A sensitive method for quantitation of β-lyase metabolites of sulfur mustard as 1,1′-sulfonylbis[2-(methylthio)ethane] (SBMTE) in human urine by isotope dilution liquid chromatography–positive ion-electrospray-tandem mass spectrometry

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2007-05, Vol.850 (1), p.120-127
• Main Authors: Daly, James D., O’Hehir, Colleen M., Frame, George M.
• Format: Article
• Language: English
• Subjects: Analysis; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Chromatography, Liquid - methods; Fundamental and applied biological sciences. Psychology; General pharmacology; Humans; Isotopes; Liquid chromatography; Lyases - metabolism; Medical sciences; Metabolites; Mustard Gas - metabolism; Pharmacology. Drug treatments; Reference Standards; SBMTE; Sensitivity and Specificity; Spectrometry, Mass, Electrospray Ionization - methods; Sulfones - urine; Sulfoxides - urine; Sulfur mustard; Tandem mass spectrometry; Tandem Mass Spectrometry - methods; Urine
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2006.11.031

A method for measurement of an important biological marker, 1,1′-sulfonylbis[2-(methylthio)ethane] (SBMTE) of sulfur mustard agent HD [bis-(2-chloroethyl)sulfide] in human urine, to quantify HD exposure, is presented. It employs TiCl 3 reduction of β-lyase metabolites to SBMTE, and automated solid-phase extraction sample preparation, followed by isotope dilution liquid chromatography–positive ion-electrospray ionization-tandem mass spectrometry with 7.5 min/sample cycle time, to achieve SBMTE quantitation of up to 200 samples/24 h a day. Percent relative standard deviations over the calibration range varied from 12.0% at 0.1 ng/mL to 0.9% at 100 ng/mL, and the limit of detection from a 0.5 mL sample was below the lowest level calibration standard of 0.1 ng/mL.