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目的:建立同时测定中药制剂中非法添加氨基比林及双氯芬酸钠的HPLC-MS/MS的方法。方法:采用C_(18)柱分离(100 mm×4.6 mm,3μm),以乙腈-水为流动相梯度洗脱,流速:0.5 ml·min~(-1),检测波长:280 nm。离子源为ESI源,正负离子交替模式进行定性检测,HPLC测定含量。结果:5批受试制剂中有2批检测到违禁添加的双氯芬酸钠,1批检测到违禁添加的氨基比林。结论:该方法选择性强、灵敏度好,可作为分析消肿止痛类中药制剂中违禁添加氨基比林及双氯酚酸钠的有效检测方法。
Objective: To establish a HPLC-MS/MS method for the simultaneous determination of aminopyrine and diclofenac sodium in Chinese medicine preparations. Methods: The separation was performed on a C 18 column (100 mm×4.6 mm, 3 μm). The gradient was eluted with acetonitrile-water mobile phase. The flow rate was 0.5 ml·min -1 and the detection wavelength was 280 nm. The ion source was an ESI source, and the positive and negative ion alternate modes were used for qualitative detection and HPLC determination. Results: The diclofenac sodium was detected in 2 batches of 5 batches of tested preparations, and the aminopyrine added in violation of the regulations was detected in 1 batch. Conclusion: The method is selective and has good sensitivity. It can be used as an effective method to detect the illegal addition of aminopyrine and diclofenac sodium in the traditional Chinese medicine preparations for detumescence and pain relief.