中成药中绿原酸的固相萃取-定量核磁共振波谱分析

摘要：目的：绿原酸具有抗菌、清热解毒的作用在许多中草药和中药复方制剂中得到使用。最近几年来，对其药理的研究无论国内还是国外都发展迅速，且对其生物活性的研究已经深入到医、食和日用品等多个方面。所以本课题以双黄连胶囊为实验对象，用定量核磁共振波谱法测定中成药双黄连胶囊中的有效成分绿原酸的含量。方法：样品制备：样品预处理：取0.4g双黄连胶囊粉末于棕色容量瓶中并加25mL水溶解，超声20分钟后冷却过滤，用HC-C18型固相萃取柱对提取液进行除杂后，用定量核磁共振波谱法测定绿原酸的含量。核磁定量：氘代溶剂选择氘代二甲基亚砜，选择对苯二甲醛作为内标，并且用基准试剂邻苯二甲酸氢钾对其进行标定。结果：固相萃取提取双黄连胶囊中的绿原酸可以在探究双黄连胶囊实验中运用，核磁定量双黄连胶囊中绿原酸通过核磁谱图可以看到绿原酸的峰，但双黄连胶囊的浓缩倍数不够，浓缩的目的欠佳，所以双黄连胶囊的样品预处理还要进一步优化。结论：该方法实验操作简单，关键在于样品的预处理过程，所以双黄连胶囊样品预处理还需待进一步探究。70085

毕业论文关键字：双黄连胶囊；绿原酸；固相萃取；核磁共振

Determination of chlorogenic acid in traditional Chinese medicine by solid phase extraction - quantitative nuclear magnetic resonance spectroscopy

Abstract: Purpose:Chlorogenic acid has antibacterial and detoxification effects in many Chinese herbal medicine and traditional Chinese medicine compound preparation. In recent years, both domestic and foreign have developed rapidly on the study of its pharmacology, and research about its biological activity has been deep into the medical, food , daily necessities or other aspects. Therefore, in this topic as the research object of Shuanghuanglian capsule，determination of effective components in Shuanghuanglian capsule on content of Chlorogenic acid by quantitative nuclear magnetic resonance spectroscopy.Method:sample preparation:sample pretreatment:take 0.4g Shuanghuanglian capsule powder in brown volumetric flask and add 25mLwater to dissolve, ultrasonic 20 minutes after the cooling filter, with HC-C18 SPE column on the extract after the impurity, with the determination of Chlorogenic Acid by Quantitative Nuclear Magnetic Resonance Spectroscopy.Nuclear magnetic quantification: select deuterated dimethyl sulfoxide as deuterated solvent , select the amount of terephthalaldehyde as the internal standard, and calibrated with the reference reagent potassium hydrogen phthalate.Results:the extraction of chlorogenic acid from Shuanghuanglian capsule by solid phase extraction can be used in the study of Shuanghuanglian capsule. The peak of chlorogenic acid can be seen by the nuclear magnetic spectrum in Shuanghuanglian capsule. But the concentration of Shuanghuanglian capsule is not enough,the purpose of enrichment is poor, so the sample pretreatment of Shuanghuanglian capsule should be further optimized.Conclusion: the method is simple to operate, the pretreatment process of the sample is the key,so the preparation of Shuanglanglian capsule sample need to be further explored.

KEY WORDS：Shuanghuanglian capsule；chlorogenic acid；solid phase extraction；nuclear magnetic resonance

1 前言 1

1.1 选题意义 1

1.2 固相萃取的概要 1

1.2.1 固相萃取技术的基本原理 1

1.2.2 固相萃取的类型 1

1.2.3 固相萃取的操作步骤 2

1.2.4 影响固相萃取柱的因素 2 中成药中绿原酸的固相萃取-定量核磁共振波谱分析:http://www.751com.cn/huaxue/lunwen_79222.html