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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,1.7μm)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4.0~11μg·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。
OBJECTIVE To establish a UPLC-MS / MS method for the determination of three chemical constituents, ibuprofen, diclofenac sodium and indomethacin, illegally added to Chinese herbal medicines for rheumatoid arthritis. Methods The samples were separated on a BEH-C18 column (2.1 mm × 100 mm, 1.7 μm), detected by tandem quadrupole mass spectrometry, and analyzed by MRM mode. The samples were extracted with methanol as solvent and the contents of cloth Lupine, diclofenac sodium, indomethacin three kinds of chemical composition. Results The linear range of the three anti-rheumatic chemical constituents was broad and the correlation was good. R2≥0.996 7; RSD was 1.7% -4.7%; the recovery was 95.1% -104.2%; the limit of quantification was 4.0-11 μg · ML-1; daytime precision RSD (n = 9) was 1.7% -4.1%. Conclusion The method is highly specific, easy to operate and fast. It can be used as an effective method to detect the three antirheumatic chemical constituents of illegally added ibuprofen, diclofenac sodium and indomethacin in proprietary Chinese medicines.