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[摘要]
目的 研究应用闪式硅胶柱色谱法从厚朴总提物中分离纯化高纯度厚朴总酚的工艺。方法 以厚朴总酚的质量分数和收率为指标,采用闪式硅胶柱色谱法从样品前处理方法、硅胶用量、洗脱溶剂、体积流量方面,优选厚朴总酚的最佳纯化工艺。结果 厚朴酚、和厚朴酚在1~100 μg/mL线性关系良好(r=0.999 9)。厚朴酚、和厚朴酚的tR值分别为9.585、6.483 min。最佳工艺为:厚朴60%乙醇提取物,用10倍量的硅胶进行装柱,以石油醚-醋酸乙酯(10:1~10:3)作为梯度洗脱溶剂,体积流量选择5 mL/min。结论 与传统工艺相比,采用闪式硅胶柱色谱法以厚朴总提物为原料,能够快速、高效纯化得到质量分数>99.5%厚朴总酚。
[Key word]
[Abstract]
Objective To optimize the separation and purification of total phenols from Magnolia officinalis with flash silica gel column chromatography. Methods The content and yield of total phenols were used as makers to optimize the purification of total phenols from the method of sample pretreatment, dosage of silica gel, elution solvent, and flow rate by flash silica gel column chromatography. Results Magnolol and honokiol had a good linearity in the range of 1-100 μg/mL (r =0.999 9). The tR values of magnolol and honokiol were 9.585 and 6.483 min, respectively. The optimal processing technology was using 60% ethanol extract with the amount of 10 times silica gel, and the mobile phase was petroleum ether-ethyl acetate (10:1-10:3) in gradient elution mode. The flow rate was controlled at 5 mL/min. Conclusion Compared with the traditional method, using flash silica gel chromatography with the total extract is easy to obtain the total magnolol with the purity more than 99.5% quickly.
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[基金项目]
辽宁省教育厅项目(L2012364);辽宁省高等学校杰出青年学者成长计划项目(LJQ2012088)