半枝莲药材质量分析及半枝莲总黄酮的集成制备研究

发布时间：2018-03-15 18:35

本文选题：半枝莲　切入点：质量控制　出处：《浙江大学》2017年硕士论文　论文类型：学位论文

【摘要】：半枝莲是一味常用中药,具有清热、解毒之功效；现代药理学研究表明,半枝莲具有抗肿瘤、抗菌、抗氧化、抗炎症、解热及免疫调节等药理作用。本论文以半枝莲为研究对象,采用高效液相色谱法(HPLC)建立了半枝莲多指标含量测定方法及指纹图谱分析方法,并采用集成提取吸附技术进行半枝莲总黄酮的制备研究,以期为半枝莲药材的质量控制及其有效成分的制备提供可靠依据。具体工作内容包括以下几个方面。1.半枝莲药材中4种黄酮类化合物的含量测定通过对半枝莲样品预处理方式进行考察,并对不同色谱柱、流动相、检测波长等色谱条件进行优化,建立了同时测定半枝莲药材中野黄芩苷(scutellarin)、野黄芩素(scuellarein)、木犀草素(luteolin)和芹菜素(apigenin) 4种黄酮类化合物含量的高效液相色谱方法。方法学考察结果表明,该方法具有较高的专属性,同时具有良好的精密度和准确度。应用该方法对10批半枝莲药材进行含量测定,结果表明不同批次之间各黄酮类成分的含量差异较大。2.半枝莲药材指纹图谱分析方法的建立采用高效液相色谱法,建立了半枝莲药材指纹图谱分析方法,方法学考察结果表明,该方法稳定可靠,可用于对半枝莲药材进行质量控制。应用该方法对10批不同批次药材进行指纹图谱分析,共选出12个共有峰,并应用中药色谱指纹图谱相似度评价系统对指纹图谱进行相似度评价,其中9批药材的相似度在0.90以上,结果表明,不同批次半枝莲药材的整体质量差别不显著。3.应用集成提取吸附技术制备半枝莲总黄酮集成提取-大孔树脂吸附技术,应用于半枝莲总黄酮的制备。基于大孔树脂静态吸附和动态吸附试验结果筛选出DM130大孔树脂,用于集成提取吸附过程。以总黄酮为考察指标,运用单因素考察结合Box-Behnken试验设计,优化了集成提取吸附过程工艺参数,优选得到最佳工艺如下：以20倍量、pH为2的水作为提取溶剂,回流提取吸附9 h,提取溶剂流速为7 BV/h。同时,考察了DM130树脂上总黄酮的洗脱过程工艺参数,确定洗脱过程最佳工艺为：3 BV体积的纯水洗柱后,使用5 BV体积70%浓度的乙醇溶液对吸附柱进行洗脱,流速为2 BV/h。上述工艺条件下,半枝莲总黄酮有效部位收率为46.70 mg/g,纯度为69.03%。
[Abstract]:Scutellaria Scutellariae is a traditional Chinese medicine with the effect of clearing away heat and detoxifying. Modern pharmacological studies show that Scutellaria Scutellariae has anti-tumor, antibacterial, antioxidant and anti-inflammatory effects. Pharmacological effects of antipyretic and immunomodulation. In this paper, a method for the determination of multiple index content and fingerprint analysis of Scutellaria barbata was established by high performance liquid chromatography (HPLC). The preparation of total flavonoids from Scutellaria barbata was studied by integrated extraction and adsorption technique. In order to provide reliable basis for the quality control of Scutellaria barbata and the preparation of its active components. The specific work contents include the following aspects. 1. Determination of four flavonoids in Scutellaria barbata by determination of the content of four flavonoids in Scutellaria Scutellariae. The way of product pretreatment was investigated, The chromatographic conditions such as different chromatographic column, mobile phase and detection wavelength were optimized. A high performance liquid chromatography (HPLC) method for simultaneous determination of four flavonoids in Scutellarinus chinensis, scutellaria reinreinn, luteolin and apigenin) was established. The method was used to determine the content of 10 batches of Herba Scutellariae. The results showed that the content of flavonoids in different batches of Scutellaria Scutellariae varied greatly. 2. The method of fingerprint analysis of Scutellaria barbata was established by HPLC, and the results of methodological investigation showed that the fingerprint of Scutellaria Scutellariae was analyzed by HPLC. The method is stable and reliable, and can be used to control the quality of Scutellaria Scutellariae. The fingerprint of 10 batches of different batches of Herba Scutellariae was analyzed and 12 common peaks were selected. The similarity evaluation system of chromatographic fingerprint of traditional Chinese medicine was used to evaluate the similarity of fingerprint. The similarity of 9 batches of medicinal materials was more than 0.90. The results showed that the similarity of 9 batches of medicinal materials was more than 0.90. There was no significant difference in the overall quality of different batches of Scutellaria barbata. 3. The integrated extraction and adsorption technology of total flavonoids of Scutellaria barbata was prepared by macroporous resin adsorption. Based on the static and dynamic adsorption experiments of macroporous resin, DM130 macroporous resin was selected for the process of integrated extraction and adsorption. Taking total flavonoids as the index of investigation, the single factor investigation combined with Box-Behnken test design was used. The parameters of the integrated extraction and adsorption process were optimized. The optimum conditions were as follows: using 20 times water as extraction solvent, refluxing and adsorbing for 9 hours, extracting solvent flow rate of 7 BV / h. At the same time, The elution process parameters of total flavonoids on DM130 resin were investigated. The optimum elution process was determined as follows: after washing column with pure water of 1: 3 BV volume, the adsorption column was eluted with ethanol solution of 5 BV volume 70% concentration. Under the above conditions, the yield of total flavonoids was 46.70 mg / g and the purity was 69.03.
【学位授予单位】：浙江大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R284

【相似文献】