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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 screen the best technology of purifying Gracilaria sylvestre with D101 macroporous adsorption resin. Methods The total flavonoids, total coumarin transfer rate and its mass fraction in the solid (purity) as an indicator, by dynamic adsorption - desorption orthogonal test macroporous resin enrichment and purification factors are optimized, The HPLC method was used to determine the mass concentration of the five active ingredients in the solid before and after purification. The mass fraction was calculated and the process reliability was verified. Results The mass concentration of crude extract of D101 macroporous adsorbent was 0.250 kg.L-1 (crude drug concentration), and the volume of sample was 2.5 times the volume of body vol- ume (BV) Adsorption rate 2 BV.h-1, washing volume 5 BV. Elution with 5 BV volume fraction of 80% ethanol, elution rate of 5 BV.h-1. After purification, the total flavonoid transfer rate was 60.2% and the total coumarin transfer rate was 81.2%. The sum (purity) of the total flavonoids and total coumarins in the solid was 60.1%, about three times of that before purification. Solid content of the five active ingredients and 3.5 times before purification. Conclusion The purification process is simple and stable, increase the content of active components in the bone spargan and reduce the dosage of drugs.