Rapid screening procedures for the hydrolysis products of chemical warfareagents using positive and negative ion liquid chromatography-mass spectrometry with atmospheric pressure chemical ionisation

Qualitative screening procedures have been developed for the rapid detectio n and identification of the hydrolysis products of chemical warfare agents in aqueous samples and extracts, using liquid chromatography-mass spectrome try with positive and negative atmospheric pressure chemical ionisation (AP CI). Previously reported screening procedures, which used positive APCI or electrospray ionisation (ESI), were modified by using LC conditions that al lowed acquisition of positive and negative ion mass spectra. APCI was gener ally found to be more robust than ESI, probably due to variable adduct ion formation with ESI, depending on the condition of the sample and the system . Negative APCI provided selective detection of acidic analytes and allowed facile differentiation of alkyl alkylphosphonic acids from isomeric dialky l alkylphosphonates. The combination of positive and negative APCI, using a C-18 column and water-methanol mobile phase modified with ammonium formate , provides a rapid screening procedure for chemical warfare agent degradati on products, with limits of detectability in the range 10-100 ng/ml. In the case of proficiency test samples, where analyte concentrations are in the range 1-10 ppm, introduction of the sample by infusion may provide an even faster preliminary screening procedure. (C) 1999 Elsevier Science B.V. All rights reserved.