老鹳草中鞣质类成分提取、纯化及其胃内漂浮片的制备
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摘要
中药老鹳草具有祛风湿、通经络、止泻痢等功能。其主要化学成分包括鞣质、挥发油、黄酮类和有机酸等,其中鞣质类成分含量较高。研究表明,老鹳草鞣质类提取物具有较好的抗溃疡作用。
对老鹳草中鞣质类成分进行提取、纯化,优化提取、纯化工艺参数,制定提取物质量标准；以老鹳草鞣质提取物为主要原料制备其胃内漂浮片,确定制剂处方和制备方法,建立质量标准。
采用超声循环提取工艺,鞣质类成分的提取率明显提高,优化工艺参数为：40%乙醇12倍量,室温下提取1h,间隔超声比为0.6：0.5s,功率为500W。
明胶沉淀总鞣质,丙酮溶液使沉淀物溶解释放鞣质,初步纯化老鹳草提取液,优化工艺参数为：老鹳草提取液:4%明胶溶液(10：1),50%丙酮溶解效果最佳。
大孔吸附树脂HPD100纯化工艺参数：径高比为1：5,上样溶液50 mL(每1 mL相当于30g生药),用500 mL蒸馏水与250 mL15%乙醇除杂,70%乙醇250 mL以1.5 BV·h-1洗脱。
提取物质量标准的研究：没食子酸为对照品,采用薄层色谱法与高效液相色谱法对老鹳草提取物进行定性鉴别与含量测定。
老鹳草总鞣质胃漂浮型缓释片的处方为：提取物粉末：HPMC:PVPP:MCC: NaHCO3 (24:78:18:12:13.2);该制剂平均片重为150.2 mg,起漂时间＜3 min,持续漂浮时间>8 h,4 h累积释放度>50%,8h累积释放度可达75%。
老鹳草中总鞣质提取、纯化工艺稳定可行,提取物质量可控；以老鹳草鞣质为原料制备的胃内漂浮片初步具备了胃内漂浮制剂特征。
Geranium wilfordii Maxim component of the Chinese medicine has the ability of reducing rheumatism, smoothening energy channel, curing durchfall and so on. Geranium wilfordii Maxim includes main chemical compositions such as tannins, volatile oils, organic acids, in particular, the tannnins are rich in it. Study suggest that the extractive tannins in Geranium wilfordii Maxim has the effective ability of antiulcer.
To optimize the extraction and purification process of tannins from Geranium wilfordii Maxim component of the Chinese medicine, and formulate the quality standard of extractive. Based on the major ingredients from extractive of Geranium wilfordii Maxim Tannins component, Preparation for the gastric-floating tablets, confirms the prescription and method, and establishes the quality standard.
By the adoption of ultrasonic and circulated extraction process, the extraction rate of the Tannins component has increased obviously. The optimal parameters were obtained as follows: dosage liquor ratio was 1:12; the solvent was 40% alcohol; the extraction temperature was 20℃; the extraction time was 1 h; the interval time of the extraction time was 0.6:0.5 s; the ultrasoud power was 500 W.
The general Tannins of gelatin sediment and acetone solution make sediment dissolve and release tannins putrefy the geranium extract preliminary. The optimal parameters were obtained as follows:the volume of Geranium wilfordii Maxim extractation was ten times than 4% gelatin solution and the optimal solvent was 50% acetone.
Macroporous resins HPD100 purification parameters were obtained as follows:diameter and height ratio was 1:5, sample solution was 50 mL (1 mL sample equals 30 g raw Geranium wilfordii Maxim), cleaning by 500 mL distilled water and 250 mL 15% alcohol, then eluting by 250ml 70% alcohol in 1.5 BV·h-1.
The research for extraction quality standard:gallic acid is control article, uses TLC and HPLC for qualitative identification and content mensuration to Geranium wilfordii Maxim extract.
The prescription for Geranium wilfordii Maxim tannins of gastric-floating tablets was obtained as follows:HPMC:PVPP:MCC:NaHCO3(0.4:1.5:0.3:0.2:0.24); the average weight of the tablet is 150.2 mg, initial floating time<3 min, continued floating time>8 h, 4 h cumulating releasing rate>50%,8h cumulating releasing rate attained to 75%.
The extraction and purification process for Geranium wilfordii Maxim tannins is steady and available, the quality of extract is controllable. The gastric-floating tablets is made by material from Geranium wilfordii Maxim tannins possesses the characteristics of gastric-floating tablets.
对老鹳草中鞣质类成分进行提取、纯化,优化提取、纯化工艺参数,制定提取物质量标准；以老鹳草鞣质提取物为主要原料制备其胃内漂浮片,确定制剂处方和制备方法,建立质量标准。
采用超声循环提取工艺,鞣质类成分的提取率明显提高,优化工艺参数为：40%乙醇12倍量,室温下提取1h,间隔超声比为0.6：0.5s,功率为500W。
明胶沉淀总鞣质,丙酮溶液使沉淀物溶解释放鞣质,初步纯化老鹳草提取液,优化工艺参数为：老鹳草提取液:4%明胶溶液(10：1),50%丙酮溶解效果最佳。
大孔吸附树脂HPD100纯化工艺参数：径高比为1：5,上样溶液50 mL(每1 mL相当于30g生药),用500 mL蒸馏水与250 mL15%乙醇除杂,70%乙醇250 mL以1.5 BV·h-1洗脱。
提取物质量标准的研究：没食子酸为对照品,采用薄层色谱法与高效液相色谱法对老鹳草提取物进行定性鉴别与含量测定。
老鹳草总鞣质胃漂浮型缓释片的处方为：提取物粉末：HPMC:PVPP:MCC: NaHCO3 (24:78:18:12:13.2);该制剂平均片重为150.2 mg,起漂时间＜3 min,持续漂浮时间>8 h,4 h累积释放度>50%,8h累积释放度可达75%。
老鹳草中总鞣质提取、纯化工艺稳定可行,提取物质量可控；以老鹳草鞣质为原料制备的胃内漂浮片初步具备了胃内漂浮制剂特征。
Geranium wilfordii Maxim component of the Chinese medicine has the ability of reducing rheumatism, smoothening energy channel, curing durchfall and so on. Geranium wilfordii Maxim includes main chemical compositions such as tannins, volatile oils, organic acids, in particular, the tannnins are rich in it. Study suggest that the extractive tannins in Geranium wilfordii Maxim has the effective ability of antiulcer.
To optimize the extraction and purification process of tannins from Geranium wilfordii Maxim component of the Chinese medicine, and formulate the quality standard of extractive. Based on the major ingredients from extractive of Geranium wilfordii Maxim Tannins component, Preparation for the gastric-floating tablets, confirms the prescription and method, and establishes the quality standard.
By the adoption of ultrasonic and circulated extraction process, the extraction rate of the Tannins component has increased obviously. The optimal parameters were obtained as follows: dosage liquor ratio was 1:12; the solvent was 40% alcohol; the extraction temperature was 20℃; the extraction time was 1 h; the interval time of the extraction time was 0.6:0.5 s; the ultrasoud power was 500 W.
The general Tannins of gelatin sediment and acetone solution make sediment dissolve and release tannins putrefy the geranium extract preliminary. The optimal parameters were obtained as follows:the volume of Geranium wilfordii Maxim extractation was ten times than 4% gelatin solution and the optimal solvent was 50% acetone.
Macroporous resins HPD100 purification parameters were obtained as follows:diameter and height ratio was 1:5, sample solution was 50 mL (1 mL sample equals 30 g raw Geranium wilfordii Maxim), cleaning by 500 mL distilled water and 250 mL 15% alcohol, then eluting by 250ml 70% alcohol in 1.5 BV·h-1.
The research for extraction quality standard:gallic acid is control article, uses TLC and HPLC for qualitative identification and content mensuration to Geranium wilfordii Maxim extract.
The prescription for Geranium wilfordii Maxim tannins of gastric-floating tablets was obtained as follows:HPMC:PVPP:MCC:NaHCO3(0.4:1.5:0.3:0.2:0.24); the average weight of the tablet is 150.2 mg, initial floating time<3 min, continued floating time>8 h, 4 h cumulating releasing rate>50%,8h cumulating releasing rate attained to 75%.
The extraction and purification process for Geranium wilfordii Maxim tannins is steady and available, the quality of extract is controllable. The gastric-floating tablets is made by material from Geranium wilfordii Maxim tannins possesses the characteristics of gastric-floating tablets.
引文
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[3]宋华.老鹳草的药理作用研究进展[J].中草药,1997,28(A10)：132-135.
[4]雷海民,魏露雪,林文翰,等.粗根老鹳草化学成分的研究[J].药学学报,2000,35(1)：67-69.
[5]吴悦涛,金哲雄.老鹳草中鞣质类化学成分及其药理活性研究进展[J].黑龙江医药,2008,21(1)：67-68.
[6]阎巧娟,韩鲁佳,江正强.老鹳草鞣质的提取工艺及其免疫作用的试验研究[J].中国农业大学学报,2002,7(6)：16.
[7]中西由香.老鹳草素对实验性大鼠盐酸、酒精性溃疡的保护作用[J].国外医学中医中药分册,1993,15(1)：23.
[8]于海玲,郭建鹏,王丹.老鹳草对小鼠无水乙醇型胃溃疡的影响.时珍国医国药杂志,2007,18(4)：874-875.
[9]于海玲,郭建鹏,孙连平.老鹳草提取物对实验性胃溃疡小鼠胃粘膜的保护作用机制研究[J].延边大学医学学报,2007,30(1)：29-31.
[10]范红艳,郭建鹏,于海玲.老鹳草提取物对消炎痛型及利血平型胃溃疡小鼠溃疡指数的影响.延边大学医学学报,2006,29(4)：256-258.
[11]马玉林,谢平.中草药提取工艺研究概括[J].中医药学刊,2002,20(5)：647-649.
[12]周淑芳,韩丽副主编,谢秀琼主编.现代中药制剂新技术[M].第一版,北京：化学工业出版设,2004：30-31.
[13]董发明,白喜婷.响应面法优化超声提取杜仲雄花中黄酮类化合物的工艺参数[J].食品科学,2008,29(8)：227-231.
[14]国家药典委员会.中华人民共和国药典一部[S].北京：化学工业出版社,2005：附录57.
[15]辛聪,郭建鹏.均匀设计优化老鹳草鞣质提取工艺[J].时珍国医国药杂志,2006,17(5)：702-703.
[16]袁怀渡,赵国华,李洪军,等.利用大孔吸附树脂纯化葛根黄酮的研究[J].食品与发酵工业,2003,29(2)：62-65.
[17]张素琼,侯晋军,李青山.大孔树脂同步分离纯化罗布麻叶总黄酮和总鞣质的研究[J].中国中药杂志,2008,33(10)：1141-1144.
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