高速逆流色谱分离纯化氧化葵花油中三亚油酸甘油酯单氢过氧化物  

Isolation and Purification of Mono-hydroperoxide of Trilinolein from Oxidized Sunflower Oil by High-speed Counter-current Chromatography

作　　者：曾慧英[1] 刘智军[1] 谢建春[1] 孙宝国[1] 

机构地区：[1]北京工商大学北京市食品风味化学重点实验室,北京100048

出　　处：《精细化工》2013年第2期182-186,192,共6页Fine Chemicals

基　　金：国家自然科学基金项目(31171755);北京市自然科学基金项目(21220213);北京市教委科技发展计划重点项目(KZ201010011011)~~

摘　　要：该文为了获得较高纯度的三亚油酸甘油酯单氢过氧化物,用于"脂肪调控氧化-热反应"制备肉味香精机理的研究。葵花油在70℃下通空气0.72 m3/(kg.h)氧化70 h制备含三亚油酸甘油酯单氢过氧化物的氧化产物,采用液-质联机定性及液相色谱-蒸发光散射检测器面积归一化定量,氧化产物中三亚油酸甘油酯单氢过氧化物质量分数为1.95%。高速逆流色谱分离该氧化产物中的三亚油酸甘油酯单氢过氧化物,较佳的两相溶剂系统为V(正己烷)∶V(二氯甲烷)∶V(乙腈)=4∶1∶3。以上相为固定相,下相为流动相,正向洗脱,流速1.5 mL/min,转速850 r/min,上样5 g,分离时间195 min,一次性得三亚油酸甘油酯单氢过氧化物53 mg,液相色谱-蒸发光散射检测器分析纯度为96.3%,回收率52.3%。The aim of the studies described in this paper was to obtain pure mono-hydroperoxide of trilinolein, which was a substance required for the investigation of the mechanism of meat flavor formation via the technology of controlled fat oxidation combined with thermal reaction. The material containing mono-hydroperoxide of trilinolein was prepared by oxidization of sunflower oil at 70 ℃ for 70 h with air ventilated at 0. 72 ma/（ kg·h） , whereby, identified by HPLC-MS and quantified by HPLC- ELSD, the percentage of mono-hydroperoxide of trilinolein in the resulting oxidized sunflower oil was 1.95%. High-speed counter-current chromatography （HSCCC） was utilized for the separation and isolation of mono-hydroperoxide of trilinolein from the oxidized sunflower oil. The optimum two-phase solvent system selected was n-hexane-dichloromethane-acetonitrile （4：1：3 ）. With the upper phase of the two-phase solvent system as the stationary phase, and the lower phase as the mobile phase, the mobile phase was eluted in the normal direction at a flow rate of 1.5 mL/min while the revolution speed was set at 850 r/min. Under the above conditions ,53 mg of mono-hydroperoxide of trilinolein was obtained in 195 min in one run from 5 g of the oxidized sunflower oil with a purity of 96.3% and a recovery of 52.3% as determined by HPLC-ELSD.

关 键 词：三亚油酸甘油酯单氢过氧化物 高速逆流色谱 葵花油 分离 液-质联机 脂肪调控氧化 蒸发光散射检测 食品与饲料用化学品 

分 类 号：TQ656.1[化学工程—精细化工]