摘要
虎杖系蓼科蓼属植物虎杖的根茎和根。白藜芦醇是植物受外界刺激而产生的一类低分子量、具有生物活性的植物抗毒素。虎杖中的白藜芦醇含量是迄今研究植物中最高的。综合提取分离虎杖中两种甚至两种以上的有效成分,未见研究报道。本文选择虎杖作为研究对象,探索虎杖中大黄素和白藜芦醇的综合提取分离,为生产企业提供有价值的参考数据。
建立了紫外分光光度法(UV法)、薄层扫描法(TLC法)以及高效液相色谱法(HPLC法)分析检测白藜芦醇和大黄素的方法。以HPLC法精度最高,主要可用于最终产品含量测定,而TLC法、UV法可用于工业生产的定性检查或检测,且简便、快速。
对不同采收期虎杖的白藜芦醇、大黄素含量进行测定,结果表明:白藜芦醇、大黄素在8、9月份的含量最高,可达0.162%、0.648%。综合考虑虎杖采收期应在8、9月较为合理。
对虎杖中白藜芦醇提取进行了单因素试验和正交试验,综合考虑确定白藜芦醇和大黄素最佳提取工艺为:用10倍量的75%乙醇热回流提取3次,每次提取120min,此法优于水热回流法,与超声提取法相近。进行了虎杖中白藜芦醇和大黄素综合提取放大实验,结果表明:从虎杖中综合提取白藜芦醇和大黄素采用乙醇热回流提取法,提取液经浓缩、萃取、水解、脱色、重结晶等方法可有效地从虎杖中分离出高纯度白藜芦醇和大黄素,其中白藜芦醇(98.04%)转化率为64.76%,大黄素(98.11%)转化率为32.08%。
Polygonum cuspidatum is the root and rootstock of Polygonum cuspidatum Sieb.et Zucc belonged to Polygonaaceae. Resveratrol is a kind of small molecular weight and having biologic active phytoalexin produced by plants when they react against the stimulus of enviroment. The resveratrol content in Polygonum cuspidatum is the highest among all studied plant species. It has not been reported that two or more effective component are comperehensively extrated and separated from Polygonum cuspidatum. Adopting Polygonum cuspidatum as the research materials, we studied the method of comprehensive extraction and separation of resveratrol and emodin from Polygonum cuspidatum, and offered valuable reference data for the corporation.
The procedures to analyze resveratrol and emodin with UV, TLC and HPLC methods were set up. The HPLC analysis method can be used for detemining final product because of its highest preciseness. The TLC and UV analysis methods can be used for analyzing half-finished product in producting process because of its convenience and quickness.
The content of resveratrol and emodin in Polygonum cuspidatum of diffent picking period is determined, and is the highest in August and September which achieve 0.162% and 0.648%. August and September is reasonable picking period of Polygonum cuspidatum.
Based on the results of single factor experiments and orthogonal experiments, the best extracting procedures is extracting them with 10 times amount of 75% ethanol at 60℃for 2 hours and repeating the process three times. This method is better than heat return extraction of water, and near to ultrasonic extraction. Experiments of comprehensive extraction and separation of resveratrol and emodin from Polygonum cuspidatum were enlarged. After concentrating, extracting, hydrolyzing, decolorizing and crystalling, resveratrol and emodin can be effectively extracted and separated from Polygonum cuspidatum. The extracting ratio of resveratrol (98.04%) is 64.76%. The extracting ratio of emodin (98.11%) is 32.08%.
引文
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