大豆油脱臭馏出物中同时提取角鲨烯、生育酚和植物甾醇的工艺研究

Study on simultaneously extracting squalene,tocopherols and phytosterols from soybean oil deodorizer distillate

采用酯化—高真空蒸馏工艺路线,从大豆油脱臭馏出物中同时提取角鲨烯、生育酚及植物甾醇。考察酯化条件(甲醇、催化剂浓硫酸用量及反应时间)对酯化率、角鲨烯和生育酚含量的影响。优化得到的最佳工艺为:催化剂浓硫酸添加量0.5%,醇油摩尔比10∶1,反应温度70℃,反应时间120 min,大豆油脱臭馏出物酯化率达到98.2%,生育酚和角鲨烯保留率分别为97.7%和97.5%。酯化后的物料通过冷析结晶,抽滤得到植物甾醇粗品,滤液高真空蒸馏,初步分离得到脂肪酸甲酯、角鲨烯、生育酚等组分。各组分中角鲨烯富集到12.2%,生育酚富集到28.6%,植物甾醇富集到60%左右,初步实现了大豆油脱臭馏出物中角鲨烯、生育酚、植物甾醇的同时提取,为角鲨烯、生育酚及植物甾醇的进一步富集提供了参考依据。

Squalene,tocopherols and phytosterols were simultaneously extracted from soybean oil deodorizer distillate（SODD） by esterification-high vacuum distillation. The effects of esterification conditions（the amounts of methanol,catalyst concentrated sulfuric acid,and reaction time） on esterification rate,the content of squalene and tocopherols were investigated. The optimum esterification conditions were as follows： concentrated sulfuric acid 0. 5%,molar ration of methanol to oil 10 ∶ 1,temperature70 ℃ and time 120 min,the esterification rate of SODD could reach 98. 2%,tocopherol and squalene retention rates were 97. 7% and 97. 5% respectively. The esterification solution was crystallized and filtered to obtain crude phytosterols. The filtrate was further treated by high vacuum distillation to extract fatty acid methyl ester,squalene and tocopherol. The squalene,tocopherols and phytosterols were enriched to 12. 2%,28. 6% and about 60% respectively. The proposed method could be used for simultaneous extraction of crude phytosterols,tocopherols,and squalene from SODD,which provided reference for the further purification and enrichment of squalene,tocopherols and phytosterols.