液质联用检测中成药中添加的双氯酚酸钠和布洛芬

目的: 建立液质联用同时测定中成药中添加双氯酚酸钠及布洛芬的定性及定量的方法。 方法: 采用C₁₈ 柱分离(100 mm×4.6 mm,3 μm),以乙腈-0.02 mol·L^-1 乙酸铵溶液(0.1%乙酸)(40∶ 60)为流动相,检测波长:220 nm、280 nm双波长测定,流速:0.5 mL·min^-1 。离子源为ESI源,负离子模式进行定性检测,HPLC测定含量。 结果: 6批受试制剂中有1批检测到添加了双氯酚酸钠及布洛芬。 结论: 该方法选择性强、灵敏度好,可作为分析消肿止痛类中成药中违禁添加双氯酚酸钠及布洛芬的有效检测方法。

Objective: To establish a LC-MS/MS method for simultaneous determination of diclofenac sodium and ibuprofen was illegal added to the Chinese traditional patent medicine. Methods: A C₁₈ column was used,with the mobile phase of acetonitrile-0.02 mol·mL^-1 ammonium acetate (0.1% acetic acid)(40∶ 60).The detective wavelength:280 nm,220 nm dual wavelength.The flow rate:0.5 mL·min^-1.It is based on high-performance liquid chromatography with electrospray ionization tandem mass (LC-ESI-MS/MS) spectrometric detection in negative ionization mode.HPLC determination of content. Results: Diclofenac sodiumand ibuprofen was found in one formulation of six. Conclusion: The method is selection and sensitive and can be used to expel pathogenic wind and remove dampness reduce swelling medicines in Chinese traditional patent medicine.