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

摘要:

本文研究是为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”制备肉味香精机理研究。葵花油在70℃下通空气0.72 m3/kg?h氧化70h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含量为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正己烷/二氯甲烷/乙腈（4:1:3，V/V/V）。以上相为固定相，下相为流动相，正向洗脱，流速1.5mL/min，转速850rpm/min，上样5g，分离时间195min，一次性得三亚油酸甘三酯单氢过氧化物53mg，液相色谱-蒸发光散射检测器分析纯度为96.3%，回收率52.3%。

Abstract:

The aim of this paper was to obtain pure mono-hydroperoxide of trilinolein, which was a substance we required for the investigation of the mechanism of meat flavor formation via the technology of controlled fat oxidation combined with the thermal reaction. The material containing mono-hydroperoxide of trilinolein was prepared by oxidization of sunflower oil at 70 oC for 70 h with air ventilated at 0.72m3/kg?h, whereby the percentage of mono-hydroperoxide of trilinolein in the resulting oxidized sunflower oil was 1.95% identified by HPLC-MS and quantified by HPLC-ELSD. High-speed counter-current chromatography (HSCCC) was utilized for 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, V/V/V). 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 rpm/min. By 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 in a purity of 96.3% analyzed by HPLC-ELSD, and the recovery was 52.3%.