超高效液相色谱-串联质谱法同时检测血浆中6种芥子气染毒标识物

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• 英文论文题名：SIMULTANEOUS DETERMINATION OF SIX SULFUR MUSTARD BIOMAKERS IN HUMAN PLASMA SAMPLES BY ULTRAHIGH PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMRTRY
• 论文作者：梁龙辉 ; 刘石磊 ; 刘昌财 ; 黄桂兰 ; 向宇 ; 于惠兰
• 英文论文作者：Liang Long Hui ; Liu Shi Lei ; Liu Chang Cai ; Huang Gui Lan ; Xiang Yu ; Yu Hui Lan ; The Laboratory of Analytical Chemistry Reasearch Institute of Chemical Defence ; State Key Laboratory of NBC Protection for Civilian
• 年：2016
• 作者机构：防化研究院分析化学实验室;国民核生化灾害防护国家重点实验室;
• 论文关键词：液质联用 ; 芥子气 ; 生物标识物 ; 染毒血浆
• 英文论文关键词：Sulfur mustard(HD) ; UPLC-MS/MS ; biomarkers ; plasma exposed to HD
• 会议召开时间：2016-07-01
• 会议录名称：中国化学会第30届学术年会摘要集-第三十四分会：公共安全化学
• 语种：中文
• 分类号：R99;O657.63
• 学会代码：ZGHY
• 会议名称：中国化学会第30届学术年会-第三十四分会 ; 公共安全化学
• 会议地点：中国辽宁大连
• 主办单位：中国化学会
• 学会名称：中国化学会
• 页数：1
• 文件大小：187k
• 原文格式：D
• 会议级别：全国

摘要

针对芥子气(HD)染毒血液样本的溯源性分析需求,采用超高效液相色谱-ESI-三重四级杆串联质谱技术(UHPLC-ESI-MS/MS),建立了芥子气染毒血浆中6种代谢产物(TDG,TDGO,SMO,SBMSE,MSMTESE,SBSNAE)的高灵敏度和专属性检测方法。应用甲醇和乙腈混合有机溶剂沉淀染毒血浆中的蛋白,然后用HLB柱进行固相萃取纯化,经超高效液相色谱系统梯度洗脱分离,在电喷雾串联质谱正离子多反应监测(MRM)模式下进行检测,采用外标法定量。方法学验证结果表明:6种目标物的线性范围为0.05~500 ng/mL(R2=0.9840~0.9955),检测限介于0.01~1.0 ng/mL之间,各分析物的日内精密度(n=5)≤5.52%,加标回收率在86.5%~110.8%之间。将此方法应用于国际禁止化学武器组织(OPCW)第5次生物医学样品演练未知浓度HD染毒血浆样品的鉴定,解决了痕量HD(10 ng/mL)染毒血浆中游离生物标识物的检出难题。
A sensitive and specific approach for retrospective detection of sulfur mustard(HD) exposed plasma was established by detection of six HD metabolites(TDG,TDGO,SMO,SBMSE,MSMTESE,SBSNAE) using ultra high performance liquid chromatography-tandem mass spectrometry. The HD exposed plasma samples were pretreated with the mixed solvent of methanol and acetonitrile to precipitate proteins. A solid phase extraction method with HLB cartridge was used to purify the target biomarkers from the matrix. The complete separation was achieved on an ultra-high performance liquid chromatography system with a program elution. The qualitative and quantitative analyses were carried out by electrospray ionization(ESI)tandem mass spectrometry in multiple reactions monitoring(MRM) mode. The results showed that the calibration curve for the six biomarkers were linear(R2=0.9840~ 0.9955)over the range from 0.05-500 ng/mL, with the limits of detection(LODs) was 0.01~1.0 ng/mL. The average intraday(n=5) relative standard deviation(RSD) was ≤5.52%, and the of recovery of the analytes range from 86.5% to 110.8%.The method is successfully applied to retrospective detection of plasma samples exposed by trace level(10.0 ng/mL) HD in the fifth confidence building exercise on biomedical sample analysis organized by the Organization for the prohibition of Chemical Weapons(OPCW).

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