MEKC/MS测定连翘败毒丸中的连翘苷、大黄酚、大黄素

Simultaneous Determination of Forsythin,Chrysophanol and Emodin in Lianqiao Baidu Pills by Micellar Electrokinetic Chromatography-electrospray Ionization Mass Spectrometry

建立了胶束电动色谱-电喷雾质谱联用法同时测定连翘败毒丸中的连翘苷、大黄酚、大黄素含量的分析方法。采用未涂层石英毛细管(50μm×78cm)为分离通道,以40mmol/L月桂酸-100mmol/L氨水(含20%的乙腈,pH=9.0)为电泳缓冲介质、50%的异丙醇(含1mmol/LNH4Ac)为鞘液。结果表明,上述各组分在14min内得到基线分离。连翘苷、大黄酚、大黄素的线性范围分别为0.100～100、2.50～250、0.0500～50.0mg/L,检出限分别为0.0200、0.800、0.00500mg/L。样品的加标回收率在95%～104%之间,相对标准偏差均小于4.0%。该方法快速、简便、重现性好,已用于实际样品的分析,结果令人满意。

An online micellar electrokinetic chromatography-electrospray ionization mass spectrometry method for simultaneous determination of forsythin,chrysophanol and emodin in Lianqiao Baidu Pills was established.The samples were separated by an uncoated capillary（50μm × 78cm） on the operating voltage of 25kV using 40 lauric acid-100mmol /L ammonia mixture containing 20% acetonitrile（pH = 9.0） as the running buffer.The effect of experimental conditions,such as selection of bases,concentration of lauric acid,addition of organic solvent,applied voltage and the composition of sheath liquid on the separation and ionization of herbicides was investigated.The baseline separation of three components was achieved within 14 minutes with satisfactory repeatability and sensitivity.The linear ranges of forsythin,chrysophanol and emodin were 0.100 ～ 100,2.50 ～ 250,0.0500 ～ 50.0mg /L with detection limits of 0.0200,0.800,0.00500mg /L,respectively.The average recoveries ranged from 95% ～ 104% with all relative standard deviations less than 4.0%.The developed method is rapid,simple,and accurate and is suitable for the quality control of the three effective components in Lianqiao Baidu Pills.