高效液相色谱-串联质谱法测定血液和尿液中7种合成大麻素类物质  

Determination of 7 Synthetic Cannabinoids in Blood and Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：陈跃 王忠娟[3] 张兆宏[3] 韩乃寒 CHEN Yue;WANG Zhongjuan;ZHANG Zhaohong;HAN Naihan(Department of Criminal Science and Technology,Shandong Police College,Jinan 250200,China;Doctoral Center for Science and Technology Innovation,Shandong police College,Jinan 250200,China;Weifang Municipal Public Security Bureau,Weifang 261041,China)

机构地区：[1]山东警察学院刑事科学技术系,山东济南250200 [2]山东警察学院博士科技创新中心,山东济南250200 [3]潍坊市公安局,山东潍坊261041

出　　处：《中国人民公安大学学报(自然科学版)》2024年第3期1-9,共9页Journal of People’s Public Security University of China(Science and Technology)

基　　金：毒品分析及禁毒技术公安部重点实验室课题(ynpc2022kf002);山东警察学院科研培育专项(YKYPYZX202103)

摘　　要：建立了一种高效液相色谱-串联质谱仪检测血液和尿液中合成大麻素类物质的方法。采用含0.1%甲酸的乙腈作为沉淀蛋白和提取溶剂,样品经过沉淀蛋白、超声提取和离心后采用高效液相色谱-串联质谱仪测定血液和尿液中7种合成大麻素,以0.1%(v/v)甲酸水溶液(含5 mmol/L甲酸铵)和乙腈作为流动相,梯度洗脱,质谱分析采用电喷雾离子源,电离模式为ESI^(+),多反应监测扫描方式进行定性定量分析。实验表明,7种合成大麻素类物质在0.1~20.0 ng/mL范围内线性良好(r>0.998),血液和尿液中7种合成大麻素类物质在低、中、高3个浓度添加平均回收率分别为66.3%~104.8%和69.1%~96.8%,检出限分别在0.030~0.117 ng/mL和0.011~0.051 ng/mL之间,定量限分别在0.100~0.390 ng/mL和0.037~0.169 ng/mL之间,日内精密度相对标准偏差为1.2%~11.4%和1.0%~10.9%,日间精密度相对标准偏差为1.6%~10.3%和1.3%~11.2%,基质效应在76.1%~97.7%和75.2%~93.3%之间。实验建立的方法快速、简便,通过小鼠实验表明,在给药后1 h的小鼠体内检出了合成大麻素类物质原体,此方法适用于合成大麻素类物质滥用者的筛查和确认。An analytical method for the simultaneous determination of synthetic cannabinoids(SCs)in blood and urine was established using high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Acetonitrile containing 0.1%formic acid was used as the precipitation protein and extraction solvent.7 kinds of SCs in blood and urine were determined by HPLC-MS/MS after protein precipitation,ultrasonic extraction and centrifugation.Using 0.1%(v/v)formic acid aqueous solution(containing 5 mmol/L ammonium formate)and acetonitrile as the mobile phase,gradient elution was performed.Qualitative and quantitative analysis were conducted by positive ion ionization mode of electron spray ionization(ESI^(+))and multiple reaction monitoring mode.The results showed that 7 kinds of SCs had good lin-earity within the calibration range of 0.1~20 ng/mL(r>0.998).The average recoveries of the 7 SCs in blood and urine at 3 spiked levels were in the range of 66.3%~104.8%and 69.1%~96.8%,respectively.The limits of detection were in the range of 0.030~0.117 ng/mL and 0.011~0.051 ng/mL,respectively.The limits of quantification were in the range of 0.100~0.390 ng/mL and 0.037~0.169 ng/mL,respectively.The relative standard deviations of intra-day precision were 1.2%~11.4%and 1.0%~10.9%,respectively.The relative standard deviations of inter-day precision were 1.6%~10.3%and 1.3%~11.2%,respectively.The matrix effects ranged from 76.1%to 97.7%and 75.2%to 93.3%,respectively.The established method was fast and simple.Mice experiments have shown that synthetic cannabinoid precursors were detected within 1 hour after administration.Therefore,the method is suitable for screening and confirming abusers of synthetic cannabinoids.

关 键 词：合成大麻素 血液 尿液 液相色谱-串联质谱 动物实验 

分 类 号：D918.93[政治法律—法学]