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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。
A method for the simultaneous determination of forsythin, chrysophanol and emodin in Lianqiao Baidu decoction by micellar electrokinetic chromatography-electrospray ionization mass spectrometry was established. Uncoated quartz capillary (50μm × 78cm) was used as the separation channel, 40mmol / L lauric acid - 100mmol / L aqueous ammonia solution containing 20% acetonitrile and pH = 9.0 was used as electrophoresis buffer medium, 50% isopropanol 1mmol / LNH4Ac) as the sheath fluid. The results showed that the above components were baseline separated in 14min. The linear ranges of forsythin, chrysophanol and emodin were 0.100 ~ 100,2.50 ~ 250,0.0500 ~ 50.0mg / L, the detection limits were 0.0200,0.800,0.00500mg / L respectively. The spiked recoveries of samples ranged from 95% to 104% with relative standard deviations less than 4.0%. The method is fast, simple and reproducible, and has been used in the analysis of real samples with satisfactory results.