Citation: LIANG Long-Hui, LIU Shi-Lei, LIU Chang-Cai, HUANG Gui-Lan, XIANG Yu, LI Xin-Hai, YU Hui-Lan. Simultaneous Determination of Six kinds of Sulfur Mustard Biomarkers in Human Plasma by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(11): 1763-1770. doi: 10.11895/j.issn.0253-3820.160356 shu

Simultaneous Determination of Six kinds of Sulfur Mustard Biomarkers in Human Plasma by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

LIANG Long-Hui ^1, ,
LIU Shi-Lei ^1,2 ,
LIU Chang-Cai ^1,2 ,
HUANG Gui-Lan ^1,2 ,
XIANG Yu ¹ ,
LI Xin-Hai ¹ ,
YU Hui-Lan ^1,2

1.
Laboratory of Analytical Chemistry, Research Institute of Chemical Defense, Beijing 102205 China;
2.
State Key Laboratory of NBC Protection for Civilian, Beijing 102205 China

Received Date: 8 May 2016
Revised Date: 23 August 2016

A sensitive method was developed for the simulation determination of six kinds of sulfur mustards (HD) biomarkers (TDGO, SBMSE, SBSNAE, TDG, MSMTESE and SMO) in human plasma by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). HD exposed plasma samples were pretreated with a mixed solvent of methanol and acetonitrile to precipitate proteins. A solid phase extraction (SPE) method with HLB cartridge was used to purify the target biomarkers from the matrix. A complete separation was achieved on an UHPLC system with a gradient elution. The qualitative and quantitative analyses were carried out by triple quadrupole tandem mass spectrometry in multiple reaction monitoring (MRM) mode. The results showed that the calibration curves for the 6 biomarkers were linear(R²=0.9840-0.9955)over the range from 0.05 to 500 ng/mL, with the limits of detection (LODs) of 0.01-1.0 ng/mL. The relative standard deviation (RSD, n=5) was ≤ 5.5%, and the recovery of the analytes ranged from 86.5% to 110.8%. The influence of the matrix backgrounds on the method's robustness was effectively diminished by introducing SPE procedure and by optimizing the UHPLC elution program. The method was successfully applied to the fifth biomedical sample analysis exercise organized by the Organization for the Prohibition of Chemical Weapons (OPCW).
- Ultra high performance liquid chromatography-tandem mass spectrometry,
- Sulfur mustard,
- Biomarkers,
- Plasma
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