加压毛细管电色谱在建立中药黄柏指纹图谱中的方法学研究

以加压毛细管电色谱（pCEC）为技术平台，对其在建立中药黄柏指纹图谱中的方法学进行了研究．通过对提取溶剂、流动相中有机相种类、盐溶液等条件的优化，发现1％盐酸的甲醇溶液为提取溶液，20mmol／LNH4C1溶液．乙腈为流动相梯度洗脱，紫外检测波长为230nm时对其分离效果最好．并通过在色谱柱上施加不同的电压，详细地阐明了pCEC的双重分离机制对分离选择性的影响，发现黄柏中的主要成分药根碱、巴马汀和小檗碱在pCEC模式中随电压的不同，有不同的出峰顺序．当电压为0—4kV时出峰顺序为药根碱、巴马汀和小檗碱，当电压为8—14kV时出峰顺序为药根碱、小檗碱和巴马汀．对此原因进行了详细讨论，同时与微径液相色谱模式进行了比较，说明pCEC可以为复杂样品的分离提供更多更好的分离途径．

Study on pressurized capillary electrochromatography as an fingerprint analytical method for Cortex Phellodendri

Pressurized capillary electrochromatography combines the best features of capillary electrophoresis （CE） and high performance liquid chromatography （HPLC）： high separation efficiency, high selectivity, high resolution and fast speed. Besides, it can suppress bubble formation and provides a solvent gradient mode. So pCEC is much more suitable to separate complex system, such as traditional Chinese medicines. The analysis methods of pCEC fingerprint of Cortex Phellodendri, which contain many alkaloid compounds and so on, were studied and optimized. Cortex Phellodendri was extracted by 1% HCl methanol solution. C 18 capillary column was used as stationary phase and 20 mmol/L NH4Cl- acetonitrile with gradient as mobile phase. The wavelength of UV detector was 230 nm. In addition, the applied voltage could affect the separation because it was part of the driving force. The value of voltage could control the retention time and the order of some compounds. The order of three standards is jatrorrhizine, palmatine and berberine when the voltage is 0-4 kV, and the order is jatrorrhizine, berberine and palmatine when the voltage is 8-14 kV. This work could provide foundation for more research of fingerprint of Cortex Phellodendri planted in different places.