目的: 建立超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ/Orbitrap HRMS)快速筛查、定性检测人全血中三甲氧基安非他明、副甲氧基安非他明、亚甲基二氧吡咯戊酮、1-戊基-3-(4-甲基-1-萘甲酰基)吲哚、3,4-亚甲二氧基甲卡西酮、4-甲基乙卡西酮、苄基哌嗪、5-甲氧-N,N-二异丙基色胺、4-羟基-N-甲基-N-异丙基色胺、依他喹酮10个新精神活性物质的分析方法。方法: 空白血加入10个新精神活性物质的标准溶液涡旋离心,上清液经固相萃取柱(HLB)纯化,采用ACQUITY UPLC® HSS T3(150 mm×2.1 mm, 1.8 μm)色谱柱,以0.1%甲酸水溶液(A)-0.1%乙腈水溶液(B)为流动相,梯度洗脱,流速0.3 mL·min-1,柱温30 ℃,进样体积3 μL,采用电喷雾正离子源(H-ESI+)、Full MS-ddMS2模式采集数据。质谱检测先采用一级全扫描进行快速筛选,然后离子阱进行碎裂得到二级质谱数据进行精确认证。结果: 经过数据的采集和认证,能够得出10个新精神活性物质的出峰时间、母离子碎片及二级特征碎片离子。10个新精神活性物质各自线性关系良好(r≥0.997),空白血加标回收率在71.4%~117.9%,检测限均≤3 ng·mL-1,并能够应用到现实案例当中。结论: 该方法有效去除了人血基质中杂质干扰,实现了对10个新精神活性物质的快速筛查检测。方法灵敏度高,分析速度快,操作简便。
Objective: To establish a rapid screening and qualitative method by ultra-high performance liquid chromatography linear ion trap/Orbitrap high resolution mass spectrometry(UPLC-LTQ/Orbitrap HRMS) for determining (±)-3,4,5-trimethoxy-alpha-methylphenethylamine(TMA), paramethoxyamfetamine(PMA), methylenedioxypyrovalerone(MDPV), (1-pentyl-1H-indol-3-yl) (4-methoxynaphthalen-1-yl) methanone(JWH-122), 3, 4-methylenedioxy-N-methylcathinone(Methylone), 4-methylethcathinone (4-MEC), benzylpiperazine(BZP), 5-methoxy-N, N-diisopropyltryptamine (5-MeO-dipt), 4-hydroxy-N-methyl-N-isopropyltryptamine(4-Hydroxy mipt), etaqualone. Methods: Blank blood was added to the standard solution vortex centrifugation of 10 new psychoactive substances, the supernatant was purified by the hydrophilic-lipophilic balanced exchange column(HLB) and the column was ACQUITY UPLC® HSS T3(150 mm×2.1 mm, 1.8 μm). The monile phase was 0.1% formic acid aqueous solution(A)-0.1% acetonitrile aqueous solution(B). Gradient elution was performed at the flow rate of 0.3 mL·min-1, the column temperature was 30 ℃, and the injection volume was 3 μL. The data were collected using electrospray positive ion source (H-ESI+) and Full MS-ddMS2 mode. Mass spectrometry detection was quickly screened using a first-level full-scan, and then the ion trap was fragmented to obtain accurate authentication of the secondary mass spectrometry data. Results: After data collection and certification, the peak time, parent ion fragments and secondary characteristic fragment ions of 10 new psychoactive substances can be obtained.The 10 new psychoactive substances had good linear relations (r≥0.995), and the recovery rate of blank blood labeling was 71.4%-117.9%,with an average detection limit≤3 ng·mL-1. At the same time, it could be applied to real drug crime cases. Conclusion: This method effectively removes the interference of impurities in the human blood matrix and realizes the rapid screening and testing of 10 new psychoactive substances. The method has high sensitivity, fast analysis speed and simple operation.
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