实时直接分析质谱法快速检测保健酒中非法添加的12种PDE5抑制剂

Rapid Detection of 12 Illegally Added PDE5 Inhibitors in Health Wine by Real-Time Direct Analysis Mass Spectrometry

目的:建立一种实时直接分析离子源(Direct analysis in real time,DART)结合四极杆/静电轨道离子阱高分辨质谱法(quadrupole/orbitrap high resolution mass spectrometry,Q-Orbitrap HRMS)快速筛查保健酒中非法添加的12种PDE5抑制剂。方法:样品经80%乙腈水超声提取,过0.22μm微孔滤膜后用DART-Q-Orbitrap HRMS联用仪测定。DART离子源的电离模式为正模式,样品传输速率为0.20 mm/s,离子化温度为400℃,栅极电压为400 V。Q-Orbitrap HRMS扫描模式为全扫描/数据依赖性二级扫描(Full MS/ddMS^(2))。结果:在全扫描模式下测定目标化合物的一级精密质量数,与理论精密质量数相比,相对质量偏差小于1.89 ppm,可实现精准定性;同时采集二级质谱信息,进一步提高定性准确性。该方法检出限范围为0.03~2.50 mg/kg,满足筛查要求。结论:该方法具有分析速度快,定性准确,环境友好等优势,可作为保健酒中非法添加的12种PDE5抑制剂的快速筛查和精准定性检测方法。

Objective:To establish a real-time direct analysis in real time(DART)combined with quadrupole/Orbitrap high resolution mass spectrometry(q-orbitrap HRMS)to quickly screen 12 kinds of PDE5 inhibitors in health wine.Methods:the samples were extracted by ultrasonic with 80%acetonitrile water and passed 0.22μM microporous membrane was filtered and determined by dart-q-orbitrap HRMS.The ionization mode of dart ion source is positive mode,the sample transfer rate is 0.20 mm/s,the ionization temperature is 400℃,and the gate voltage is 400 V.Q-orbitrap HRMS scanning mode is full scanning/data dependent secondary scanning(full MS/ddms2).Results:the first-order precision mass number of the target compound was determined in the full scanning mode.Compared with the theoretical precision mass number,the relative mass deviation was less than 1.89 ppm,accurate and qualitative;At the same time,the secondary mass spectrometry information is collected to further improve the qualitative accuracy.The detection limit of this method is 0.03~2.50 mg/kg,which meets the screening requirements.Conclusion:this method has the advantages of fast analysis speed,accurate qualitative and environment-friendly.It can be used as a rapid screening and accurate qualitative detection method for 12 kinds of PDE5 inhibitors illegally added in health wine.