论文部分内容阅读
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/LNH4Cl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.
Using pressure capillary electrochromatography (pCEC) as a technical platform, the methodologies for establishing fingerprints of Phellodendron chinese Phellodendron communis were studied. Through the optimization of extraction solvent, organic phase types in the mobile phase, salt solution and other conditions, we found 1 The methanol solution of hydrochloric acid was used as the extract solution, and the 20 mmol/L NH4Cl solution-acetonitrile was used as the mobile phase gradient elution. The UV detection wavelength was the best when the wavelength was 230 nm. The different voltages were applied to the column and the details were elucidated. The effect of the dual separation mechanism of pCEC on the selectivity of separation revealed that the main components of phellobacter pallidum, palmatine and berberine had different peaks in the pCEC mode with different voltages. When the voltage was 0~ The order of peaks at 4kV was jatrorrhizine, palmatine and berberine. The order of the peaks at 8kV to 14kV was jatrorrhizine, berberine and palmatine. This reason was discussed in detail. Comparing with the micro-phase liquid chromatography mode, pCEC can provide more and better separation routes for the separation of complex samples.