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题名	柴达木枸杞子化学成分测定及品质分析
作者	曹静亚
学位类别	硕士
答辩日期	2014-05
授予单位	中国科学院研究生院
授予地点	北京
导师	胡风祖
关键词	柴达木枸杞子 快速溶剂萃取 β-胡萝卜素 东莨菪内酯 品质分析
学位专业	中药学
中文摘要	本论文对柴达木不同地区枸杞子的化学成分进行了定量分析，对其中一些活性成分进行了提取工艺和测定方法研究，并在此基础上，采用统计学方法，对不同产地枸杞子进行一个综合品质分析，得到以下结论： 1. 建立了ASE依次提取工艺流程，依次对枸杞子中类胡萝卜素、黄酮、还原糖、多糖类等成分进行了测定。采用HPLC、UPLC-ELSD、比色等方法，对枸杞子中的β-胡萝卜素、水溶性糖、东莨菪内酯等进行了定量分析，为其品质分析奠定了基础。 2. 以单因素试验结果为依据，通过四因素三水平正交试验对枸杞子中β-胡萝卜素成分的ASE提取工艺进行了优化。最佳提取条件为：称样0.8 g，以石油醚：丙酮(1:2)作为提取溶剂，提取20 min，循环2次，在该条件下，得出枸杞子中β-胡萝卜素的总含量为208.17 μg/g。 3. 对枸杞子中东莨菪内酯提取和测定方法进行了优化。最佳提取条件为：甲醇-盐酸溶液(4:1，v/v)，水浴回流提取1 h。最佳测定方法为：采用甲醇-0.05 %磷酸溶液 (35: 65) 为流动相，流速：1 mL/min，柱温：30 °C，检测波长：344 nm。在此条件下，东莨菪内酯峰形对称，与杂质峰可达到基线分离。 4. 建立了UPLC-ELSD法测定柴达木枸杞子中的鼠李糖、木糖、果糖、葡萄糖和蔗糖的方法。以ACQUITY UPLC BEH Amide柱为分析柱，乙腈和水(各含0.2 % TEA) 作为流动相，流速为0.15 mL/min，柱温为45 °C，ELSD为检测器，漂移管温度为50 °C，N2流量为40 psi。结果表明，枸杞子中的水溶性糖主要为果糖和葡萄糖，建立的方法操作简单、效率高、重现性好、结果准确可靠，适用于枸杞子中水溶性糖的含量测定。 5. 以β-胡萝卜素、类胡萝卜素、总黄酮、还原糖、多糖、甜菜碱、东莨菪内酯为评价指标，采用SPSS 13.0对实验结果进行主成分分析，提取枸杞子影响因素指标，综合分析不同产地枸杞子品质。分析得出：枸杞子中多个功效性成分间有较强的相关性，类胡萝卜素的含量对枸杞子品质影响最大，其次为总黄酮、多糖和甜菜碱。这一系统的综合性分析，为柴达木枸杞子实现生态防护，推动当地经济发展起到一个理论支撑作用。
英文摘要	This thesis is aimed at quantitative analysis of the chemical composition of Lycii Fructus from different regions of Qaidam. In this study, the extraction and determination process of some active ingredients have been studied, and based on this, we conduct a comprehensive analysis of the quality of the Lycii Fructus from different origins with the statistic methods, and then we get the following conclusions: 1. We established ASE one-step extraction process and determined carotenoids, flavonoids, reducing sugars, polysaccharides and other ingredients in proper order. With HPLC, UPLC-ELSD, ICP-AES and colorimetric method, we carried out quantitative analysis of β-carotene, water soluble sugar and scopoletin to lay the foundation for subsequent quality analysis. 2. To study the optimal extraction technology of β-carotene in Lycii Fructus. The extraction conditions of ASE were optimized through single-factor test and orthogonal experiment design. The optimum extractions of ASE were that the sample weight was 0.8 g, extraction solvent was petroleum ether: acetone (1:2), the time of extraction was 20 min and the extraction times was twice. The total content of β-carotene in Lycii Fructus was 208.17 μg/g through the optimum conditions above. 3. A method was developed and validated to determine the contents of scopoletin in the Lycii Fructus. The optimum extraction condition was: methanol-hydrochloric acid solution (4:1, v / v), bath reflux extraction 1 h. The optimum determination method was: methanol-0.05 % phosphoric acid buffer (35:65) as the mobile phase. The flow rate was 1 mL/min. The column temperature was set at 30 °C and the detecting wavelength was 344 nm. Under this condition, scopoletin has a symmetrical peak shape, and the impurity peak can reach a baseline separation. 4. An ultra performance liquid chromatography coupled with evaporative light scattering detector (UPLC-ELSD) method was developed to determine the contents of rhamnose, xylose, fructose, glucose and sucrose in the Lycii Fructus from Qaidam Basin. The carbohydrates were separated on an ACQUITY UPLC BEH Amide column by using acetonitrile-water (0.2 % TEA in both of solvent) as the mobile phase. The flow rate was 0.15 mL/min with the column temperature set at 45 °C. The drift tube temperature of the ELSD was set at 50 °C and the flow rate of N2 was set at 40 psi. It was found that fructose and glucose were the major water-soluble sugar in Lycii Fructus. The method was sensitive, reliable and accurate. It was applicable to determine water-soluble sugar in Lycii Fructus. 5. With β-carotene, carotenoids, flavonoids and reducing sugars, polysaccharides, betaine and scopoletin as evaluation index, the experimental results were carried out using principal component analysis to extract influence index and give a comprehensive assessment of Lycii Fructus from different origin using SPSS 13.0. The experiment result indicates that a strong correlation exists among multiple functional components in Lycii Fructus. The content of carotenoid has the greatest impact on the quality of Lycii Fructus, followed by total flavonoids, polysaccharides and betaine. This systemic comprehensive analysis promotes a theoretical support for achieving ecological protection and promoting local economic development.
公开日期	2014-09-03
内容类型	学位论文
源URL	[http://ir.nwipb.ac.cn/handle/363003/4005]
专题	西北高原生物研究所_中国科学院西北高原生物研究所
推荐引用方式 GB/T 7714	曹静亚. 柴达木枸杞子化学成分测定及品质分析[D]. 北京. 中国科学院研究生院. 2014.

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