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Determination of hydrolytic degradation products of nerve agents by injection port fluorination in gas chromatography/mass spectrometry for the verification of the Chemical Weapons Convention
Author(s) -
Pardasani Deepak,
Mazumder Avik,
Gupta Arvinda K.,
Kanaujia Pankaj K.,
Tak Vijay,
Dubey Devendra K.
Publication year - 2007
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.3196
Subject(s) - chemistry , trifluoroacetic anhydride , injection port , derivatization , mass spectrometry , chromatography , gas chromatography–mass spectrometry , gas chromatography , trifluoroacetic acid , hydrolysis , organic chemistry , medicine , surgery
Retrospective detection and identification of markers of chemical warfare agents are important aspects of verification of the Chemical Weapons Convention. Alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs) are important markers of nerve agents. We describe the development and optimization of a new gas chromatography/mass spectrometry (GC/MS) injection port fluorination method for the derivatization of AAPAs and APAs. The process involved the injection of acids with trifluoroacetic anhydride in GC/MS, where acids are converted into their corresponding volatile fluorides. Various reaction conditions such as fluorinating agent, injection port temperature and splitless time were optimized. The maximum reaction efficiency of the acids with trifluoroacetic anhydride was observed at 230°C injection port temperature with a splitless time of 2 min. APAs showed best analytical efficiencies at 400°C injection port temperature, while the other conditions were similar to those of AAPAs. The linearities of response for APAs and AAPAs were in the range of 1–25 and 5–100 µg mL −1 , respectively, with limits of detection ranging from 500 pg to 800 ng mL −1 . Copyright © 2007 John Wiley & Sons, Ltd.