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高效毛细管电泳分析鉴定药物
Analysis and Determination of pharmaceuticals by Capillary Electrophoresis
【作者】 赵敬湘;
【导师】 杨更亮;
【作者基本信息】 河北大学 , 分析化学, 2001, 硕士
【摘要】 本文共分五章: 第一章:介绍了毛细管电泳(CE)的基础理论和毛细管电泳的发展状况。 第二章:建立了毛细管区带电泳分析中药金银花中绿原酸的分析方法。最佳分离条件为,缓冲液10mmol/L硼酸盐+19mmol/磷酸盐+10%乙醇(pH=8.86),电压16kV。紫外检测214nm。此方法用于分离鉴定中药金银花中的绿原酸具有样品处理简单、定量准确的特点。 第三章:建立了中药穿心莲中有效成分穿心莲内酯、脱氧穿心莲内酯和新穿心莲内酯的胶束毛细管电泳(MEKC)分析方法。缓冲体系包括硼酸盐和SDS(pH=9.5)。通过优化分离参数,例如,SDS浓度、pH值、背景电解质的相对浓度等。使这三种有效成分均能和其相邻组分实现基线分离。此分离条件也适合于穿心莲制剂,如穿心莲片和消炎利胆片中有效成分的分离测定。另外,本文将建立的胶束毛细管电泳分析方法同高效液相色谱法(HPLC)进行了比较。 第四章:建立了胶束毛细管电泳(MEKC)分离合成产物维生素E中的异构体的实验方法。本实验采用SDS和胆酸盐为混合胶束,以乙腈为有机改性剂,成功分离了合成产物中的杂质、结构异构体和旋光异构体。另外,本文考察了对多个分离参数,如SDS浓度,胆酸盐浓度,乙腈比例,缓冲液pH值等对分离的影响。 第五章:介绍了毛细管电色谱(CEC)的研究进展,包括电色谱柱的制备、柱填料、CEC的梯度洗脱及其CEC发展前景探究。
【Abstract】 This thesis consists of five chapters.Chapter one: Introduction of the basic theory of capillary electrophoresis, the application of CE and its future directions.Chapter two: A CZE method is developed to analyze the active component chlorogentic acid in Chinese herb Lonicera japonica Thump. The analysis was carried out under a buffer condition of 1 Ommol/L borate + I 9mmol/L phosphate + 1 0%(v/v) ethanol (p1-1=8.86). The applied voltage was 16kV and UV detector was set at 214nm, In this method, the treatment of the herb was simple and the quantitative analysis was accurate.Chapter three: A MEKC method determining the active components (andrographolide, neoandrographolide and deoxyandrographolide) in Chinese crude herb Andrographis paniculata was developed. The electrophoretic condition was 15 mM sodium dodecyl sulfate (SDS) +30 mM borate (pH 9.5). Under the optimized condition, three active components in the samples extracted by the mixture of water and ethanol (3:2, v/v) were quantitatively analyzed, and some preparations of Andrographis paniculata (Chuanxinlian table and Xiaoyan Lidan tablet) extracted by the same solvent were also determined. In order to validate the MEKC method, HPLC method was presented to compare with MEKC in respect of separation efficiency, sensitivity, linearity and repeatability.Chapter four: We developed a MEKC method for direct determination of the content of synthesized cxNitamin E, It was found that under the optimum separation condition (7mM borate +14mM phosphate +1 5mM sodium dodecyl sulfate (SDS) +10mM sodium cholate (NaCh) +8% acetonitrile; pH 92) with UV detection wavelength at 21 4nm, 16 kV constant voltage and 260C constant temperature, c&Vitamin E and its isomers can be baseline separated and x-Vitamin E was quantitatively analyzed. In addition, the sample recovery, the limit of detection and the repeatability of the method were investigated. Moreover, the influences of various parameters on the separation such as SDS concentration, NaCh concentration, pH of the buffer and acetonitrile percentage were also discussed.Chapter five: The advances in capillary electrochromatography including the packing method, its stationary phases, Gradient elution and the limitations of CEC.
- 【网络出版投稿人】 河北大学 【网络出版年期】2002年 01期
- 【分类号】O658.9;TQ460.7
- 【被引频次】1
- 【下载频次】233