基质分散固相萃取-超高效液相色谱-串联高分辨质谱法同时测定干血斑样品中22种镇定催眠类药物  

Simultaneous Determination of 22 Sedative and Hypnotic Drugs in Dry Blood Samples by Ultra High Performance Liquid Chromatography-Tandem High Resolution Mass Spectrometry with Dispersive Solid Phase Extraction

作　　者：于峰 魏萌 文迪 苗鑫刚 张路迪 张晓光[4] YU Feng;WEI Meng;WEN Di;MIAO Xingang;ZHANG Ludi;ZHANG Xiaoguang(College of Forensic Medicine,Key Laboratory of Forensic Medicine of Hebei Province,Collaborative Innovation Center for forensic molecular identification of Hebei Province,Hebei Medical University,Shijiazhuang 050017;Nursing School of Hebei Medical University,Shijiazhuang 050031;Forensic identification center of Hebei Medical University,Shijiazhuang,050017;Core Facilities and Centers of Hebei Medical University,Shijiazhuang 050017)

机构地区：[1]河北医科大学法医学院,河北省法医学重点实验室,河北省法医分子鉴定协同创新中心,河北石家庄050017 [2]河北医科大学护理学院,河北石家庄050031 [3]河北医科大学法医鉴定中心,河北石家庄050017 [4]河北医科大学,医学与健康研究院大型科研仪器设备共享服务平台,河北石家庄050017

出　　处：《分析科学学报》2022年第6期716-722,共7页Journal of Analytical Science

基　　金：河北省卫生健康委员会医学科学研究课题项目(20200038);中央引导地方科技发展资金项目(226Z5601G)。

摘　　要：构建了干血斑样品中22种镇定催眠类药物的超高效液相色谱-串联高分辨质谱法定性、定量检测方法。干血斑样品经过乙腈提取后,应用基质分散固相萃取法对提取液进行净化,考察了不同种类净化剂以及用量对净化效果的影响,采用C18色谱柱进行分离,对色谱条件和质谱条件进行优化,使用同位素内标法进行定量分析。结果表明:22种被测物质在5 ng~800 ng/mL范围内线性表现良好(r^(2)>0.99),检出限为2 ng/mL~8 ng/mL,定量限为5 ng/mL~20 ng/mL,被测物质在低、中、高三个添加水平下回收率为80.2%~113.5%,相对标准偏差为0.9%~14.3%。本研究样本存储方便,保存时间长,前处理操作简单,应用精确质量数进行定性和定量,极大降低了假阳性的发生,为临床药物研究和法医毒物分析提供了新的技术支持。A research for the qualitative and quantitative determination of 22 sedative and hypnotic drugs in dry blood spot samples by ultra high performance liquid chromatography tandem high resolution mass spectrometry was established.Dry blood spot samples were extracted with acetonitrile.The extraction solution was purified by matrix dispersion solid phase extraction.The effects of different kinds of purifying agents and their amount on the purification were investigated.Waters BEH C18 column was employed for separation,and the chromatographic and mass spectrometry conditions were optimized.The isotopic internal standard method was used for quantitative analysis.The results showed that the linearities for the 22 analytes were from 5 ng/mL to 800 ng/mL with their correlation coefficients(r^(2))higher than 0.99.The limits of detection(LODs)for 22 analytes ranged from 2 ng/mL to 8 ng/mL,while the limits of quantitation(LOQs)ranged from 5 ng/mL to 20 ng/mL.Recoveries for the 22 analytes at three spiked levels ranged from 80.2%to 113.5%with relative standard deviations from 0.9%to 14.3%.The research significantly reduced the incidence of false positives and provides a new approach for clinical drug research and forensic toxic analysis.

关 键 词：干血斑 高分辨率质谱 基质分散固相萃取 镇定催眠类药物 

分 类 号：O657.63[理学—分析化学]