Determination of Hydrolytic Transformation Products of Sesquimustards in Water by High Resolution Liquid Chromatography/Mass Spectrometry

• Published in: Journal of analytical chemistry (New York, N.Y.) N.Y.), 2023-12, Vol.78 (14), p.1897-1905
• Main Authors: Vokuev, M. F., Braun, A. V., Rybalchenko, I. V., Rodin, I. A.
• Format: Article
• Language: English
• Subjects: Analysis; Analytical Chemistry; Chemistry; Chemistry and Materials Science; High performance liquid chromatography; Hydrolysis; Identification and classification; Mass spectrometry; Organosulfur compounds
• ISSN: 1061-9348; 1608-3199
• DOI: 10.1134/S1061934823140095

An approach to the determination of five sesquimustard markers, namely, bis(2-hydroxyethylthio)methane (BHETM), 1,2-bis(2-hydroxyethylthio)ethane (BHETE), 1,3-bis(2-hydroxyethylthio)- n -propane (BHETPr), 1,4-bis(2-hydroxyethylthio)- n -butane (BHETB), and 1,5-bis(2-hydroxyethylthio)- n -pentane (BHETPe) in environmental water using high-performance liquid chromatography with high-resolution mass spectrometry was developed for the first time. These substances are produced in aqueous media during hydrolysis of sulfur sesquimustards (bis(2-chloroethylthio)alkanes, n = 1–5). In this study, the conditions of mass spectrometric detection (optimal transitions for multiple reaction monitoring) and the gradient elution program for the HPLC separation of the analytes were optimized. The proposed technique was tested with water samples, and it showed good accuracy, precision, and selectivity. Accuracy was estimated by comparing the calculated concentration and the actual concentration entered into the sample. The absence of interfering influence of water sample components was also indicated. Limits of detection of BHETM, BHETE, BHETPr, BHETB, and BHETPe by using the proposed HPLC–MS/MS approach were 50, 5, 2, 2, and 0.5 ng/mL, respectively.