Analysis of mustard hydrolysis products by packed capillary liquid chromatography electrospray mass spectrometry

Packed capillary column liquid chromatography (LC)-electrospray mass spectrometry (ESI-MS) was used to identify munitions grade mustard hydrolysis products, including five longer chain diols, two partial hydrolysis products and three ether/thioether macrocycles. All ESI-MS data were collected under collisionally activated dissociation (CAD) conditions optimized to facilitate acquisition of both molecular and product ion information that could be used for structural identification purposes. Interpretation of the ESI-MS data enabled characterization of the diols resulting from hydrolysis of all three principal sulfur vesicants, bis(2-chloroethyl)sulfide (mustard or H), bis(2-chloroethylthio)ethane (sesquimustard or Q) and bis[(2-chloroethylthio)ethyl] ether (T), as well as novel products not previously associated with sulfur vesicant hydrolysis. The developed packed capillary LC-ESI-MS method was successfully applied to the analysis of aqueous samples collected at a former mustard destruction site. Both thiodiglycol and the hydrolysis product of T, 6-oxa-3,9-dithia-1,11-undecanediol, were detected. (C) 1998 Published by Elsevier Science B.V.