| 引用本文: | 励炯,朱健,沈国芳,裘一婧.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[J].中国现代应用药学,2014,31(10):1234-1238. |
| LI Jiong,ZHU Jian,SHEN Guofang,QIU Yijing.Detection of Ibuprofen, Didofenac Sodium and Indometacin Illegally Added in Traditional Chinese Medicine Preparation by UPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2014,31(10):1234-1238. |
|
| 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。 |
| 关键词: 超高效液相色谱 质谱 中成药 抗风湿 非法添加 |
| DOI： |
| 分类号: |
| 基金项目: |
|
| Detection of Ibuprofen, Didofenac Sodium and Indometacin Illegally Added in Traditional Chinese Medicine Preparation by UPLC-MS/MS |
|
LI Jiong, ZHU Jian, SHEN Guofang, QIU Yijing
|
|
Hangzhou Institute for Food and Drug Control, Hangzhou 310017, China
|
| 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. |
| Key words: UPLC MS Chinese medicine preparation anti-inflammatory illegally added |
