High throughput quantitative analysis of the β-lyase sulfur mustard metabolite, 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] in urine via high performance liquid chromatography tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Apr 15:1051:1-8. doi: 10.1016/j.jchromb.2017.02.030. Epub 2017 Mar 3.

Abstract

Sulfur Mustard (HD) has a 100year history of use as a chemical warfare agent and recent events in the Middle East are causing it to once again be a potential concern. We report a new high-throughput method for the determination of HD exposure by the analysis of the β-lyase metabolite 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE) in human urine. This method features a hydrogen peroxide (H2O2) oxidative conversion of the β-lyase metabolites to SBMSE, followed by sample extraction and concentration using solid phase extraction in 96-well plate format. Subsequent high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis gave linear quantitation over a calibration range of 0.1-100ng/mL, with a method detection limit of 0.03ng/mL. Liquid chromatographic separation was achieved using a hydrophilic interaction liquid chromatography (HILIC) column with an analyte retention time of 0.9min and method time of 1.5min (cycle time=2.0min). Users of this method could prepare and analyze approximately 650 samples in 24h which would be important for an emergency response.

Keywords: Biomarker; Exposure; HPCL-MS/MS; High throughput; Oxidation; Sulfur mustards (HD).

Publication types

  • Validation Study

MeSH terms

  • Chemical Warfare Agents / metabolism*
  • Chromatography, High Pressure Liquid / instrumentation
  • Chromatography, High Pressure Liquid / methods*
  • Equipment Design
  • High-Throughput Screening Assays
  • Humans
  • Hydrogen Peroxide / metabolism
  • Limit of Detection
  • Lyases / metabolism
  • Mustard Gas / metabolism*
  • Oxidation-Reduction
  • Solid Phase Extraction / methods
  • Sulfones / metabolism
  • Sulfones / urine*
  • Sulfoxides / metabolism
  • Sulfoxides / urine*
  • Tandem Mass Spectrometry / instrumentation
  • Tandem Mass Spectrometry / methods*

Substances

  • Chemical Warfare Agents
  • Sulfones
  • Sulfoxides
  • 1,1'-sulfonylbis(2-(methylsulfinyl)ethane)
  • Hydrogen Peroxide
  • Lyases
  • Mustard Gas