实时直接分析-高分辨质谱法快速筛查凉茶中非法添加的21种解热镇痛类药物

Rapid screening of 21 kinds of antipyretics and analgesics drugs illegally added in herbal tea by direct analysis in real time-high resolution mass spectrometry

中文关键词:  实时直接分析  四极杆/静电轨道离子阱高分辨质谱法  凉茶  解热镇痛类药物  快速筛查

英文关键词:direct analysis in real time  quadrupole/orbitrap high resolution mass spectrometry  herbal tea  antipyretics and analgesics drugs  rapid screening

中文摘要:

      目的 建立一种实时直接分析(direct analysis in real time, DART)离子源结合四极杆/静电轨道离子阱高分辨质谱法(quadrupole/orbitrap high resolution mass spectrometry, Q-Orbitrap HRMS)快速筛查凉茶中非法添加的21种解热镇痛类药物。方法 样品经50%甲醇水超声提取, 过0.22 μm微孔滤膜后, 用DART-Q-Orbitrap HRMS测定。DART离子源的样品传输速度为0.2 mm/s、离子化温度为400 ℃、栅极电压为300 V, 扫描模式为正离子模式。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, 相对误差小于1.65×10?6, 可实现精准定性; 同时建立的21种解热镇痛类药物的二级质谱信息库进一步提高定性分析的准确性。方法筛查限范围为1.00~270.00 μg/kg, 满足筛查要求。结论 该方法具有分析速度快、精准定性、无需冗长色谱分离过程、环境友好等优势, 可作为凉茶中21种解热镇痛类非法添加化学药物的高通量筛查和精准定性检测方法。

英文摘要:

      Objective To establish a method for the rapid screening of 21 kinds of antipyretics and analgesics drugs illegally added in herbal tea by direct analysis in real time (DART) coupled to quadrupole/orbitrap high resolution mass spectrometry (Q-Orbitrap HRMS). Methods The samples were extracted with 50% methanol water solution, filtrated by 0.22 μm microporous membrane, and determined by DART-Q-Orbitrap HRMS. The sample transfer speed, ionization temperature and grid electrode voltage of DART were set to 0.2 mm/s, 400 ℃ and 300 V, respectively, the samples were analyzed in positive electrospray ionization. Results The measured accurate mass-to-charge ratios of the 21 kinds of antipyretics and analgesics drugs were obtained in full scan mode with a relative deviation lower than 1.65×10?6 compared with precision mass number, which could realize accurate qualitative analysis; tandem mass spectrometric database based on characteristic fragment ions of the 21 kinds of antipyretics and analgesics drugs were built to further improve the accuracy of qualitative analysis. The limits of screening ranged from 1.00 μg/kg to 270.00 μg/kg, which could satisfy the requirements of screening. Conclusion The method has the advantages of fast speed, accurate qualitative analysis, no need of lengthy chromatographic separation process and environmentally friendly, which can be used as a high-throughput screening and precise qualitative detection method for 21 kinds of antipyretics and analgesics drugs illegally added in herbal tea.