Quantitative Identification of Hydrolysis Products of Mustards by Novel Acetylation Method and Liquid Chromatography–High Resolution Mass Spectrometric Analysis

A novel derivatization method was developed for the analysis of hydroxy degradation products of the Chemical Weapons Convention (CWC)-related chemicals present in aqueous and soil samples. The analytes were acetylated with acetyl chloride and quantitatively identified by liquid chromatography-tandem mass spectrometry technique in electrospray ionization and atmospheric pressure chemical ionization modes. The acetylated products showed good separation and peak shapes with characteristic fragmentation. The developed method was validated, and the results showed linearity in the range of 1-5000 ng/mL quantities from aqueous and soil samples. The intraday and interday validation results show the deviation of less than 10% with greater than 90% recovery. The limit of detection and limit of quantification of the method, measured at a signal-to-noise ratio of 3:1 and 10:1, respectively, are in the range of 1-20 ng/mL. The developed method was applied to the analysis of samples given in the 56th and 57th official proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons (OPCW), and the chemicals were successfully identified by the developed method.