【作者】 郑立友； 黄健花； 金俊； 常明； 王兴国； 金青哲；

【Author】 Zheng Liyou;Huang Jianhua;Jin Jun;Wang Xingguo;Jin Qingzhe;Synergetic Innovation Center of Food Safety and Nutrition,State Key Laboratory of Food Science and Technology,School of Food Science and Technology,Jiangnan University;Zhonghai Ocean Wuxi Marine Engineering Equipment Co.,Ltd.;

【机构】 江南大学食品学院食品科学与技术国家重点实验室食品营养与安全协同创新中心； 中海海洋无锡海洋工程装备有限公司；

【摘要】 现阶段由于α-生育酚的生物活性最强,对其生理活性的研究报道比较广泛,而对其他生育酚单体研究相对不足。本研究拟通过Grace高压制备液相系统制备生育酚单体。结果如下:将纯度为95%的生育酚混合物经甲醇溶解后进行高压制备液相色谱制备,经正反相色谱系统对比,发现反相系统相较于正相系统更为节约流动相,节约成本。反相制备具体条件如下:色谱柱为C18高压制备液相柱,流速1 mL/min,柱温为室温,反相流动相为甲醇:水(98:2,V:V),检测波长为295 nm,得到δ-生育酚纯度高达99.0%以上,其含有的其他物质主要为<1.0%的γ-+β-生育酚,得率为85.6%以上;得到的γ-+β-生育酚纯度高达99.0%以上,其含有的其他物质主要为<1.0%的δ-生育酚-生育酚,得率为76.0%以上;得到的α-生育酚纯度高达98.0%以上,其含有的其他物质主要为<2.0%的δ-生育酚-生育酚和γ-+β-生育酚,得率为60.2%。上述结果可以看出,通过该方法可以实验室内获得纯度较高的生育酚单体,用于后续单体功能性质的科学研究。更多还原

【Abstract】 Four tocopherols(a-,β-,γ-,and δ-Tocopherol) chemical difference consists in the number and position of the methyl groups of the chromanol ring.Since the biological activity of a-tocopherol is highest among the four tocopherols,studies upon this aspect are widely reported.Whereas other tocopherols apart from a-tocopherol are relatively scare.In order to investigate the biological activity of another three tocopherols,this study tried to obtain high purity of these substances with high pressure preparative HPLC.Results were below:After the mixed tocopherols were dissolved in methanol,and then applied to the high pressure preparative HPLC(both normal and reverse phase).Concerned with the purity we got and the volume mobile phase we wasted,we found the reverse phase system was better for separating the individual tocopherol.Detailed information of the reverse high pressure preparative HPLC included:mobile phase(methanol:water,98:2),wave length(295 nm),velocity(1 mL/min),temperature(ambient temperatures) and the column(C18).The purity of 8-,β-+γ-,α-tocopherol were 99%,99%,and 98%,respectively.What is more,the yield of the upper three tocopherols were 85.6%,76.0%,and 60.2%,respectively.In a word,the reverse high pressure preparative HPLC was effective to obtain the high purity and yield of individual tocopherol,which was more convenient for further researches.更多还原