LC-MS/MS快速测定血液中13种安眠镇静类药物及其代谢产物  

Rapid Determination of 13 Sedative Substances and Their Metabolites in Blood by LC-MS/MS

作　　者：石银涛[1] 王绘军[1] 王俊伟[1] 郑经[1] 吴玉红[2,3] SHI Yin-tao;WANG Hui-jun;WANG Jun-wei;ZHENG Jing;WU Yu-hong(Institute of Forensic Science,Chongqing Public Security Bureau,Chongqing 400021,China;Chongqing Police College,Chongqing 401331,China;Chongqing Key Laboratory of Toxicant and Drug Analysis,Chongqing 401331,China)

机构地区：[1]重庆市公安局物证鉴定中心,重庆400021 [2]重庆警察学院,重庆401331 [3]重庆市毒物毒品分析重点实验室,重庆401331

出　　处：《法医学杂志》2020年第1期45-51,共7页Journal of Forensic Medicine

基　　金：公安部技术研究计划资助项目(2016JSYJB11);重庆市公安局科技攻关计划资助项目(G2016-01,G2016-04)。

摘　　要：目的采用液液提取与液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)技术,建立同时测定血液中13种安眠镇静类药物及其代谢产物的分析方法,并将其应用于实际案例。方法血液加入内标后,用乙酸乙酯提取,浓缩至近干后,用甲醇溶解残渣,过0.22μm滤膜后测定。13种安眠镇静类药物及其代谢物经C18色谱柱分离,以甲醇和20 mmol/L甲酸铵(含0.1%甲酸)水溶液进行梯度洗脱,电喷雾正离子模式检测,内标法定量。结果血液中13种安眠镇静类药物及其代谢物在5~200μg/L范围内具有良好的线性关系,相关系数为0.990 3~0.999 8,检出限为0.1~1.0μg/L;在10、50、200μg/L3个添加浓度水平的回收率为71.2%~93.4%,日内和日间精密度≤8.6%,准确度(偏倚)在±9.8%范围内。结论本方法快速、简单、高效、灵敏度高,可用于法医毒物学领域血液中13种安眠镇静类药物及其代谢产物的分析。Objective To establish an analysis method for simultaneous determination of 13 sedative substances and their metabolites in blood by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry(LC-MS/MS) technology and to apply the method to actual cases. Methods The samples were extracted with ethyl acetate after an internal standard was added. The extract was condensed until it was nearly dry and then its residues were dissolved with methanol, filtered through0.22 μm filter and finally determined. The 13 sedative substances and their metabolites were separated through the C18 chromatographic column, then gradient elution was performed on them with methanol and 20 mmol/L ammonium formate(containing 0.1% formic acid) solution. After that, they were determined in the electrospray positive ion mode and quantified by internal standard method. Results The13 sedative substances and their metabolites in blood showed good linearity in the range of 5-200 μg/L with correlation coefficients ranging from 0.990 3 to 0.999 8. The detection limits were 0.1-1.0 μg/L.Recovery rates of sedative substances were in the range of 71.2%-93.4% when solutions with concentrations of 10, 50 and 200 μg/L were added. The deviations of intra-day and inter-day relative standard deviations(RSD) were not more than 8.6%. Accuracies(bias) were within ± 9.8%. Conclusion This method is rapid, simple, effective and sensitive, and can be applied to analysis of 13 sedative substances and their metabolites in blood in forensic toxicology.

关 键 词：法医毒理学 催眠药和镇静药 色谱法 液相 质谱分析法 液液萃取 血液 

分 类 号：DF795.1[医药卫生—法医学]