超高效液相色谱-串联质谱法检验血斑中抗高血压药物  

Determining Hypertension-resistant Drugs in Bloodstains by UPLC-MS

作　　者：李昕潼 张云峰[2] 杨煜[1] 黄健[2] 常靖[2] 于忠山[2] LI Xintong;ZHANG Yunfeng;YANG Yu;HUANG Jian;CHANG Jing;YU Zhongshan(People’s Public Security University of China, Beijing 100038, China;Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China)

机构地区：[1]中国人民公安大学,北京102600 [2]公安部物证鉴定中心,北京100089

出　　处：《刑事技术》2019年第2期126-131,共6页Forensic Science and Technology

基　　金："十三五"国家重点研发计划资助(NO.2017YFC0803504);公安部技术研究计划(NO.2015JSYJC49)

摘　　要：目的建立非渗透性客体(载玻片)和渗透性客体(滤纸)上血迹斑痕中3种钙离子通道阻滞剂类抗高血压药物的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。方法采用空白外周静脉血加标后在非渗透性客体(载玻片)上制备成血斑,采用棉签提取法提取;空白外周静脉血和空白经血加标后分别在渗透性客体(滤纸)上制成血斑,采用剪取法收集。样品经甲醇沉淀蛋白法提取后,采用UPLC-MS/MS进行检测。在ACQUITY UPLC?HSS T3 (2.1mm×50mm,1.8μm)反相柱上分离,梯度洗脱,流动相为乙腈-0.1%甲酸溶液,质谱采集为电喷雾正离子多反应检测模式(MRM)。结果三种目标物在5～1000μg/L范围内具有良好的线性关系,决定系数(R2)大于0.9915,检出限在0.1～0.2μg/L之间,添加浓度水平为10、100、500μg/L时,取25μL加标血液制成血斑,方法回收率为68.5%～90.7%,相对标准偏差在2.0%～15.0%之间。结论本方法可用于多种客体上血斑中3种钙离子通道阻滞剂类抗高血压药物的法庭与临床毒物分析,为刑事案件中刻画血斑供体信息提供理论基础。Objective For rapid screening of three-kind hypertension-resistant drugs of calcium channel blockers (nimodipine, nifedipine and felodipine) in bloodstains on non-permeable and/or permeable objects, a method was established by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) so that a theoretic foundation can be built up for depicting the donors of bloodstains from criminal cases. Methods The blank venous blood was spiked and dried onto one glass slide (representing the non-permeable object), with the so-prepared bloodstain being wiped by cotton swab. The filter paper, representing the permeable object, was similarly stained with the spiked blood, then having been clipped into pieces. The bloodstain samples (the wiped cotton-swabs or clipped filter pieces) were extracted by methanol, with the supernatant being detected by UPLC-MS/MS which was run with the mobile phase of acetonitrile - formic acid (0.1%) solution flowing through a phase-reversed column of ACQUITY UPLC?HSS T3 (2.1×50 mm, 1.8 μm), and taken of electrospray ionization multiple reaction detection mode (MRM) for mass spectrometry. Results The correlation coefficients (R2) were more than 0.9915 among 5~1000 μg/L, with the detection limits between 0.1 and 0.2 μg/L, and the concentration levels being 10, 100 and 500 μg/L, respectively. The recovery was 68.5%~90.7% and the relative standard deviation was between 2.0% and 15.0%. Conclusion This method can be used onto a variety of objects carrying the bloodstains that contained the three kinds of hypertension-resistant drugs of calcium channel blockers (nimodipine, nifedipine and felodipine).

关 键 词：血迹斑痕 钙离子通道阻滞剂类抗高血压药物 超高效液相色谱-串联质谱 

分 类 号：DF795.1[医药卫生—法医学]