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目的:优选D101型大孔树脂纯化九龙藤总黄酮的工艺条件,为该成分的工业制剂开发提供参考。方法:以总黄酮纯度及回收率为评价指标,在单因素试验基础上,采用正交试验考察上样液质量浓度、洗脱剂浓度、洗脱速度及上样液p H对九龙藤总黄酮大孔树脂纯化工艺的影响。采用UV测定黄芩苷含量,检测波长278.5 nm。结果:最佳纯化工艺为上样液质量浓度15.5 g·L-1,上样液p H 2~3,最大上样量16.85 mg·g-1,上样速度0.125 BV·h-1,径高比1∶6,加60%乙醇4 BV以1 BV·h-1洗脱。总黄酮纯度48.95%,回收率96.08%。结论:优选的纯化工艺稳定可行,有效提高了九龙藤总黄酮纯度及回收率,适用于九龙藤总黄酮的纯化。
Objective: To optimize the process conditions of D101 macroporous resin for purification of total flavonoids from Jiulongtong, and provide a reference for the industrial formulation development of this component. Methods: The purity and recovery of total flavonoids as the evaluation index, on the basis of single factor experiment, using orthogonal test to examine the sample solution concentration, eluent concentration, elution rate and the sample p H on the total flavonoids Effect of macroporous resin purification process. Determination of baicalin by UV, detection wavelength 278.5 nm. Results: The optimal purification process was as follows: the sample concentration of 15.5 g · L-1, the sample of p H 2 ~ 3, the maximum loading amount of 16.85 mg · g -1, the loading speed of 0.125 BV · h -1 High 1: 6, plus 60% ethanol 4 BV at 1 BV · h-1. Total flavonoids purity 48.95%, 96.08% recovery. Conclusion: The optimized purification process is stable and feasible, which can effectively improve the purity and recovery rate of total flavonoids in Jiulongtang, and is suitable for the purification of total flavonoids in Jiulongtong.