UPLC-MS/MS测定抗风湿中成药中非法添加布洛芬、双氯芬酸钠和吲哚美辛

Detection of Ibuprofen, Didofenac Sodium and Indometacin Illegally Added in Traditional Chinese Medicine Preparation by UPLC-MS/MS

关键词:  超高效液相色谱  质谱  中成药  抗风湿  非法添加

Key words:  UPLC  MS  Chinese medicine preparation  anti-inflammatory  illegally added

摘要:

目的 建立抗风湿中成药中非法添加布洛芬、双氯芬酸钠和吲哚美辛3种化学成分的UPLC-MS/MS检测方法。方法 以BEH-C₁₈(2.1 mm×100 mm，1.7 μm)色谱柱分离，串联四级杆质谱仪检测，MRM模式进行定性定量分析，样品以甲醇为溶剂超声提取，检测添加在中成药中的布洛芬、双氯芬酸钠、吲哚美辛3种化学成分。结果 3种抗风湿性化学成分质谱检测的线性范围宽，相关性好，r²≥0.996 7；重复性RSD为1.7%~4.7%；方法回收率为95.1%~104.2%；定量限为4.0~11 μg·mL^-1；日间精密度的RSD(n=9)为1.7%~4.1%。结论 本方法专属性强，操作简单，快捷，可作为中成药中非法添加布洛芬、双氯芬酸钠和吲哚美辛3种抗风湿性化学成分的有效检测方法。

Abstract:

OBJECTIVE To develop a UPLC-MS/MS method to determine ibuprofen, didofenac sodium and indometacin illegally added in traditional Chinese medicine preparation. METHODS The analysis was performed by a UPLC-MS/MS system of Waters ACQUITY UPLC/Quattro Premier, with BEH-C₁₈(2.1 mm×100 mm, 1.7 μm) column. Multiple-reaction monitoring(MRM) was performed to identify and quantify ibuprofen, didofenac sodium and indometacin, which were extracted with methanol by ultrasonic. RESULTS Three linear calibration curves were obtained with r²≥0.996 7. The precision of the method were showed by RSD (n=6) ranged from 1.7% to 4.7%. The recoveries were determinated at three concentrations and ranged from 95.1% to 104.2%. The ranges of LOQ were from 4.0 μg·mL^-1 to 11 μg·mL^-1 and the RSDs (n=9) of inter-day precision were from 1.7% to 4.1%. CONCLUSION The method is specific, simple and fast to detect ibuprofen, didofenac sodium and indometacin illegally added in traditional Chinese medicine preparation.