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秦艽中龙胆苦苷的提取及分离纯化工艺研究

Optinization of the Extraction and Purification Technology of Gentiopicroside from Gentiana Macrophylla Pall

【作者】 郝晓霞

【导师】 余淑娴;

【作者基本信息】 南昌大学 , 物理化学, 2007, 硕士

【摘要】 本文以甘肃产秦艽(Gentiana macropHylla Pall.)为原料,研究了其有效成分龙胆苦苷(gentiopicroside,GPS)的分析、提取、分离和纯化。以龙胆苦苷标样为对照品,建立了HPLC法、UV法为手段的定性、定量分析方法。本实验按照国家标准要求GB/T 5009.3-2003、GB/T 5009.6-2003、GB/T5009.4-2003、GB/T 5009.10-2003测定了秦艽原药材中水份、脂肪、灰份、粗纤维的含量,结果表明秦艽中以上各指标的平均含量依次为:11.41%、9.284%、4.094%、12.34%。各个含量平行实验的偏差较小,测量结果较为可信,这可以作为对中药秦艽一般化学成分的初步研究。在单因素实验的基础上,设计正交试验,优选出超声醇提秦艽中龙胆苦苷的最佳工艺条件为:乙醇用量为30mL、提取时间为20min、提取次数为4次、提取温度为50℃。在单因素实验的基础上,设计正交试验,优选出超声水提秦艽中龙胆苦苷的最佳工艺条件为:溶剂用量为15mL、提取时间为40min、提取次数为2次、提取温度为40℃。在单因素实验的基础上,设计正交试验,优选出索氏醇提秦艽中龙胆苦苷的最佳工艺条件为:溶剂用量为180mL、提取时间为2.5h。通过正交试验法优选出冷浸法提取秦艽中龙胆苦苷的最佳工艺条件为:乙醇浓度为60%、提取时间为12h、料液比为1∶9、提取次数为2次。选择了7种树脂对秦艽水提液中的龙胆苦苷进行吸附-解吸实验,结果表明D-101型树脂的吸附-解吸效果较好。筛选出D-101树脂的吸附-解吸条件为:pH值在2-3范围内、盐离子浓度约为1.0mol/L。

【Abstract】 Extraction、separation、purification of gentiopicroside from Gentiana macrop-Hylla Pall, produced in GanSu have been studied in this paper..The qualitative and quantitative analysis method was established by HPLC、UV with normal GPS as comparison. The method can offer favorable evidence to analyze GPS in the course of Extraction and separation.The experiments were in accordance with the national standard GB/T5009.3-2003、GB/T5009.6-2003、GB/T5009.4-2003、GB/T5009.10-2003 in measuring gentiana original herb moisture、fat、ash、crude fiber content, the results showed the average levels for targets above as followed: 11.41 %, 9.284%, 4.094%, 12.34%. Parallel experiments in various deviations were small, the measurement results were relatively credible, this can regard as right medicine general chemical composition of gentiana.On the basis of the single factor, using gentiopicroside as the index, the effects of ethanol amount, extraction time, extraction degree and extraction temperature on extraction technology were evaluated by orthogonal design method and UV. The superior technology of gentiopicroside was as followed: the ethanol was 30 ml; extraction time of 20 min, the number of extraction 4th, and the temperature was 50℃. The effects of water amount, extraction time, and extraction degree and extraction temperature on extraction technology were evaluated by orthogonal design method and Ultrasonic Wave. The superior technology of gentiopicroside was as followed: the ethanol was 15 ml; extraction time of 40 min, the number of extraction 2nd, and the temperature was 40℃.Optimized Soxhlet ethanol method, using gentiopicroside as the index, the optimum condition is the solvent dosage of 180 ml; extraction time for 2.5 h.Using cold-immersion method, by orthogonal design the optimal extraction condition was confirmed. The superior technology of gentiopicroside was as followed: ethanol concentration of 60%, extraction time of 12h and feed ratio of 1:9, 2 extraction times. Choose 8 types of resin for gentiana water extract of gentiopicroside adsorption -desorption experiments, the results showed D-101 resin adsorption - desorption method was better than others. D-101 resin selected adsorption - desorption conditions were as followed: pH within 2 -3, salt concentration of about 1.0 mol / L.

【关键词】 秦艽龙胆苦苷提取纯化
【Key words】 Gentiana macropHylla Pall.GentiopicrosideExtractionpurification
  • 【网络出版投稿人】 南昌大学
  • 【网络出版年期】2008年 06期
  • 【分类号】TQ463
  • 【被引频次】12
  • 【下载频次】996
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