陆燕婷.硅胶柱层析精制中长链结构甘油三酯[J].中国油脂,2021,46(12):104~107.[LU Yanting.Purification of medium and long chain triacylglycerols by silica gel column chromatography[J].China Oils and Fats,2021,46(12):104~107.] |
硅胶柱层析精制中长链结构甘油三酯 |
Purification of medium and long chain triacylglycerols by silica gel column chromatography |
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DOI: |
中文关键词: 中长链结构甘油三酯 硅胶柱层析 甘二酯 精制 |
英文关键词:medium and long chain triacylglycerols silica gel column chromatography diacylglycerides purification |
基金项目:江苏省科技计划项目(BE2018376); 高等学校学科创新引智计划(111计划)项目(B90719028) |
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中文摘要: |
为探究硅胶柱层析在中长链结构甘油三酯(MLCT)精制方面的应用,以亚麻籽油和中链脂肪酸甘油三酯为原料合成MLCT粗产品,采用硅胶柱层析进行精制,优化精制工艺条件并对硅胶柱层析精制前后MLCT的质量指标进行了测定。通过硅胶薄层层析确定硅胶柱层析的洗脱剂,通过洗脱曲线确定洗脱液收集体积,以甘二酯脱除率和产品回收率为评价指标,确定洗脱流速和上样量。结果表明:以正己烷-无水乙醚(体积比5∶ 1)为洗脱剂,等梯度洗脱,洗脱流速2.0 mL/min,上样量4 g,硅胶40 g,收集洗脱液500 mL条件下对MLCT粗产品进行精制,所得产品甘二酯脱除率达到99.40%,MLCT回收率为95.07%。精制后产品酸值(KOH)和过氧化值显著降低,分别为0.04 mg/g和0.00 g/100 g,色泽变浅,色值为R0.0,Y0.1。硅胶柱层析具有同时脱除副产物,降低酸值、过氧化值、脱色等综合效果,在MLCT精制方面有良好的应用前景。 |
英文摘要: |
To explore the application of silica gel column chromatography(SGCC) in the purification of medium and long chain triacylglycerols(MLCT), crude MLCT was prepared with flaxseed oil and medium chain triacylglyceride as materials, and then was purified with SGCC. The purification process was optimized, and the quality indexes of MLCT before and after purification were determined. The eluent was determined by silica gel thin layer chromatography and elution curve was used to determine the collection volume of elute, and the flow rate and sample loading were determined by investigating the removal rate of diacylglycerides and product recovery rate as indexes. The results showed that the optimal purification conditions were obtained as follows: binary solvent system(n-hexane-anhydrous ether (volume ratio 5∶ 1)), equal gradient elution, flow rate 2.0 mL/min, sample loading 4 g, silica dosage 40 g, collection volume of elute 500 mL. Under the optimal conditions, the removal rate of the diacylglycerols reached 99.40% and the recovery rate of MLCT was 95.07%. After purification, the acid value and peroxide value of the product decreased significantly, which were 0.04 mgKOH/g and 0.00 g/100 g, respectively. The color of the product became lighter, and the color value was R0.0, Y0.1. Silica gel column chromatography could achieve the comprehensive effect of removing by-products, reducing acid value, peroxide value and bleaching, which had a good application prospect in the purification of MLCT. |
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