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

    • 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.

       

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