固相萃取法纯化制备水飞蓟宾和异水飞蓟宾

发布时间：2018-03-17 09:32

本文选题：固相萃取　切入点：液相色谱　出处：《色谱》2017年01期 　论文类型：期刊论文

【摘要】：水飞蓟宾和异水飞蓟宾是水飞蓟素中的主要有效成分,其纯化制备主要借助柱色谱法,制备量大,纯化效果好,但过程非常费时。该研究的主要目的是利用更为快速高效的固相萃取(SPE)法从水飞蓟粗提物中分离纯化水飞蓟宾和异水飞蓟宾。建立了用于分析水飞蓟宾和异水飞蓟宾的高相液相色谱法,通过优化洗脱梯度,实现了水飞蓟宾、异水飞蓟宾与其他组分的分离。试用了3种保留机理不同的SPE填料,包括亲水亲脂(HLB)填料、亲水色谱(HILIC)填料及反相C18硅胶填料。通过对比发现C18硅胶对目标化合物的选择性最佳。进一步控制SPE的淋洗及洗脱条件,收集相应的洗脱液,经氮吹干燥后得到纯化的样品。提纯后的水飞蓟宾和异水飞蓟宾混合物的纯度可达94%以上。水飞蓟宾和异水飞蓟宾的平均回收率分别为70.5%~81.7%和66.7%~81.8%,相对标准偏差分别为2.7%~9.4%和1.5%~6.1%。该方法简单、高效,免去传统分离纯化过程中长时间的柱色谱分离过程,适合制备纯度较高的水飞蓟宾和异水飞蓟宾的二元混合标准样品。
[Abstract]:Silybin and isosilybin are the main effective components in silymarin. The main purpose of this study was to separate and purify silybin and isosilybin from the crude extract of silythistle by a more rapid and efficient solid-phase extraction (SPE) method. A method was established for the analysis of silybin and isosilybin. High Phase liquid Chromatography of Thistbin, By optimizing the elution gradient, the separation of silybin and isosilybin from other components was achieved. Three kinds of SPE fillers with different retention mechanisms, including hydrophilic lipophilic SPE fillers, were used. Hydrophilic chromatographic packing and reverse phase C18 silica gel filler. The results showed that C18 silica gel had the best selectivity to the target compound. The elution and elution conditions of SPE were further controlled, and the corresponding elution solution was collected. The purity of the purified silybin and isosilybin mixture can reach more than 94%. The average recoveries of silybin and isosilybin are 70.5% 81.7% and 66.7% 81.8%, respectively. The relative standard deviations are respectively. 2.7percent and 1.5percent. The method is simple, The method is highly effective and eliminates the long time column chromatographic separation process during the traditional separation and purification process. It is suitable for the preparation of binary mixed standard samples of silybin and isosilybin with high purity.
【作者单位】：大连理工大学食品与环境学院;大连理工大学文法学院;
【基金】：国家自然科学基金项目(21205058) 中央高校基本科研业务费专项资金资助项目(DUT15RC(3)048) 大连理工大学大学科技园专项项目~~
【分类号】：TQ28;O658.2

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