【作者】 高彤文；

【导师】 郑嘉明；

【作者基本信息】 天津大学 ， 化学工艺， 2008， 硕士

【摘要】 本文研究了遵义地区野生黄花蒿中青蒿素的提取和分离,确定了一条由青蒿原料出发,较为合理的提取分离工艺路线。主要研究内容和结果如下:1.对青蒿素测定方法进行了验证,研究表明,用紫外分光光度法测定青蒿素的含量,方法简便、准确,但衍生反应中要严格控制反应温度在50℃±1℃,NaOH的质量分数在0.2%±0.02%范围内,否则Q292的吸光度降低,会影响测定结果的准确性。2.根据文献,青蒿素含量大于2mg/g的青蒿才有提取的价值。本文采用紫外分光光度法,经五次平行实验,测得青蒿样品中青蒿素的平均含量为8.957mg/g,远大于规定值,具有开发利用价值。3.为确定四氟乙烷提取青蒿素的最佳工艺操作条件,分别针对原料粒度、提取时间、提取温度、溶剂量、搅拌速度等因素对青蒿素提取率的影响进行单因素实验,结果表明这些因素在一定范围内都可以显著提高青蒿素提取率。优化这些数据后采用五因素四水平正交实验,得到了四氟乙烷提取青蒿素较好的提取工艺条件。工艺参数为原料粒度[80,100]目,提取时间60min,提取温度50℃,搅拌速度为400r/min,溶剂用量120ml/g。五次平行实验得到该条件下青蒿素的平均提取率为90.37%,大于有机溶剂萃取平均数83%,为以后工业化提供参考。4.本文采用沸点为30℃—60℃的石油醚萃取精制脱蜡,效果较佳。通过结晶和重结晶操作,得到了青蒿素晶体。5.通过对提取(四氟乙烷恒温搅拌)、分离(石油醚萃取)、精制(重结晶)工艺过程的研究,最终确定了一条总提取回收率为77.7%的工艺路线。更多还原

【Abstract】 Extraction and separation of Artemisinin from wild Artemisia annua L.in Zunyi was studied in this dissertation, a rational extraction technical route based on Artemisinin raw material was established. The main contents and results of the research included:1. The measuration method of Artemisinin was verified based on previous studies, and the Ultraviolet Spectrophotometry was selected as a simple accurate method, but the temperature of the ramification should be within 50℃±1℃and the mass concentration of NaOH solution should be within 0.2%±0.02%,otherwise, the absorbance of Q292 would be reduced , and the accuracy of the content determination was also affected.2. Artemisinin from Artemisia annua L. was only worth extracting when it’s content of Artemisinin was above 2mg/g according to literature. Using the Ultraviolet Spectraphotometey, the content of Artemisinin was determined as 8.957mg/g after five parallel experiments. Thus the conclusion was confirmed that the content of Artemisinin in Zunyi was comparatively high, and Artemisia annua L. in Zunyi was Worth exploiting and using.3. In order to ascertain the best technical route to extract Artemisinin from Artemsia annua L.by Tetrafluoroethane, we discuss the monofactor effects of time,temperature,stirring speed,grinding degree of material and the quantity of Tetrafluoroethane on the extraction rate of recovery,and the results were also given that those factors were beneficial to the extraction within a certain range. By the optimizing experiment,the appropriate technical condition were established as extraction time at 60min,temperature at 50,stirring rate at 400r/min,material grinding degree at [80,100]meshes,solvent quantity at 120mL/g.Under those conditions,an average extraction recovery rate we can concluded was 90.37%,but in literature the average was only 83% by organic solvent.Those experature results could be a guide for industrialization later. 4. The better result of refining and dewaxing was achieved by using the petroleun ether with boiling point of 30℃-60℃.The crystal of Artemisinin was obtained by the crystallization and recrystallization.5. Through the technical route to extract Artemisinin from Artemsia annua L. which was established by the way of extraction(constant-temperature atirring with Tetrafluoroethane),separation(extracting of petroleun ether), refining (recrystallization), a new technical route with the total recovery rate we can got was 77.7%.更多还原