超高效液相色谱串联质谱法检验全血中三种合成大麻素

发布时间：2018-07-11 17:01

本文选题：合成大麻素 + 超高效液相色谱-串联质谱　；参考：《分析试验室》2017年08期

【摘要】：建立了同时测定全血中合成大麻素JWH-018,JWH-250和AM-2201超高效液相色谱-三重四极杆质谱(UPLC-TQ/MS)快速检验方法。分别考察了沉淀蛋白法,改良后的Qu ECh ERS方法和Oasis HLB固相萃取3种前处理方法,以回收率为考察标准,比较了3种前处理方法的优缺点。沉淀蛋白法使用乙腈沉淀血液中的蛋白质,振荡、离心、过膜后直接进样;改良后的Qu ECh ERS方法采用无水M g SO4平衡水相;固相萃取选用HLB柱,对p H、淋洗液、缓冲液等条件进行优化,选用p H 9的硼砂-硼酸(4:1,V/V)缓冲液,甲醇-水(5:95,V/V)溶液为淋洗液,0.1%甲酸-乙腈(1:4,V/V)为洗脱液。选用ZORBAX Eclipse Plus C18色谱柱,以A相0.1%甲酸水和B相0.1%甲酸-乙腈作为流动相,进行梯度洗脱。采用液相色谱-串联质谱仪的电喷雾电离,正离子模式扫描,多反应监测(MRM)模式检测合成大麻素JWH-018,JWH-250及AM-2201。结果表明,3种合成大麻素在其各自的浓度范围内线性关系良好(R20.999);3个添加水平(5,50,100 ng/m L)下,固相萃取方法回收率在70.1%~98.5%之间,改良后的Qu ECh ERS方法回收率在80.3%~108.6%之间,沉淀蛋白法回收率在62.0%~92.3%之间,3种合成大麻素检出限(S/N=3)在0.01~0.05 ng/m L范围内,定量限(S/N=10)在0.05~0.1 ng/m L范围内。
[Abstract]:A rapid method for simultaneous determination of synthetic cannabinoid JWH-250 and AM-2201 in whole blood by UPLC-TQ / MS was established. The precipitation protein method, the improved QU ECh ERS method and the Oasis HLB solid-phase extraction method were investigated respectively. The advantages and disadvantages of the three pretreatment methods were compared with the standard of recovery. The precipitation protein method uses acetonitrile to precipitate the protein in the blood, oscillates, centrifuges, directly injects the sample after passing the membrane, the modified qu ECh ERS method uses the anhydrous mg so 4 equilibrium water phase, the solid phase extraction uses the HLB column, for the pH, the eluate, The buffer solution was optimized with pH 9 borax / boric acid (4: 1 / V / V) buffer solution and methanol / water (5: 95 V / V) solution as eluant. The eluent was 0.1% formic acid-acetonitrile (1: 4 V / V). ZORBAX Eclipse Plus C18 column was used for gradient elution with A phase 0.1% formic acid water and B phase 0.1% formic acid-acetonitrile as mobile phase. The synthetic cannabinoids JWH-018G JWH-250 and AM-2201 were detected by liquid chromatography-tandem mass spectrometer electrospray ionization, positive ion mode scanning and multiple reaction monitoring (MRM). The results showed that the linear relationship of three synthetic cannabinoids was good in their respective concentration range (R20.999), the recovery rate of solid phase extraction method was between 70.1% and 98.5%, and the recovery rate of improved QU ECh ERS method was between 80.3% and 108.6%. The recovery rate of precipitation protein method was between 62.0% and 92.3%. The detection limits of three synthetic cannabinoids (S / N ~ (3) were in the range of 0.01 ~ 0. 05 ng/m / L, and the quantitative limit (S / N ~ (10) was in the range of 0. 05 ~ 0. 1 ng/m / L.
【作者单位】：中国人民公安大学刑事科学技术学院;公安部物证鉴定中心;
【基金】：国家重点研发计划项目资助(2017YFC0803604-2)
【分类号】：D918.93;O657.63

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