大孔树脂分离纯化菊苣中香豆素的工艺研究

目的筛选大孔树脂分离纯化菊苣香豆素的最佳工艺。方法以香豆素的吸附量为指标,采用单因素试验法对影响菊苣提取物纯化效率的因素进行优化,分别采用UV和HPLC测定纯化后固形物中总香豆素和秦皮乙素的浓度。结果最佳洗脱程序为,选定D101大孔树脂,上样浓度为0.35 mg.mL 1,最大上样量为35 BV(35倍柱体积),上样速度为0.067BV.min 1,依次用11 BV的蒸馏水以0.067 BV.min 1的流速洗脱,9 BV的30%乙醇以0.033 BV.min 1的流速洗脱,弃去洗脱液,再用9 BV的80%乙醇以0.033 BV.min 1的流速洗脱,收集洗脱液。纯化得到的固形物中菊苣香豆素含量为47.00%,秦皮乙素含量为6.38%,香豆素的转移率为81.74%。结论纯化工艺简便、稳定,能提高菊苣中活性组分的含量。

Study on the Purification of Coumarin in Chicory with Macroporous Resin

OBJECTIVE To select the optimal purification technology of coumarin in Cichorium glafulosum Boiss. et Huet with macroporous resin. METHODS Mono factor test were employed to investigate the main parameters which may affect the purification procedures with the concentration of coumarin as index. The contents of the total coumarin and esculetin were verified by UV and HPLC separately in purified dried solid. RESULTS The optimal procedure was using D101 macroporous resin, the content of coumarin was 0.35 mg·mL^-1, the volume was 35 BV, the flow rate was 0.067 BV·min^-1. To elute with distilled water, the volume was 11 BV, the flow rate was 0.067 BV·min^-1, and with 30% ethanol, the volume was 9 BV, the flow rate was 0.033 BV·min^-1, giving up the eluate. To elute with 80% ethanol, the volume was 9 BV, the flow rate was 0.033 BV·min^-1, gathering the eluate. The content of coumarin and esculetin reached 47.00% and 6.38% separatelyin purified powders, the transfer rates of coumarin reached 81.74%. CONCLUSION The optimized technology is simple, stable, can significantly improve the contents of active constituents in Cichorium glafulosum Boiss.et Huet.