Quantitative determination of acidic hydrolysis products of Chemical Weapons Convention related chemicals from aqueous and soil samples using ion-pair solid phase extraction and in-situ butylation

Chemical warfare agents such as organophospshorus nerve agents, mustard agents, and psychotomimetic agent like 3-quinuclidinylbenzilate degrade in the environment and form acidic degradation products the analysis of which is difficult under normal analytical conditions. In the present study a simultaneous extraction and derivatization method in which the analytes are butylated followed by gas chromatography and mass spectrometric identification of the analytes from aqueous and soil samples was carried out. The extraction was carried out using ion-pair solid-phase extraction with tetrabutylammonium hydroxide followed by gas chromatography with mass spectrometry in the electron ionization mode. Various parameters such as optimum concentration of the ion-pair reagent, pH of the sample, extraction solvent, type of ion pair reagent was optimised. The method was validated for various parameters such as linearity, accuracy, precision, limit of detection and quantification. The method was observed to be linear from 1-1000 ng/mL range in selected ion monitoring mode. The extraction recoveries were in the range of 85-110% from the matrixes with the limit of quantification for alkyl phosphonic acids at 1 ng/mL, thiodiglycolic acid at 20 ng/mL and benzilic acid at 50 ng/mL with intraday and interday precisions below 15%. The developed method was applied for the samples prepared in the scenario of challenging inspection.

Authors: Pal Anagoni S, Kauser A, Maity G, Upadhyayula VVR. ; Full Source: Journal of Separation Science. 2017 Nov 9. doi: 10.1002/jssc.201700955. [Epub ahead of print]

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