分析化学2016，Vol.44Issue(11)：1763-1770,8.DOI:10.11895/j.issn.0253-3820.160356
超高效液相色谱-串联质谱法同时检测人血浆中6种芥子气染毒标识物
Simultaneous Determination of Six kinds of Sulfur Mustard Biomarkers in Human Plasma by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry
梁龙辉 1刘石磊 1刘昌财 2黄桂兰 1向宇 2李欣海 1于惠兰2
作者信息
- 1. 防化研究院中国分析化学实验室，北京102205
- 2. 国民核生化灾害防护国家重点实验室，北京102205
- 折叠
摘要
Abstract
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) .关键词
超高效液相色谱-串联质谱/芥子气/生物标识物/血浆Key words
Ultra high performance liquid chromatography-tandem mass spectrometry/Sulfur mustard/Biomarkers/Plasma引用本文复制引用
梁龙辉,刘石磊,刘昌财,黄桂兰,向宇,李欣海,于惠兰..超高效液相色谱-串联质谱法同时检测人血浆中6种芥子气染毒标识物[J].分析化学,2016,44(11):1763-1770,8.
