超高效液相色谱-串联质谱法测定指纹中的咖啡因及常见镇静药物  

Determination of Caffeine and Common Sedative Drugs in Fingerprints by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄成龙 满瀚泽 宋禧林 赵雅彬[1,2] 孙婧 HUANG Cheng-long;MAN Han-ze;SONG Xi-lin;ZHAO Ya-bin;SUN Jing(Academy of Investigation,People’s Public Security University of China,Beijing 100038,China;Public Security Behavioral Science Laboratory,People’s Public Security University of China,Beijing 100038,China;Beijing Public Security Bureau,Beijing 100085,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]中国人民公安大学公共安全行为科学实验室,北京100038 [3]北京市公安司法鉴定中心,北京100085

出　　处：《分析测试学报》2025年第2期285-293,共9页Journal of Instrumental Analysis

基　　金：中国人民公安大学基本科研业务项目(2023JKF01ZK02);公安部技术研究计划项目(2023JSZ03)。

摘　　要：指纹中含有个体代谢产生的多种内源性物质,对指纹组分进行检测能够判断遗留者的服药或饮食习惯,对遗留者身份和特点的分析有重要意义。该文以指纹物质中咖啡因及常见镇静药为目标物,通过优化甲醇沉淀蛋白前处理方法、改进液相色谱洗脱条件和质谱检测方法,建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)测定指纹中咖啡因及常见镇静药物的新方法,并以实际样本进行了验证。该方法以0.1%甲酸-10 mmol/L甲酸铵水溶液与0.1%甲酸-甲醇作为流动相进行梯度洗脱,在电喷雾电离源(ESI)多反应监测模式(MRM)下检测。结果表明:目标物在一定质量浓度范围内具有较好的线性关系,相关系数大于0.99;在3个加标水平(10、100、400 ng/mL)下,目标物的回收率为64.2%~111%,相对标准偏差不大于12%。该方法样品前处理简单,检测灵敏度高,选择性好。The fingerprint contains a variety of endogenous substances produced by individual metab⁃olism,and the detection of fingerprint components can determine the medication or eating habits of the remnant.In this paper,an ultra-high performance liquid chromatography tandem mass spectrom⁃etry method(UHPLC-MS/MS)for the determination of caffeine and common sedatives in fingerprint substances was established by optimizing the pretreatment method of methanol-precipitated protein,improving the elution conditions of liquid chromatography and the detection method of mass spectrom⁃etry.And the method was verified with a fingerprint.The method was used for the detection of caf⁃feine and common sedative drugs by gradient elution of 0.1%formic acid-10 mmol/L ammonium for⁃mate aqueous solution and 0.1%formic acid-methanol solution as mobile phase using electrospray ionization source(ESI)and multiple reaction monitoring(MRM)mode.The results showed that the sedative drugs and caffeine had a good linear relationship in certain mass concentration ranges,and the correlation coefficients was greater than 0.99.At 3 spiked levels(10,100,400 ng/mL),the re⁃coveries of caffeine and sedative drugs ranged from 64.2%to 111%,and the relative standard devia⁃tions were not more than 12%.The method has the advantages of simple sample pretreatment,high sensitivity and good selectivity,and is suitable for the screening test of caffeine and sedative drugs in fingerprints.

关 键 词：指纹物质 超高效液相色谱-串联质谱法 咖啡因 镇静药物 

分 类 号：O657.7[理学—分析化学] D918.93[理学—化学]