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[摘要]
目的 优选大孔吸附树脂同时纯化雪松松针中莽草酸和总黄酮的最佳工艺。方法 以雪松松针中莽草酸和总黄酮的质量分数为评价指标,考察了6种树脂的纯化效果;以上样质量浓度、上样体积流量、上样量、水洗脱用量、乙醇质量浓度和乙醇洗脱用量考察了最佳树脂的纯化能力;在单因素实验的基础上,采用正交试验法,通过综合评分优选最佳的纯化工艺。结果 XAD 7HP树脂对雪松松针中莽草酸和总黄酮的纯化效果最佳,水洗脱部分为莽草酸,乙醇洗脱部分为总黄酮,其最佳的纯化工艺为上样液中莽草酸的质量浓度11.59 mg/mL和总黄酮的质量浓度6.96 mg/mL、上样体积流量8 BV/h、上样量2.0 mL/g;水洗脱用量为上样液加4 BV的水洗液、70%的乙醇洗脱4 BV。纯化后莽草酸的质量分数由19.25%提升到28.98%,总黄酮的质量分数由11.92%提升到54.45%。结论 优选的纯化工艺稳定、可行,为工业化生产雪松松针中莽草酸和总黄酮提供参考。
[Key word]
[Abstract]
Objective To research the simultaneous purification process of shikimic acid and total flavonoids from pine needles of Cedrus deodara (Roxb.) G. Don. Methods Taking the purity of shikimic acid and total flavonoids as the evaluation indicator, the purification effect of six macroporous resins were evaluated. Orthogonal design L9(34) and single factor experiments were employed to optimize the purification conditions by comprehensive scoring. The purification capacity of the best resin was investigated by the sample mass concentration, the volume flow of the sample, the ratio of the resin to the drug, the amount of water for washing, the concentration of ethanol, and the elution of ethanol. Results XAD 7HP macrophous resin offered better purification effect of shikimic acid and total flavonoids from pine needles of C. deodara than other macrophous resins. The optimum purification condition was confirmed as follows:The concentration of shikimic acid in the sample was 11.59 mg/mL, and total flavonoids concentration was 6.9 mg/mL; The flow rate was 8 BV/h, and the sample volume was 2.0 mL/g; The shikimic acid was eluted with loading capacity and 4 BV of water; The total flavonoids was eluted with 4 BV of 70% ethanol successively. The purity of shikimic acid can be increased from 19.25% to 28.98%, and the purity of total flavonoids can be increased from 11.92% to 54.45%. Conclusion The optimized purification process is stable, feasible and suitable for pilot enrichment of shikimic acid and total flavonoids from pine needles of C. deodara.
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[基金项目]
兰州市2016年第二批科技计划项目(2016-2-65);兰州市人才创新创业项目(2014-RC-62);甘肃省科技支撑计划项目(1204FKCA152)