胶束电动毛细管色谱-电喷雾质谱联用法同时测定妇宁栓中的5种有效成分

Simultaneous determination of berberine,palmatine,matrine,catechin and baicalin in Funing Shuan by micellar electrokinetic capillary chromatography-electrospray ionization mass spectrometry

应用胶束电动毛细管色谱-电喷雾电离质谱联用法同时测定了妇宁栓中的小檗碱、巴马汀、苦参碱、儿茶素和黄芩苷5种主要有效成分的含量。在未涂层石英毛细管柱(80cm×50μm)中,以40mmol/L月桂酸-100mmol/L氨水溶液(含25%的乙腈,pH9.5)为缓冲液,分离电压为25.0kV,各组分在16min内得到完全分离。电喷雾质谱检测时采用50%异丙醇水溶液(含3mmol/L乙酸)为鞘液。结果表明,小檗碱、巴马汀、苦参碱、儿茶素、黄芩苷的线性范围分别为0.03～15、0.05～15、0.2～250、1.5～300和2.0～500mg/L,检出限分别为0.01、0.02、0.05、0.5、0.6mg/L。5种组分的加标回收率为94.0%～104.0%,相对标准偏差(RSD)在0.3%～3.2%之间。该法简便、快速、准确,重现性好,可用于妇宁栓中小檗碱、巴马汀、苦参碱、儿茶素、黄芩苷含量的同时测定。

A method for the simultaneous determination of berberine,palmatine,matrine,catechin and baicalin in Funing Shuan was established using micellar electrokinetic capillary chromatography-electrospray ionization mass spectrometry （MEKC-ESI MS）.The compounds were separated on an uncoated capillary （80 cm×50 μm） with the operating voltage of 25 kV and the running buffer of 40 mmol/L lauric acid-100 mmol/L ammonia mixture containing 25% acetonitrile （pH 9.5）.The baseline separation of the five compounds was achieved within 16 min with a satisfactory repeatability and sensitivity.The solution of 50% 2-propanol/water solution （containing 3 mmol/L acetic acid） was used as the sheath liquid for the ESI MS analysis.The results showed that the linear ranges for berberine,palmatine,matrine,catechin and baicalin were 0.03-15,0.05-15,0.2-250,1.5-300 and 2.0-500 mg/L,respectively,and the detection limits were 0.01,0.02,0.05,0.5 and 0.6 mg/L,respectively.The average recoveries of the five components were between 94.0%-104.0% with the relative standard deviations （RSDs） of 0.3%-3.2%.The developed method is simple,rapid,and accurate,and it is suitable for the routine analysis of the five effective components in Funing Shuan.