大豆油脱臭馏分重相组分中甾醇酯的柱层析法分离提取Separation and extraction of sterol esters by column chromatography from the waste residue of soybean oil deodorizer distillate

为减少甾醇酯的生产工序，提高大豆油脱臭馏分重相组分中总甾醇得率，采用柱层析法直接分离提取甾醇酯，通过单因素试验考察吸附剂种类、上样量、洗脱剂比例和柱长直比（填料高度与直径比）对甾醇酯产品纯度和得率的影响，确定最佳工艺条件，并对最佳工艺条件下分离提取的甾醇酯产品进行傅里叶红外光谱表征，以及甾醇组成和脂肪酸组成测定。结果表明，柱层析法分离提取甾醇酯的最佳工艺条件为吸附剂为硅胶（粒径50~75 μm），上样量0.5 g，洗脱剂比例为正己烷、乙醚、冰乙酸体积比95∶ 5∶ 1，柱长直比16∶ 1。在最佳工艺条件下，甾醇酯产品纯度为(89.90±0.94)%，得率为(9615±1.49)%；傅里叶红外光谱分析证实提取的产品中含甾醇酯，甾醇酯上的甾醇组成主要为β-谷甾醇、豆甾醇、菜油甾醇，脂肪酸组成主要为亚油酸、油酸、棕榈酸、硬脂酸和亚麻酸。综上，柱层析法无需复杂工序，即可实现大豆油脱臭馏分重相组分中甾醇酯的有效回收。In order to reduce the process of sterol ester production and increase the yield of total sterols in the waste residue of soybean oil deodorizer distillate (WRSODD), column chromatography was used to extract the sterol esters from WRSODD. The influence of absorbent type, sample loading amount, eluent ratio and ratio of column material height to diameter on the recovery rate and purity of sterol esters were examined by single factor experiment, and the optimum process conditions were selected. The sterol esters obtained under the optimum process conditions was analyzed by Fourier-infrared spectroscopy, and its sterols and fatty acid compositions were analyzed. The results showed that the optimum conditions were as follows: with silica gel powder (particle size 50-75 μm) as absorbent, sample loading amount 0.5 g, volume ratio of a mixture of n-hexane, diethyl ether and glacial acetic acid 95∶ 5∶ 1, and ratio of column material height to diameter 16∶ 1. Under these conditions, the purity and recovery rate of sterol esters were (89.90±0.94)% and (96.15±1.49)%, respectively. Fourier-infrared spectroscopy results verified that the product contained sterol esters. The sterol compositions of sterol esters were mainly β-sitosterol, stigmasterol and campesterol. The fatty acid compositions were palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. In conclusion, effective recovery of sterol esters from the waste residue of soybean oil deodorizer distillate can be achieved through column chromatography without complex process.