中性氧化铝柱层析分离纯化鲨肝醇制品及其组成分析  

Separation and Purification of Batyl Alcohol Products by Neutral Aluminum Oxide Column Chromatography and Analysis of Its Composition

作　　者：宋恭帅 戴志远 沈清 崔益玮 朱蓓薇[3] 王加斌 郑平安 Song Gongshuai;Dai Zhiyuan;Shen Qing;Cui Yiwei;Zhu Beiwei;Wang Jiabin;Zheng Pingan(Institute of Seafood,Zhejiang Gongshang University,Hangzhou 310012;State Key Laboratory of Aquatic Products Processing of Zhejiang Province,Hangzhou 310012;School of Food Science and Technology,Dalian Polytechnic University,Dalian 116034,Liaoning;Hailisheng Group Co.Ltd.,Zhoushan 316021,Zhejiang)

机构地区：[1]浙江工商大学海洋食品研究院,杭州310012 [2]浙江省水产品加工技术研究联合重点实验室,杭州310012 [3]大连工业大学食品学院,辽宁大连116034 [4]海力生集团有限公司,浙江舟山316021

出　　处：《中国食品学报》2021年第5期221-229,共9页Journal of Chinese Institute Of Food Science and Technology

基　　金：国家重点研发计划项目(2018YFC0311204)。

摘　　要：为分离纯化鲨肝醇制品,以鲨鱼肝油中不皂化物为原料,以鲨肝醇纯度为评价指标,通过响应面法优化中性氧化铝柱层析富集鲨肝醇制品的工艺参数,采用薄层层析法(TLC)与气相色谱(GC)对其纯度及组成进行定性与定量分析。结果表明:最优工艺条件是:洗脱液比例(V_(二氯甲烷)∶V_(无水甲醇))为9∶1,上样量3 g,色谱柱负载量0.012 g/g氧化铝,洗脱流速为2 mL/min,所得鲨肝醇制品纯度达18.23%,得率为38.70%。经TLC与GC综合分析可知,鲨肝醇制品中主要含有鲨肝醇与角鲨烯两大类活性物质。中性氧化铝柱层析富集鲨肝醇的同时,会造成不皂化物中角鲨烯的损失。根据角鲨烯标准曲线计算,角鲨烯纯度由54.21%减至49.18%。通过精密度与回收率试验证明GC具有良好的稳定性与精密度。本研究结果为高纯度鲨肝醇制品的工业化制备提供一定的理论基础。In order to separate and purify the batyl alcohol products,the unsaponifiable matter in shark liver oil was used as the raw material,and the purity of batyl alcohol was used as the evaluation index,and the process parameters of the batyl alcohol product were optimized by the response surface method to optimize the neutral alumina column chromatography.The purity and composition were qualitatively and quantitatively analyzed by thin layer chromatography(TLC)and gas chromatography(GC).The results showed that the optimum conditions were as follows:the volume ratio of eluent(dichloromethane:anhydrous methanol)was 9∶1,the loading amount was 3 g,the column loading was 0.012 g/g alumina,and the elution flow rate was 2 mL/min,the obtained batyl alcohol product purity was 18.23%,and the yield was 38.70%.According to the comprehensive analysis of TLC and GC,the batyl alcohol product mainly contains two kinds of active substances,batyl alcohol and squalene.Neutral alumina column chromatography enriches batyl alcohol and causes loss of squalene content in unsaponifiable matter.According to the standard curve of squalene,the purity of squalene was reduced from 54.21%to 49.18%.Finally,the precision and precision of the GC proved that the GC has good stability and precision.This study provides a theoretical basis for the industrial preparation of high-purity batyl alcohol products.

关 键 词：鲨肝醇制品 中性氧化铝柱层析 角鲨烯 薄层层析法 气相色谱法 

分 类 号：TS225.24[轻工技术与工程—粮食、油脂及植物蛋白工程]