文章简介
超高效液相色谱-串联质谱法同时检测毛发中3种新精神活性物质
  

要:目的 建立在毛发样本中同时精准测定ADB-BUTINACAADB-4en-PINACAPB-22的超高效液相-串联质谱检测方法。方法 毛发样品经甲醇提取破碎溶解后,0.1%甲酸水溶液11比例涡旋混匀后超声10min,经0.22 μm滤膜后,采用ACQUITY UPLC BEH C18 ( 2.1 mm ×100 mm1.7 μm) 色谱柱,以含0.1% 甲酸的乙腈-水为流动相进行梯度洗脱,流速0.4 mL/min。质谱的检测采用电喷雾电离-正离子、动态MRM的检测模式。结果 该方法实现了对3种新精神活性物质的定性、定量分析,各目标物在 0.240 ng/mL 范围内具有良好的线性关系,R2均大于0.998,最低检出限在 50200 pg/mL范围内,最低定量限在200 pg/mL回收率在94.63%100.4%范围内基质效应在93.47%130.27%范围内结论 该方法具有快速、灵敏、准确、适用性广等突出特点,能够满足相关合成大麻素在毛发中定性定量分析的要求,可以为相关案件中新精神活性物质的检验鉴定提供借鉴。

关键词:合成大麻素毛发检测;超高效液相色谱-串联质谱

Simultaneous determination of three synthetic cannabinoids in hair by HPLC/MS/MS

Qi Guan*Chou Wen PuBai Deng WenChai Yi LinYang Shu YiYang Li

Sichuan Provincial Technical Center for drug monitoring (Sichuan branch of the State Drug Laboratory)Chengdu 610000China

Abstractobjective establish an ultra performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the simultaneous determination of ADB-BUTINACAADB-4en-PINACAPB-22 in hair samples. Methods after the hair sample was broken and dissolved by methanol extractit was mixed with 0.1% formic acid solution in a ratio of 1:1After vortex mixingthe sample was ultrasonic-processed for 10 min and filtered with 0.22 μm filter membrane, acetonitrile-water containing 0.1% formic acid was used as mobile phase for gradient elution at a flow rate of 0.4 ml/min. The detection mode of mass spectrometry was electrospray ionization-positive ion and dynamic MRM. Results the qualitative and quantitative analysis of the three new psychoactive substances was realized by this method. The linear relationship of the three new psychoactive substances was good in the range of 0.2 ~ 40 ng/mL, and R2 was all greater than 0.998, the detection limit was in the range of 50-200 pg/mL, the quantitative limit was in the range of 200 pg/mL, and the recovery was in the range of 94.63%-100.4%The matrix effect was in the range of 93.47%~130.27%. Conclusion the method is rapid, sensitive, accurate and widely applicable, and can meet the requirements of qualitative and quantitative analysis of synthetic cannabinoids in hair, it can provide reference for the test and identification of new psychoactive substances in relevant cases.

Keywords: synthetic cannabinoidshair detectionHPLC-MS/MS



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