骨疏丹提取物的大孔吸附树脂纯化工艺研究

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。

Purification technology of Gushudan extracts with D101 macroporous adsorption resin

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.