碱水解橄榄苦苷制备羟基酪醇及其抗氧化活性研究  

Preparation and anti-oxidative activity of hydroxytyrosol by alkaline hydrolysis of oleuropein

作　　者：谢普军[1,2] 黄立新[1,2] 张彩虹[1,2] 游凤[1,2] 张耀雷[1,2] 

机构地区：[1]中国林业科学研究院林产化学工业研究所生物质化学利用国家工程实验室,国家林业局林产化学工程重点开放性实验室,江苏省生物质能源与材料重点实验室,江苏南京210042 [2]中国林业科学研究院林业新技术研究所,北京100091

出　　处：《中草药》2013年第15期2075-2078,共4页Chinese Traditional and Herbal Drugs

基　　金："十二五"国家科技支撑计划(2012BAD32B10);"863"课题项目"食品高效节能干燥装备开发与新技术研究"(2011AA100802)

摘　　要：目的以橄榄苦苷粗制品为原料,在强碱作用下水解制备羟基酪醇,并对其进行体外抗氧化活性研究。方法选取4个因素,即水解温度、NaOH浓度、水解时间和料液比进行单因素试验;在其基础上进行L9(34)正交试验设计优化;利用HPLC-MS对羟基酪醇进行定性分析,同时在相同条件下进行酸水解对比试验和对羟基酪醇清除DPPH抗氧化活性评价。结果选取的4个因素均极显著,主次因素顺序为水解温度>NaOH浓度>水解时间>料液比,优化水平组合为水解温度90℃,NaOH浓度0.2 mol/L,水解时间45 min,料液比1∶15;羟基酪醇的色谱保留时间约为10.3 min,且质谱条件下产生的碎片离子相对分子质量为134.8。通过酸与碱水解对比试验发现,橄榄苦苷在碱性条件下水解制备羟基酪醇的效率更高;与2,6-二叔丁基-4-甲基苯酚(BHT)对比,羟基酪醇清除DPPH能力是BHT的2.45倍。结论羟基酪醇的制备在碱性条件下产率较高,且具有较好的抗氧化活性。Objective To prepare hydroxytyrosol （HT） by alkaline hydrolysis of oleuropein and to investigate its anti-oxidative property. Methods According to single factor experiments, four variables： temperature, sodium hydroxide concentration, time, and the ratio of solid to liquid, were selected. On the basis of single factor experiments, orthogonal tests of L9（34） were carried out. HPLC-MS method was also further applied for the qualitative analysis on HT. Under the same conditions, contrast experiments on the acid and alkaline actions were made. Finally, anti-oxidative activity of HT was evaluated. Results The results showed that the selected variables were all highly significant. Also, the descending influence orders on HT were temperature 〉 sodium hydroxide concentration 〉 time 〉 the ratio of solid to liquid. Lastly, the optimal conditions on HT yield were obtained as follow： temperature 90 ℃, sodium hydroxide concentration 0.2 mol/L, time 45 min, and the ratio of solid to liquid 1 ： 15. The HPLC retention time of HT was about 10.3 min, and its relative molecular weight of fragment ion by MS was 134.8. By comparison with the acid action, it was proved that the alkaline action was better in HT yield. In addition, the anti-oxidative activity of HT was carded out on scavenging DPPH radical. The results showed that DPPH scavenging capability of HT was 2.45 times of BHT. Conclusion HT yield is well obtained under the alkaline condition and has a good anti-oxidation.

关 键 词：橄榄苦苷 碱水解 羟基酪醇 HPLC-MS DPPH 自由基 正交试验设计 

分 类 号：R284.1[医药卫生—中药学]