乙肝解毒胶囊中5种有效成分的胶束电动色谱-质谱联用法测定

Simultaneous Determination of Five Effective Components in Yiganjiedu Capsule by Micellar Electrokinetic Chromatography-Electrospray Ionization Mass Spectrometry

建立了胶束电动色谱-电喷雾电离质谱联用法同时测定乙肝解毒胶囊中的小檗碱、巴马汀、药根碱、黄芩苷、大黄素5种药效成分含量的分析方法。使用未涂层石英毛细管，以30mmol／L月桂酸-70mmol／L氨水溶液（含20％乙腈，pH10．0）为缓冲液、70％异丙醇（含3mmol／L乙酸）为鞘液。结果表明，在18min内各组分达到基线分离，小檗碱、巴马汀、药根碱、黄芩苷、大黄素的线性范围分别为0．02～20、0．05～15、0．05～10、2．0～500、0．02～15mg／L，检出限分别为0．007、0．02、0．02、0．60、0．006mg／L。样品的加标回收率为95％～104％，相对标准偏差均小于3．9％。方法简便、快速、灵敏，已成功用于乙肝解毒胶囊中小檗碱、巴马汀、药根碱、黄芩苷、大黄素含量的同时测定。

A new method for the simultaneous determination baicalin and emodin in Yiganjiedu capsule was established by of berberine, palmatine, jatrorrhizine, micellar electrokinetic chromatography - electrospray ionization mass spectrometric （ MEKC - ESI MS） method. The samples were separated by an uncoated capillary on the operating voltage of 25 kV. The effect of experimental conditions, such as concentration of lauric acid, selection of bases, addition of organic solvent, capillary temperature, applied voltage and the composition of sheath liquid on the separation and ionization of herbicides was investigated. A good baseline separation of five compounds was achieved within 18 minutes by using 30 mmol/L lauric acid -70 mmol/L ammonia solution （containing 20% acetonitrile, pH 10. 0） as the running buffer and 70% 2-propanol（ containing 3 mmol/L acetic acid） solution as the sheath liquid. The calibration curves of berberine, palmatine, jatrorrhizine, baicalin and emod- in were linear in the range of 0.02 - 20, 0. 05 - 15, 0. 05 - 10, 2.0 - 500 and 0.02 - 15 mg/L, respectively, and detection limits were 0. 007, 0.02, 0. 02, 0. 60, 0. 006 mg/L, respectively. The average recoveries The method was tive components ranged simple, rapid in Yiganjiedu from 95% to 104% with relative standard deviations less than 3.9%. and accurate, and was suitable for the quality control of the five effeccapsule.