Determination of Hydrolysis Products of Sulfur Mustards by Reversed-Phase Microcolumn Liquid Chromatography Coupled On-Line with Sulfur Flame Photometric Detection and Electrospray Ionization Mass Spectrometry Using Large-Volume Injections and Peak Compression

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Abstract
On-line coupling of reversed-phase microcolumn liquid chromatography (micro-RPLC) and sulfur-selective flame photometric detection (S-FPD) was studied for the selective and direct determination of thiodiglycol, bis(2-hydroxyethylthio)methane, 1,2-bis(2-hydroxyethylthio)ethane, 1,3-bis(2-hydroxyethylthio)propane, and 1,4-bis(2-hydroxyethylthio)butane, which are breakdown products of the chemical warfare agents called sulfur mustards. Both isocratic and gradient elution were used. To improve sensitivity, large-volume injections were applied together with peak compression by displacement for late-eluting analytes. With S-FPD, detection limits of 1 μg/mL were obtained for all compounds. Using the same approach, the target analytes as well as various oxidation products could be identified by micro-RPLC with electrospray ionization mass spectrometry (ESI-MS) and ESI-MS/MS. The optimized micro-RPLC−S-FPD system was successfully used for the analysis of a spiked soil sample.