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目的建立直接实时分析质谱(DART-MS)超速分析方法应用于药品监管检验工作。方法 DART-MS将实时直接分析离子源(DART)与离子阱质谱联用,离子源放电电压为4 kV,载气为氦气,流速为6 L.min-1,温度为400℃。在不进行样品色谱分离的前提下,直接分析被测物质或其溶液。结果 DART-MS与液质联用相比检定效率提高近50倍,对西地那非、米诺地尔等已知物质可在20 s内检测出,对未知衍生物可在4 min内完成其多级质谱研究,对传统液相色谱法难以分析的辅料如混合脂肪酸甘油酯等也能准确分析。结论 DART-MS样品处理简单,方法准确速度快,能广泛应用于非法添加、药物污染、制剂辅料成分的快速检定,开创了药品监管的新方法,能有效提高对突发安全事件的反应能力。
Objective To establish a direct real-time analytical mass spectrometry (DART-MS) speed analysis method used in drug regulatory inspection. Method DART-MS combined real-time direct analysis ion source (DART) with ion trap mass spectrometry. The ion source discharge voltage was 4 kV, the carrier gas was helium, the flow rate was 6 L.min-1 and the temperature was 400 ℃. In the absence of sample chromatographic separation under the premise of direct analysis of the test substance or its solution. Results The efficiency of DART-MS was 50 times higher than that of LC-MS. The known substances such as sildenafil and minoxidil could be detected within 20 seconds, and the unknown derivatives could be completed in 4 minutes Its multi-level mass spectrometry, traditional liquid chromatography difficult to analyze excipients such as mixed fatty acid glycerides can also be accurately analyzed. Conclusion The DART-MS sample is simple, accurate and rapid. It can be widely used in the rapid assay of illegal additives, drug contamination and formulation accessories, and opens up a new method of drug regulation, which can effectively improve the response to emergent safety events.