信长颖,刘彦杉,张上上,熊志立,郭兴杰,李发美
XIN Chang-ying,LIU Yan-shan,ZHANG Shang-shang,XIONG Zhi-li,GUO Xing-jie,LI Fa-mei(School of Pharmacy

• 1:沈阳药科大学药学院

摘要(Abstract)：

目的筛选D101大孔吸附树脂纯化骨疏丹提取物的最佳工艺。方法以总黄酮、总香豆素的转移率及其在固形物中的质量分数之和(纯度)为指标,通过动态吸附-解吸正交试验对影响大孔吸附树脂富集纯化因素进行优化,用HPLC法测定优选工艺纯化前后固形物中5种活性成分的质量浓度,计算其含量质量分数,并验证工艺的可靠性。结果 D101型大孔吸附树脂纯化骨疏丹提取物的上样质量浓度为0.250 kg.L-1(生药质量浓度),上样体积为2.5倍树脂柱床体积(body vol-ume,BV),吸附速率2 BV.h-1,水洗体积5 BV。用体积分数为80%乙醇溶液洗脱5 BV,洗脱速率5 BV.h-1。纯化后总黄酮转移率为60.2%,总香豆素转移率为81.2%,固形物中总黄酮、总香豆素质量分数之和(纯度)为60.1%,约为纯化前的3倍。固形物中5种活性成分质量分数之和为纯化前的3.5倍。结论纯化工艺简单、稳定,提高骨疏丹中活性组分的含量,减少药物服用量。
Objective To select the optimal purification technology of Gushudan(traditional Chinese medicines)extracts with D101 macroporous adsorption resin.Methods The dynamic adsorption and desorption orthogonal tests were employed to investigate effects of enrichment and purification procedures for the total flavonoids and coumarins from Gushudan extracts with the transfer rates and the sum of contents in the dried solid(degree of purity)of the total flavonoids and coumarins as index.At last,the contents of five active constituents(naringin,epimedin,icariin,osthole,tanshinoneⅡA)were verified by HPLC.Results The optimal purifying condition was as follows:the Gushudan extracts solution of 2.5 times of the resin body volume(BV)(0.250 kg · L-1 of the raw material concentration)was loaded with a speed of 2 BV · h-1 in room temperature,and the diameter-high ratio of the resin was 1∶ 3,the impurity was washed away with 5 times of the resin BV water.And then,the total flavonoids and coumarins were eluated with 80% ethanol.And the eluant volume was 5 times of the resin BV.The eluting rate was 5 times of BV · h-1.After purification,the transfer rate of total flavonoids and coumarins was 60.2% and 81.2%,the sum of contents of total flavonoids and coumarins in the dried solid(degree of purity)was 60.1%,and was twice higher more than before.The sum of five active constituents′ contents in dried solid was 2.5 times higher than before.Conclusions The optimized technology is simple,stable,can significantly improve the contents of active constituents in Gushudan extracts,and thus the administrated amount of the drug is decreased.

关键词(KeyWords)： 骨疏丹;黄酮;香豆素;大孔吸附树脂;纯化
Gushudan;flavonoid;coumarin;macroporous adsorption resin;purification

Abstract:

Keywords:

基金项目(Foundation): 国家科技重大专项资助项目(2010ZX09401-304)

作者(Author): 信长颖,刘彦杉,张上上,熊志立,郭兴杰,李发美
XIN Chang-ying,LIU Yan-shan,ZHANG Shang-shang,XIONG Zhi-li,GUO Xing-jie,LI Fa-mei(School of Pharmacy

DOI: 10.14066/j.cnki.cn21-1349/r.2012.01.012

参考文献(References)：

• [1]张丹,刘铮,李发美,等.骨疏丹抗骨质疏松的药理作用[J].中草药,2008,39(8):1205-1206.
• [2]李发美,孟繁浩,梁茂新,等.治疗骨质疏松症的中药小复方及其制备方法:中国,200410021121.0[P].2004-12-29.
• [3]孟繁浩.中药精选小复方骨疏丹促成骨细胞骨形成作用的研究[D].沈阳:沈阳药科大学,2004:80-102.
• [4]赵丽恋,刘韶,罗杰英,等.大孔吸附树脂-超声波辅助解吸附法纯化淫羊藿中的总黄酮[J].中国中药杂志,2009,34(6):702-704.
• [5]刘健伟,陈勇,熊富良,等.骨碎补总黄酮提取和大孔吸附树脂纯化的工艺研究[J].中国药学杂志,2006,41(16):1222-1224.
• [6]史万忠,刘瑾,吕海阳,等.大孔吸附树脂纯化补肾方中总黄酮的工艺研究[J].中成药,2009,31(7):1024-1028.
• [7]张霄翔,邵胜男,周慧慧,等.大孔吸附树脂纯化丹参总酚酸的工艺研究[J].中成药,2007,29(9):1288-1291.
• [8]孟召全,陈鸿楠,钱捷.丹参酮ⅡA的分离纯化[J].中国实验方剂学杂志,2010,16(2):6-7.
• [9]刘曼.骨疏丹促成骨细胞活性的物质基础相关研究[D].沈阳:沈阳药科大学,2007:28-35.
• [10]张兆旺.中药药剂学[M].北京:中国中医药出版社,2002:624.