芝麻、独活、绿咖啡豆及白桦树皮中生物活性成分的研究
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摘要
本文对芝麻、独活、绿咖啡豆及白桦树皮中的活性成分展开了研究,建立了各研究对象中多种活性成分的分析方法和多种活性成分的分离纯化方法,有效的解决了芝麻素、绿原酸及白桦三萜类物质分离纯化中的诸多难题,为这些产品在终端市场的应用打下坚实的基础。此外,探讨了白桦脂酸在纯溶剂及混合溶剂中的溶解度及溶液的热力学性质。
本论文的主要内容如下：
论文第一章为绪论部分,对芝麻、独活、咖啡豆及白桦树皮中的活性成分的相关背景和研究现状进行了介绍,在此基础上阐述了本论文的主要研究意义和研究内容。
第二章建立了同时检测芝麻中芝麻素和芝麻林素的HPLC方法,并应用此方法对市售芝麻油中的芝麻素和芝麻林素进行分析。此外,以芝麻油生产过程中的废弃物芝麻油除臭馏出物为原料,采用碱皂化法对其中的芝麻素进行分离纯化,并应用柱色谱得到高纯度芝麻素。此工艺易应用于工业化生产芝麻素,简单有效,成本低廉。
第三章对我国传统中药独活中三种活性成分进行研究,建立了一种简单、准确的同时分析独活中O-乙酰基-山芹醇、蛇床子素和山芹醇的液相检测方法,可以用于中药独活质量控制的方法。
第四章对绿咖啡豆中绿原酸类物质进行研究,建立了咖啡豆中绿原酸类物质的分析方法,优化得到绿咖啡豆中绿原酸类物质的最佳提取条件。此外,我们重点研究了大孔树脂对咖啡豆中绿原酸类物质和咖啡因的吸附和分离性能。实验对比了绿原酸在6种不同型号的树脂吸附和解吸能力,筛选出的大孔树脂可实现咖啡豆中的绿原酸类物质和咖啡因的有效分离,得到高品质的低咖啡因咖啡豆提取物(5-CQA≥50％,caffeine≤2％),解决了目前咖啡豆生产中咖啡因不易去除的难题。
第五章测定白桦脂酸在13种纯溶剂及四氢呋喃+水混合溶剂中的溶解度,针对白桦脂酸在各溶剂体系中所表现出来的特殊现象,以TG/DSC和SEM为手段,研究了白桦脂酸晶体的物化性质。运用三参数方程和UNIQUAC模型对白桦脂酸在各溶剂体系中的溶解度数据进行关联和分析,并讨论溶液的热力学性质。此外,我们依据这些溶解度数据以及已有的研究,开发出一种简单的、低成本的、易于工业化的白桦脂醇和白桦脂酸的纯化方法,有效的解决了目前白桦三萜类化合物工业化生产的问题。
在第六章中,对所有的研究工作进行了总结,继承优点,改进不足,并提出本研究的后续研究思路。
The boiactive components in the sesame, radix angelicae pubescentis, green coffee bean, and birch bark were studied in this research. The analytical method for the quantitative determination and purification process of these constituents has been developed. Many separation problems of bioactive composition have been solved, which will forge a solid basis for natural products. Moreover, the solid-liquid equilibrium of betulinic acid in pure solvents and mixed solvents has been discussed.
The main contents could be summarized as follows:
The preface includes the research's purpose, method, process and working, the document's source, the frame of the theory and the thesis.
In the second chapter, simultaneous determination of sesamin and sesamolin in sesame by high performance liquid chromatography has been developed. The established method was successfully applied to simultaneous determination of the two analytes in ten different brands of sesame oils which were purchased from different companies and batches. Furthermore, sesamin was obtained through saponification and chromatography with silica gel. A pilot test showed that this process was applied to a large-scale production.
In the third chapter, we established an HPLC method to simultaneously determine three bioactive components of radix angelicae pubescentis. This improved method is convenient and suitable for control the quality of radix angelicae pubescentis.
In the fourth chapter, we established the HPLC analytical methods of the chlorogenic acids (CGAs) in the coffee beans, evaluated the optimal extraction parameters of the CGAs from the coffee bean. In addition, the adsorption and desorption properties of CGAs on macroporous resins including AB-8, HPD-826, LS-303, LX-60, LX-17, and LX-68have been compared. LX-60resin offers the best adsorption and desorption capacity for CGAs than other resins based on the research results. The optimum parameters for adsorption were obtained. After treating with LX-60resin, the superior quality green coffee bean extract, the contents of CGAs were more than50%and caffeine was less than2%, was obtained. The results showed that LX-60resin revealed a good ability to separate CGAs. Therefore, we conclude that results in this study may provide scientific references for the large-scale CGAs production.
In the fifth chapter, the solubilities of betulinic acid in thirteen commonly used organic solvents and THF+water mixed solvents were determined using HPLC method at different temperatures. The solubilities data was correlated with a semi-empirical equation and UNIQUAC equation. The calculated solubilities showed excellent agreement with the experimental data. The thermodynamic properties of the solution process and the crystal habit of betulinic acid were also discussed. Furthermore, we developed a novel method to separate betulin and betulinic acid from birch bark. This method is simple, cost effective, and has commercial feasibility.
In the last chapter, all of the experimental work was summarized. We find the deficiencies in this thesis and propose the idea of the latter research.
本论文的主要内容如下：
论文第一章为绪论部分,对芝麻、独活、咖啡豆及白桦树皮中的活性成分的相关背景和研究现状进行了介绍,在此基础上阐述了本论文的主要研究意义和研究内容。
第二章建立了同时检测芝麻中芝麻素和芝麻林素的HPLC方法,并应用此方法对市售芝麻油中的芝麻素和芝麻林素进行分析。此外,以芝麻油生产过程中的废弃物芝麻油除臭馏出物为原料,采用碱皂化法对其中的芝麻素进行分离纯化,并应用柱色谱得到高纯度芝麻素。此工艺易应用于工业化生产芝麻素,简单有效,成本低廉。
第三章对我国传统中药独活中三种活性成分进行研究,建立了一种简单、准确的同时分析独活中O-乙酰基-山芹醇、蛇床子素和山芹醇的液相检测方法,可以用于中药独活质量控制的方法。
第四章对绿咖啡豆中绿原酸类物质进行研究,建立了咖啡豆中绿原酸类物质的分析方法,优化得到绿咖啡豆中绿原酸类物质的最佳提取条件。此外,我们重点研究了大孔树脂对咖啡豆中绿原酸类物质和咖啡因的吸附和分离性能。实验对比了绿原酸在6种不同型号的树脂吸附和解吸能力,筛选出的大孔树脂可实现咖啡豆中的绿原酸类物质和咖啡因的有效分离,得到高品质的低咖啡因咖啡豆提取物(5-CQA≥50％,caffeine≤2％),解决了目前咖啡豆生产中咖啡因不易去除的难题。
第五章测定白桦脂酸在13种纯溶剂及四氢呋喃+水混合溶剂中的溶解度,针对白桦脂酸在各溶剂体系中所表现出来的特殊现象,以TG/DSC和SEM为手段,研究了白桦脂酸晶体的物化性质。运用三参数方程和UNIQUAC模型对白桦脂酸在各溶剂体系中的溶解度数据进行关联和分析,并讨论溶液的热力学性质。此外,我们依据这些溶解度数据以及已有的研究,开发出一种简单的、低成本的、易于工业化的白桦脂醇和白桦脂酸的纯化方法,有效的解决了目前白桦三萜类化合物工业化生产的问题。
在第六章中,对所有的研究工作进行了总结,继承优点,改进不足,并提出本研究的后续研究思路。
The boiactive components in the sesame, radix angelicae pubescentis, green coffee bean, and birch bark were studied in this research. The analytical method for the quantitative determination and purification process of these constituents has been developed. Many separation problems of bioactive composition have been solved, which will forge a solid basis for natural products. Moreover, the solid-liquid equilibrium of betulinic acid in pure solvents and mixed solvents has been discussed.
The main contents could be summarized as follows:
The preface includes the research's purpose, method, process and working, the document's source, the frame of the theory and the thesis.
In the second chapter, simultaneous determination of sesamin and sesamolin in sesame by high performance liquid chromatography has been developed. The established method was successfully applied to simultaneous determination of the two analytes in ten different brands of sesame oils which were purchased from different companies and batches. Furthermore, sesamin was obtained through saponification and chromatography with silica gel. A pilot test showed that this process was applied to a large-scale production.
In the third chapter, we established an HPLC method to simultaneously determine three bioactive components of radix angelicae pubescentis. This improved method is convenient and suitable for control the quality of radix angelicae pubescentis.
In the fourth chapter, we established the HPLC analytical methods of the chlorogenic acids (CGAs) in the coffee beans, evaluated the optimal extraction parameters of the CGAs from the coffee bean. In addition, the adsorption and desorption properties of CGAs on macroporous resins including AB-8, HPD-826, LS-303, LX-60, LX-17, and LX-68have been compared. LX-60resin offers the best adsorption and desorption capacity for CGAs than other resins based on the research results. The optimum parameters for adsorption were obtained. After treating with LX-60resin, the superior quality green coffee bean extract, the contents of CGAs were more than50%and caffeine was less than2%, was obtained. The results showed that LX-60resin revealed a good ability to separate CGAs. Therefore, we conclude that results in this study may provide scientific references for the large-scale CGAs production.
In the fifth chapter, the solubilities of betulinic acid in thirteen commonly used organic solvents and THF+water mixed solvents were determined using HPLC method at different temperatures. The solubilities data was correlated with a semi-empirical equation and UNIQUAC equation. The calculated solubilities showed excellent agreement with the experimental data. The thermodynamic properties of the solution process and the crystal habit of betulinic acid were also discussed. Furthermore, we developed a novel method to separate betulin and betulinic acid from birch bark. This method is simple, cost effective, and has commercial feasibility.
In the last chapter, all of the experimental work was summarized. We find the deficiencies in this thesis and propose the idea of the latter research.
引文
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