LC-MS同时测定伤科黄水中8种成分的含量

Content determination of eight constituents in Shangke Huangshui by LC-MS

目的:采用LC-MS技术同时测定伤科黄水中8种有效成分的含量。方法:采用XBridge C_(18)色谱柱(2.10mm×100.00mm,2.50μm);柱温35℃;流动相A为水-甲酸(100∶0.3),流动相B为甲醇-甲酸(100∶0.3),梯度洗脱,0~15min 70%A,15~20min 70%~60%A,20~25min 60%~85%A;流速0.30mL/min。结果:黄柏碱、药根碱、表小檗碱、黄连碱、巴马汀、小檗碱、栀子苷、绿原酸8种成分在各检测条件下无明显干扰峰;在测定浓度范围内(1.00~1 000.00ng/mL)线性关系良好,相关系数R^2>0.9990;加样回收率均在95.00%~115.00%之间,RSD均<5.00%;精密度RSD均<5.00%。3个不同批次供试品的测定结果较一致。结论:本研究建立的LC-MS分析方法可用于同时测定伤科黄水中8种有效成分的含量。

Objective： The content of 8 active ingredients in the Shangke Huangshui was simultaneously determined by LC-MS technique. Methods： XBridge C（18） column（2.10 mm×100.00 mm, 2.50μm） was applied： column temperature 35°C; mobile phase A was water-formic acid（100∶0.3）, mobile phase B was methanol-formic acid（100∶0.3）, gradient elution, 0 to 15 min, 70%A; 15 to 20 min, 70% to 60%A; 20 to 25 minutes, 60% to 85%A; flow rate was 0.30 mL/min. Results： There were 8 components, such as phellodendron, jatrorrhizine, epiberberine, coptisine, palmatine, berberine, geniposide and chlorogenic acid. There were no obvious interference peaks under various detection conditions. The linear relationship was good in the concentration range（1.00-1 000.00 ng/mL）, the correlation coefficient R^2〉0.9990; the recovery rate of the sample was between 95.00% and 115.00%, RSD〈5.00%; precision RSD〈5.00%. The results of three different batches of test samples were consistent. Conclusion： The LC-MS method established in this study can be used to simultaneously determine the content of 8 active ingredients in the Shangke Huangshui.