大豆油脱臭馏出物中角鲨烯的分离纯化工艺研究

Study on separation and purification of squalene from soybean oil deodorizer distillate

文章采用银离子络合萃取结合柱层析的方法从大豆油脱臭馏出物中分离纯化角鲨烯。先利用响应面法优化银离子络合萃取角鲨烯的最佳工艺条件。然后以硅胶为固定相,正己烷为流动相,考察洗脱速度和上样量等因素对层析效果的影响,最终确定柱层析的最佳工艺条件。实验结果显示:银离子络合萃取的最佳工艺条件为甲醇体积分数60%、萃取温度0℃、萃取时间8 h、AgNO_3的浓度1.5 mol/L、投料比4∶1、反萃取时间60 min、反萃取温度65℃,在此条件下,角鲨烯纯度为46.52%,得率为77.27%;经柱层析进一步纯化,在流速为15 mL/min,上样量与干硅胶的质量比为1∶20的条件下收集流出液,经高效液相色谱(high performance liquid chromatography,HPLC)分析,收集的流出液中角鲨烯回收率达到96.13%,纯度为94.16%;银离子络合萃取结合柱层析的方法分离纯化角鲨烯的得率和纯度比现有方法均有明显提高,且选择性强、易操作。

In this paper, the separation and purification of squalene by silver ion complexation extraction combined with column chromatography from soybean oil deodorizer distillate were studied. Response surface methodology was used to optimize the optimal extraction conditions of squalene by silver ion complexation extraction method. Then the optimal column chromatography conditions were determined by using silica gel as the stationary phase and n-hexane as the mobile phase, considering the effect of the elution rate and the amount of sample on the chromatography. It was found that the optimal extraction conditions of squalene by silver ions extraction method were a methanol volume fraction of 60%, extraction temperature of 0 ℃, extraction time of 8 h, AgNO 3 concentration of 1.5 mol /L and feed ratio of 4∶1. The optimum reverse extraction time was 60 min and the reverse extraction temperature was 65 ℃. Under these conditions, the yield of squalene was 77.27% and the purity was 46.52%. Squalene was further purified by the column chromatography. The effluent was collected under the conditions that the flow rate was 15 mL/min and the ratio of the amount of sample to dry silica gel was 1∶20. By high performance liquid chromatography(HPLC) analysis, the recovery of squalene in the collected solution reached 96.13% and the purity was 94.16%. The results showed that the yield and purity of squalene obtained by silver ion complexation extraction and column chromatography were higher than those obtained by other methods. The proposed method exhibited the advantages of simplicity, high selectivity and easy operation.