定向逆流色谱新方法及其在天然产物分离中的应用
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摘要
天然产物以其多样性的化学结构和强的生物活性等特性而成为新药研发的重要资源。然而,由于其组成的的复杂性和和结构的多样性,人们常常很难有针对性地对特定活性组分实现高效的分离。因此,如何定向分离出天然产物的活性成份是当前药物研发的热点之一。本论文利用常规逆流色谱仪和自制的新型逆流色谱仪,建立了新型逆流色谱溶剂体系的快速选择理论和定向分离方法,发展了线性梯度逆流色谱理论和锥度逆流色谱新方法,并在此基础上建立了新型的二维逆流色谱技术用于多个目标化合物的定向分离。这些理论和实践,对于天然产物的高效开发和应用具有重要意义。
本论文首先利用气相色谱分离分析技术对两种四元溶剂体系(正己烷-乙酸乙酯-甲醇／乙醇-水体系)的组成及其相互关系的研究,建立了一套四元溶剂体系上下相体系的科学配制以及快速选择的新方法。其次,利用已经得到的溶剂体系组成数据和理论规律,结合标准化合物在不同溶剂体系中的分配系数,进行完善的数据分析。揭示了不同化合物在不同溶剂体系中的分配规律,建立了不同化合物的分配系数与溶剂系统组成之间的数学模型。提出一种新的、具有普遍适用性的、准确的逆流色谱靶向分离方法。
其次,在实践应用和应用方面,本论文以中药材丹参作为主要的研究对象,以上述高速逆流色谱靶向分离的新型方法为基础,建立了梯度逆流色谱和锥度逆流色谱的新型理论和靶向分离方法,实现了中药材丹参中多种复杂成分的高效、快速和准确的分离。
最后,在多靶向化合物定向分离方法的发展方面,本论文成功地建立了二维逆流色谱技术和适用于水溶性成分高效分离的双水相溶剂体系,揭示了其在分离纯化天然产物化学成分中的应用方法和操作模式,并凭借此方法从紫花苜蓿中成功分离得到了两种新的黄酮类化合物。
Natural products are important resources for drug discovery and food development for their diversities in structure and bio-activities. However, the components in natural products are difficult to be resolved by conventional separation methods for their high complexity and diversity. In this paper, several novel targeted counter-current chromatography (CCC) methods and theries were eatablished for separation of some typical natural products. They are important for the development and application of natural products.
First, the compositions and relationships for each component in upper lower phases of quaternary solvent systems (n-hexane-ethyl acetate-methanol/ethanol-water in different ratios) were determined by gas chromatography (GC) and a new scientific method for solvent system preparation and selection was built. And then, the partition coefficients (K) of standard compounds in different solvent systems were determined and the distribution rules of all compounds and the related mathematic models were built by analyzing all the data of solvent compositions and the K valves of standard compounds. As a result, a novel targeted counter-current chromatography (CCC) method was built for fast preparation and selection of solvent system and targeted separation components with high applicability.
Secondly, new methods and theories for gradient CCC, conical coils CCC were developed based on the targeted isolation theory above and have been successfully applied in the high efficient separation of different components in Salvia Miltiorrhiza Bung.
In addition, a new two-dimensional CCC and liquid-liquid solvent system were built for the multi-targets component separation. And two novel flavoids were obtained from Alfafa by this new method and system.
本论文首先利用气相色谱分离分析技术对两种四元溶剂体系(正己烷-乙酸乙酯-甲醇／乙醇-水体系)的组成及其相互关系的研究,建立了一套四元溶剂体系上下相体系的科学配制以及快速选择的新方法。其次,利用已经得到的溶剂体系组成数据和理论规律,结合标准化合物在不同溶剂体系中的分配系数,进行完善的数据分析。揭示了不同化合物在不同溶剂体系中的分配规律,建立了不同化合物的分配系数与溶剂系统组成之间的数学模型。提出一种新的、具有普遍适用性的、准确的逆流色谱靶向分离方法。
其次,在实践应用和应用方面,本论文以中药材丹参作为主要的研究对象,以上述高速逆流色谱靶向分离的新型方法为基础,建立了梯度逆流色谱和锥度逆流色谱的新型理论和靶向分离方法,实现了中药材丹参中多种复杂成分的高效、快速和准确的分离。
最后,在多靶向化合物定向分离方法的发展方面,本论文成功地建立了二维逆流色谱技术和适用于水溶性成分高效分离的双水相溶剂体系,揭示了其在分离纯化天然产物化学成分中的应用方法和操作模式,并凭借此方法从紫花苜蓿中成功分离得到了两种新的黄酮类化合物。
Natural products are important resources for drug discovery and food development for their diversities in structure and bio-activities. However, the components in natural products are difficult to be resolved by conventional separation methods for their high complexity and diversity. In this paper, several novel targeted counter-current chromatography (CCC) methods and theries were eatablished for separation of some typical natural products. They are important for the development and application of natural products.
First, the compositions and relationships for each component in upper lower phases of quaternary solvent systems (n-hexane-ethyl acetate-methanol/ethanol-water in different ratios) were determined by gas chromatography (GC) and a new scientific method for solvent system preparation and selection was built. And then, the partition coefficients (K) of standard compounds in different solvent systems were determined and the distribution rules of all compounds and the related mathematic models were built by analyzing all the data of solvent compositions and the K valves of standard compounds. As a result, a novel targeted counter-current chromatography (CCC) method was built for fast preparation and selection of solvent system and targeted separation components with high applicability.
Secondly, new methods and theories for gradient CCC, conical coils CCC were developed based on the targeted isolation theory above and have been successfully applied in the high efficient separation of different components in Salvia Miltiorrhiza Bung.
In addition, a new two-dimensional CCC and liquid-liquid solvent system were built for the multi-targets component separation. And two novel flavoids were obtained from Alfafa by this new method and system.
引文
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