。就产率和反应时间而言，TFAI和TFABI给出了最佳结果。在GC-MS分析中，三氟乙酰衍生物的总离子色谱图比三甲基硅烷基（TMS）衍生物的更清晰。这些衍生物的负离子化学电离分析给出了准分子量信息，检测限较低。