【作者】 宋秀荣；

【导师】 孙汉文； 杨更亮；

【作者基本信息】 河北大学 ， 分析化学， 2002， 博士

【摘要】 本文首先以近年来国内外天然产物研究取得的成果为例，概述了天然产物化学在研究策略与方向、资源保护、分离技术、生物与化学合成等主要领域的研究现状，并对雷公藤提取制备方法、检测技术等方面的研究现状加以综述。 研究了几种天然产物有效成分如生物碱类化合物、萜内酯类化合物、糖类化合物及甙类化合物的提取制备工艺。建立了雷公藤内酯醇、雷公藤内酯酮等二萜内酯类化合物柱色谱制备分离方法；建立了雷公藤生物碱类化合物如雷公藤次碱、雷公藤定碱的柱色谱制备分离方法。 建立了雷公藤二萜内酯类化合物高效毛细管电泳优化分离分析方法。考察了此方法的回收率、精密度、线性和检测限，讨论了缓冲溶液的组成中，硼砂及磷酸二氢钠的浓度、表面活性剂的浓度和pH值等因素对分离的影响，其优化分离的缓冲溶液组成为10mM磷酸二氢钠20mM硼砂加入20mM SDS，pH值为8.62，采用此方法分离雷公藤二萜内酯类化合物，可得到较好的分离效果。 建立了中成药雷公藤多甙片有效成分高效毛细管电泳优化分离分析方法。在熔融硅胶毛细管（60.2cm有效柱长52.6cm，内径为75μm）柱上，施加20kV电压，温度298K，进样时间5s，214nm紫外检测，缓冲体系包括10 mM硼砂中加入20 mM十二烷基硫酸钠（SDS）作表面活性剂，用硼酸调节pH=7.30。优化分离条件下有效成分可达基线分离，有良好的线性关系，方法简便快速。 建立了雷公藤生物碱类化合物非水相毛细管电泳优化分离分析方法。优化条件是：操作电压15kV，温度保持301K，进样时间5s，运行介质为20mM醋酸铵和3mM氨水加到甲醇媒介中。实验结果证明此方法是可行的。 建立了手性药物佐米曲坦毛细管电泳优化分离分析方法，其优化分离的缓冲溶液组成为84mM Tris—H₃PO₄中加入30 mM磺化—β—环糊精作手性拆分剂，pH=4.10；分离通道为未涂层熔硅弹性石英毛细管，内径50μm，柱长60cm，有效柱长52cm；分离条件是温度298K，运行电压为18kV，紫外检测波长设在214nm，进样时间为5s。更多还原

【Abstract】 Based on the current achievement on natural product, a general review ofnatural product chemistry and its application on investigation protocol, resourcesprotection, analysis technology, biology and chemistry synthesis was made. Furthermore, this review also covers the preparation and detection of Tripterygium \vilfordii.First, several extraction and preparation technologies of the alkaloid compounds, the diterpenoid triepoxides compounds and the saccharide compounds were studied. Two column chromatography methods for the separation wilforine and wilfordine , the triptolide and triptonide were developed, respectively.Second, a micellar electrokinetic capillary chromatography (MEKC) method has been established for the identification and determination of diterpenoid triepoxides in Chinese herb Tripterygium wilfordii Hook F and its preparations. The detailed investigations of the influence of SDS concentration, pH, boric acidand borax concentration were carried out. From the experiments, the MEKC was found to exhibit good accuracy, precision and repeatability.A capillary electrophoresis method has been established for the determination of triptonide and triptolide in Multi-glycosides Tripterygium wilfordii tablets. Capillary separation was carried out by using 0.01mol L-1 borax + + 0.02mol L-1 SDS (pH =7.3) as the buffer, 20kV applied voltage and 301K temperature.A method for the separation of wilforine and wilfordine in Tripterygium wilfordii Hook F based on nonaqueous capillary eletrophoresis has been developed. The optimum separation conditions are as follows: voltage 15kV, the temperature was kept at 301K and the running medium consisted of 20mM ammonium acetate and 3mM ammonium hydroxide in methanol. The feasibility of this method was demonstrated by the determination of wilforine and wilfordine in Tripterygium wilfordii Hook F.A capillary electrophoresis method has been established for the zolmitriptan of chiral drug.更多还原