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目的:对大孔树脂富集纯化布渣叶总黄酮的工艺条件及参数进行优化。方法:先以总黄酮比吸附量和解吸率为指标,通过静态和动态吸附-解吸附试验筛选出合适的树脂;再通过单因素试验考察最佳洗脱剂浓度,利用均匀设计对富集纯化工艺参数进行优化;并用液相色谱对处理前后的试样进行定性分析。结果:D101树脂具有良好的吸附分离性能;选择70%乙醇为洗脱剂,以总黄酮收率为指标,优选的工艺参数为:上样流速1.0BV/h、洗脱流速2.0BV/h、上样浓度7.88 mg/mL、洗脱剂用量2.0BV和pH值4.8,其收率达到90.18%,纯度54.37%;以总黄酮纯度为指标,优化的工艺参数为:上样流速1.0BV/h、洗脱流速2.0BV/h、上样浓度2.0 mg/mL、洗脱剂用量2.8BV和pH值7.8,其纯度为61.77%,收率80.25%。色谱分析结果表明,大孔树脂处理前后布渣叶总黄酮主成分相同。结论:D101大孔树脂吸附分离工艺能有效地对布渣叶总黄酮进行富集。
OBJECTIVE: To optimize the conditions and parameters of macroporous resin enrichment and purification of total flavonoids from Clorius leaf. Methods: The total flavonoids than the amount of adsorption and desorption rate as an indicator, through static and dynamic adsorption-desorption test screened the appropriate resin; and then through the single factor test to study the optimal concentration of eluent, uniform design enrichment purification Process parameters were optimized; and qualitative analysis of the sample before and after treatment with liquid chromatography. Results: D101 resin had good performance of adsorption and separation. 70% ethanol was chosen as eluent and total flavonoid yield was taken as an index. The optimal process parameters were as follows: sample flow rate 1.0BV / h, elution flow rate 2.0BV / h, The yield of the sample was 7.88 mg / mL, the amount of eluent was 2.0BV and the pH value was 4.8. The yield was 90.18% and the purity was 54.37%. The optimized process parameters were as follows: the sample flow rate 1.0BV / h , The elution flow rate was 2.0BV / h, the sample concentration was 2.0 mg / mL, the eluent dosage was 2.8BV and the pH was 7.8. The purity was 61.77% and the yield was 80.25%. The results of chromatographic analysis showed that the main components of the total flavonoids from the cloth residue were the same before and after macroporous resin treatment. Conclusion: D101 macroporous resin adsorption separation technology can effectively enrich the total flavonoids of the cloth residue.