QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法同时测定全血中10种新型合成大麻素  

Simultaneous Determination of 10 New Synthetic Cannabinoids in Blood by UPLC-QE-Orbitrap MS with QuEChERS Extraction

作　　者：张志远 宋辉[1] 李想[1] 许英健[1] 朱昱[1] 王磊 ZHANG Zhi-yuan;SONG Hui;LI Xiang;XU Ying-jian;ZHU Yu;WANG Lei(Department of Forensic Science and Technology,Criminal Investigation Police University of China,Shenyang 110854,China;Kashgar Public Security Bureau,Kashgar 844000,China)

机构地区：[1]中国刑事警察学院刑事科学技术学院,辽宁沈阳110854 [2]新疆喀什市公安局,新疆喀什844000

出　　处：《分析测试学报》2022年第11期1658-1663,共6页Journal of Instrumental Analysis

基　　金：辽宁省教育厅科学研究经费重点项目(LJKZ0071)。

摘　　要：建立了QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap MS)同时测定全血中10种新型合成大麻素的分析方法。全血样本经优化的QuEChERS法提取后,采用Hypersil GOLD^(TM) Vanquish色谱柱(100 mm×2.1 mm,1.9μm),以0.1%甲酸水和0.1%甲酸乙腈为流动相进行梯度洗脱分离,在加热电喷雾离子源正离子/平行反应监测(HESI+/PRM)模式下同时进行检测。结果表明,10种目标物质在对应质量浓度范围内呈良好线性,相关系数(r^(2))均不小于0.9990,检出限(LOD)为0.01~0.05 ng/mL,定量下限(LOQ)为0.05~0.20 ng/mL,回收率为92.1%~115%,基质效应为86.6%~115%,日内相对标准偏差(RSD)均不大于8.5%,日间RSD均不大于10%。该方法具有操作简便、选择性好,检测灵敏度及回收率高的特点,适用于法庭科学全血样本中合成大麻素的检验鉴定。An ultra liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry(UPLC-QE-Orbitrap MS)with QuEChERS extraction was developed for the simultaneous determi⁃nation of 10 new synthetic cannabinoids in blood.The whole blood samples were firstly extracted by optimized QuEChERS method,then separated on an Hypersil GOLD^(TM) Vanquish column(100 mm×2.1 mm,1.9μm)by gradient elution,with 0.1%formic acid water and 0.1%formic acid acetoni⁃trile as mobile phases,and finally determined with positive heated electrospray ion source(HESI+)in parallel reaction monitoring(PRM)mode.The results indicated that the calibration curves for 10 tar⁃get compounds exhibited good linear relationships in their respective mass concentration ranges,with correlation coefficients(r^(2))not less than 0.9990.The limits of detection(LODs)and limits of quanti⁃tation(LOQs)for 10 compounds were in the range of 0.01-0.05 ng/mL and 0.05-0.20 ng/mL,respectively.The recoveries for 10 compounds ranged from 92.1%to 115%,and the matrix effects ranged from 86.6%to 115%,with the intra-day relative standard deviations(RSDs)and the inter-day RSDs not more than 8.5%and 10%,respectively.The method has the advantages of simple opera⁃tion,good selectivity,high sensitivity and recovery,and it is suitable for the identification of syn⁃thetic cannabinoids in whole blood samples.

关 键 词：QUECHERS 超高效液相色谱-四极杆/静电场轨道阱质谱 全血 新型合成大麻素 

分 类 号：O657.63[理学—分析化学] D918.93[理学—化学]