摘要
建立了超高效液相色谱-四极杆/静电场轨道阱(UPLC-QE-Orbitrap)高分辨质谱同时测定口腔液中15种新型合成大麻素的方法。以地西泮为内标物质,口腔液样本经乙腈沉淀蛋白后,采用Hypersil GOLD^(TM) vanquish色谱柱(100 mm×2.1 mm,1.9μm),以0.1%甲酸水(A)和0.1%甲酸乙腈(B)作为流动相进行梯度洗脱,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。15种目标物分别在0.05~50和0.20~50 ng/mL浓度范围内呈良好线性关系,相关系数(r^(2))均≥0.9990,检出限(LOD)和定量限(LOQ)分别为0.01~0.05 ng/mL和0.04~0.18 ng/mL,回收率为80.5%~113.6%,基质效应为95.8%~114.7%,日内相对标准偏差(RSD)≤6.7%,日间RSD≤9.1%。本方法适用于口腔液样本中合成大麻素物质的检验鉴定。
An ultrahigh performance liquid chromatography(UPLC)-quadrupole/electrostatic fieldorbitrap mass spectrometry(QE-Orbitrap-MS)method was established for the simultaneous determination of 15 new synthetic cannabinoids in oral fluid. Protein in oral fluid was precipitated by acetonitrile,and diazepam was added as internal standard. The Hypersil GOLD^(TM) Vanquish column(100 mm×2.1 mm,1.9 μm) was used as the stationary phase,and the 0.1% formic acid water(A)and 0.1% formic acid acetonitrile(B)were selected as mobile phases for gradient elution separation,followed by MS detection in positive ion source(HESI^(+))parallel reaction monitoring(PRM) mode for qualitative analysis. The experimental results of 15 target substances showed good linearity in the concentration range of 0.05-50 ng/mL or 0.20-50 ng/mL,and the determination coefficients(r^(2))were all greater than 0.9990. The limits of detection were 0.01-0.05 ng/mL,and limits of quantification were 0.05-0.20 ng/mL. The recoveries were 80.5%-113.6%,and the matrix effects were 95.8%-114.7%. The intra-day relative standard deviatons(RSDs)were all less than 6.7%,and inter-day RSDs were all less than 9.1%. This method is suitable for the detection and identification of synthetic cannabinoid substances in oral fluid samples.
作者
宋辉
张志远
李想
许英健
朱昱
王磊
SONG Hui;ZHANG Zhiyuan;LI Xiang;XU Yingjian;ZHU Yu;WANG Lei(Department of Forensic Science and Technology,Criminal Investigation Police University of China,Shenyang 110854,China;Public Security Bureau of Kashi,Kashi 844000,China)
出处
《分析试验室》
EI
CAS
CSCD
北大核心
2022年第10期1153-1159,共7页
Chinese Journal of Analysis Laboratory
基金
辽宁省教育厅科学研究经费重点项目(LJKZ0071)资助。
