蒙药漏芦花总黄酮提取和纯化工艺研究
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摘要
[目的]优化漏芦花总黄酮提取工艺和纯化工艺,为漏芦花抗炎药效部位的开发奠定基础。[方法]以总黄酮为指标,采用UV测定方法,在检测波长413 nm下,测定总黄酮含量,确定纯化漏芦花总黄酮纯化大孔树脂型号;并采用正交试验分别考察乙醇浓度、回流次数、回流时间和乙醇用量对漏芦花总黄酮提取工艺的影响及乙醇体积分数、上样液质量浓度、p H和上样液流速对总黄酮纯化工艺的影响。[结果]确定漏芦花总黄酮提取工艺的最优方案为采用75%乙醇溶液,回流2次,每次回流时间45 min,乙醇用量12倍,影响因素的顺序从大到小依次为乙醇浓度、回流时间、乙醇用量、回流次数。纯化工艺试验中,最优纯化工艺条件为上样液浓度0.05 g/m L,上样液p H为5,上样液流速为3 m L/min,径高比为1∶9,最佳上样量为药材量与树脂用量比2∶1,乙醇体积分数50%,洗脱液用量5 BV;纯化后干膏里漏芦花抗炎有效部位总黄酮含量为42.3%。[结论]AB-8型大孔树脂可有效富集、纯化漏芦花总黄酮,优选的提取和纯化工艺稳定可行。
[Objective] To optimize extraction and purification process of total flavonoids from Rhaponticum uniflorum,to lay a foundation for development of anti-inflammatory parts of Rhaponticum uniflorum. [Method]UV was employed to determine the content of total flavonoids with detection wavelength at 413 nm; using orthogonal design to investigate effects of ethanol concentration,reflux times,reflux time and alcohol dosage on extraction of total flavonoids from Rhaponticum uniflorum,as well as effects of ethanol volume fraction,mass concentration of sample solution,p H and sample liquid flow rate on purification of total flavonoids. [Result] As for extraction process,the optimum scheme was: 12 times extraction solvent dosage,75% ethanol reflux,extraction for 2 times,each time for 45 minutes. The order of influencing factors was ethanol concentration,reflux time,ethanol dosage and reflux times. As for purification process,optimum technological conditions were as follows: ratio of diameter-height 1∶ 9,sample solution concentration of 0. 05 g/m L,sample solution flow rate of 3 m L/min,p H 5. 0,with 5 BV of 75% ethanol as eluent; total flavonoids was 42. 3% in anti-inflammatory parts of Rhaponticum uniflorum after purification. [Conclusion]Total flavonoids from Rhaponticum's dried flowers could be effectively purified and enriched by AB-8 macroporous resin.
[Objective] To optimize extraction and purification process of total flavonoids from Rhaponticum uniflorum,to lay a foundation for development of anti-inflammatory parts of Rhaponticum uniflorum. [Method]UV was employed to determine the content of total flavonoids with detection wavelength at 413 nm; using orthogonal design to investigate effects of ethanol concentration,reflux times,reflux time and alcohol dosage on extraction of total flavonoids from Rhaponticum uniflorum,as well as effects of ethanol volume fraction,mass concentration of sample solution,p H and sample liquid flow rate on purification of total flavonoids. [Result] As for extraction process,the optimum scheme was: 12 times extraction solvent dosage,75% ethanol reflux,extraction for 2 times,each time for 45 minutes. The order of influencing factors was ethanol concentration,reflux time,ethanol dosage and reflux times. As for purification process,optimum technological conditions were as follows: ratio of diameter-height 1∶ 9,sample solution concentration of 0. 05 g/m L,sample solution flow rate of 3 m L/min,p H 5. 0,with 5 BV of 75% ethanol as eluent; total flavonoids was 42. 3% in anti-inflammatory parts of Rhaponticum uniflorum after purification. [Conclusion]Total flavonoids from Rhaponticum's dried flowers could be effectively purified and enriched by AB-8 macroporous resin.
引文
[1]中华人民共和国卫生部药典委员会.中华人民共和国卫生部药品标准:蒙药分册[S].北京:人民卫生出版社,1998.
[2]内蒙古自治区卫生厅.内蒙古蒙药材标准[S].呼和浩特:内蒙古科学技术出版社,1987:511.
[3]朱培忠,蒋素容.漏芦花泡麻油治疗烧、烫伤[J].四川中医,1985(8):47.
[4]武雪琴.蒙药漏芦花的研究及在蒙医临床中的应用[J].中国民族医药杂志,2015(8):46-47.
[5]张学武,李天洙,孙权.漏芦提取物抗炎、镇痛、耐缺氧及抗疲劳作用的研究[J].四川中医,2005,23(7):22,23.
[6]孙洁宇,虞玮.蒙药漏芦花化学成分分析及活性成分筛选实验[J].中国民族医药杂志,2003(S1):29-31.
[7]萨楚拉图.蒙药漏芦花黄酮类化合物的提取分离与结构表征[D].呼和浩特:内蒙古大学,2009.
[8]刘明生,李铣.祁州漏芦化学成分研究[J].时珍国医国药,1998,9(4):329.
[9]王晓静,丁杏苞,吴克霞,等.祁州漏芦茎叶化学成分的研究[J].中草药,2001,32(7):590.
[10]包小妹,刘乐乐,罗素琴,等.蒙药漏芦花的化学成分研究[J].中华中医药杂志,2012(7):1914-1915.
[11]程捷恺,张永红,张自义,等.祁州漏芦中蜕皮甾酮类化学成分的研究[J].高等学校化学学报,2002,23(11):2084-2088.
[12]赵继明.枸杞子不同提取物中总黄酮含量比较[J].现代中西医结合杂志,2012,21(6):647-648.
[13]池玉梅,居羚,邓海山,等.分光光度测定总黄酮法的适用性[J].分析化学,2010,38(6):893-896.
[14]刘计权,谢树莲,蔡瑾,等.UV和HPLC测定草问荆总黄酮及山柰素含量[J].山西大学学报(自然科学版),2011,34(3):480-484.
[2]内蒙古自治区卫生厅.内蒙古蒙药材标准[S].呼和浩特:内蒙古科学技术出版社,1987:511.
[3]朱培忠,蒋素容.漏芦花泡麻油治疗烧、烫伤[J].四川中医,1985(8):47.
[4]武雪琴.蒙药漏芦花的研究及在蒙医临床中的应用[J].中国民族医药杂志,2015(8):46-47.
[5]张学武,李天洙,孙权.漏芦提取物抗炎、镇痛、耐缺氧及抗疲劳作用的研究[J].四川中医,2005,23(7):22,23.
[6]孙洁宇,虞玮.蒙药漏芦花化学成分分析及活性成分筛选实验[J].中国民族医药杂志,2003(S1):29-31.
[7]萨楚拉图.蒙药漏芦花黄酮类化合物的提取分离与结构表征[D].呼和浩特:内蒙古大学,2009.
[8]刘明生,李铣.祁州漏芦化学成分研究[J].时珍国医国药,1998,9(4):329.
[9]王晓静,丁杏苞,吴克霞,等.祁州漏芦茎叶化学成分的研究[J].中草药,2001,32(7):590.
[10]包小妹,刘乐乐,罗素琴,等.蒙药漏芦花的化学成分研究[J].中华中医药杂志,2012(7):1914-1915.
[11]程捷恺,张永红,张自义,等.祁州漏芦中蜕皮甾酮类化学成分的研究[J].高等学校化学学报,2002,23(11):2084-2088.
[12]赵继明.枸杞子不同提取物中总黄酮含量比较[J].现代中西医结合杂志,2012,21(6):647-648.
[13]池玉梅,居羚,邓海山,等.分光光度测定总黄酮法的适用性[J].分析化学,2010,38(6):893-896.
[14]刘计权,谢树莲,蔡瑾,等.UV和HPLC测定草问荆总黄酮及山柰素含量[J].山西大学学报(自然科学版),2011,34(3):480-484.