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A robust high‐throughput sample preparation and liquid chromatography/tandem mass spectrometry method for the quantitation of β‐lyase metabolites of sulfur mustard as 1,1′‐sulfonylbis‐[2‐(methylthio)ethane] in human urine
Author(s) -
Reddy Muntha K.,
Nixon Christopher,
Wyatt Shane A.,
Croley Timothy R.
Publication year - 2013
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.6541
Subject(s) - chemistry , chromatography , tandem mass spectrometry , tandem , liquid chromatography–mass spectrometry , sulfur mustard , mass spectrometry , sulfur , urine , organic chemistry , biochemistry , toxicity , materials science , composite material
RATIONALE Sulfur mustard (HD) is a major chemical warfare agent threat to humans. Since World War I, several incidents of human exposure to sulfur mustard have been reported. In order to assist health professionals during an exposure event and support biological monitoring, a rapid analytical method is required to measure the exposure of humans to HD. METHOD The β‐lyase metabolites of HD, 1‐methylsulfinyl‐2‐[2‐(methylthio)ethylsulfonyl]ethane (MSMTESE) and 1,1′‐sulfonylbis[2‐(methylsulfinyl)ethane] (SBMSE) were reduced to the single biomarker, 1,1′‐sulfonylbis‐[2‐(methylthio)ethane] (SBMTE), using titanium(III) chloride. High‐throughput sample preparation was performed on a Tecan Freedom EVO liquid handler and analysis was performed by electrospray ionization liquid chromatography and tandem mass spectrometry (LC/MS/MS) in the multiple‐reaction monitoring mode. RESULTS Each analytical run consisted of a matrix blank, calibration standards (0.1–100 ng/mL), low quality controls (QCs), 2.5 ng/mL, and high QCs, 25.0 ng/mL, of SBMTE in human urine. The method was validated with 20 analytical runs performed by four analysts. The mean calculated concentrations of the low and high QCs were 2.52 and 25.5 ng/mL with relative standard deviations of 3.6% and 2.3%, respectively. CONCLUSION This semi‐automated method has few manual transfer steps, thus minimizing common manual errors and saving time. Therefore, this method would be very helpful to responding laboratories in a large‐scale exposure event related to HD. Copyright © 2013 John Wiley & Sons, Ltd.