鱼油中二十碳五烯酸乙酯和二十二碳六烯酸乙酯的超临界流体色谱分离技术
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82 2012, Vol.33, No.24
食品科学
※工艺技术
鱼油中二十碳五烯酸乙酯和二十二碳六烯酸 乙酯的超临界流体色谱分离技术
陈伟珠1,2，洪 专1,*，赵 敏1，张怡评1，谢全灵1，易瑞灶1
(1.国家海洋局第三海洋研究所，福建 厦门 361005； 2. 厦门大学化学化工学院化学系，化学生物学福建省重点实验室，福建 厦门 361005)
Keywords：supercritical fluid chromatography (SFC)；eicosapentaenoic acid ethyl ester (EPA-EE)； docosahexae (DHA-EE)；separation
中图分类号：O657.74
rate of 2 mL/min. Under these conditions, baseline separation of EPA-EE and DHA-EE was achieved. The developed method was
simple, rapid, highly reproducible and suitable for the separation of EPA-EE and DHA-EE from fish oil.
摘 要：建立鱼油中二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)的超临界流体色谱纯化方法。比 较Luna 5u Silica、Hedera ODS-BP、Hypersil ODS2、ZORBAX SB-C8和Hypersil C8等色谱柱对EPA-EE和DHA-EE的 分离效果，确定以Hedera ODS-BP作为优选色谱柱，进一步以容量因子、选择性和分离度为考核指标，考察改性 剂、流动相比例、背压及温度对分离效果的影响。得到的优化分离条件为：以Hedera ODS-BP为色谱柱，10%甲醇 为改性剂，总流速2mL/min、柱温40℃、背压100bar。在此条件下，鱼油中EPA-EE和DHA-EE可以达到基线分离。 结论：本法简便、快速、重现性好，可用于鱼油中EPA-EE和DHA-EE的分离。 关键词： 超临界流体色谱(SFC)；二十碳五烯酸乙酯(EPA-EE)；二十二碳六烯酸乙酯(DHA-EE)；分离
were investigated. The optimum conditions forthese factors were found to be separation on Hedera ODS-BP column at a column temperature of 40 ℃ an a back pressure of 100 bar using a mobile phase containing 10% methanol as a modifier at a total flow
Xiamen University, Xiamen 361005, China)
Abstract：A supercritical fluid chromatographic method to separate eicosapentaenoic acid ethyl ester (EPA-EE) and
Supercritical Fluid Chromatographic Separation of Eicosapentaenoic Acid Ethyl Ester and Docosahexaenoic Acid Ethyl Ester from Fish Oil
CHEN Wei-zhu1,2，HONG Zhuan 1,*，ZHAO Min1，ZHANG Yi-ping1，XIE Quan-ling 1，YI Rui-zao 1
docosahexaenoic acid ethyl ester (DHA-EE) from fish oil was established. Hedera ODS-BP was found to be the most effective
column for separating EPA-EE and DHA-EE from fish oil as demonstrated by a comparison with Luna 5u Silica, Hypersil ODS2,
(1. The Third Institute of Oceanography of the State Oceanic Administration, Xiamen 361005, China； 2. Key Laboratory for Chemical Biology of Fujian Province, Department of Chemistry, College of Chemistry and Chemical Engineering,
ZORBAX SB-C8, and Hypersil C8. The effects of mobile phase modifier type, methanol percentage in mobile phase, back pressure and column temperature for the separation of both esters by Hedera ODS-BP on capacity factor, diastereoselectivity and resolution
文献标识码：A
文章编号：1002-6630(2012)24-0082-04
二十碳五烯酸(EPA) 、二十二碳六烯酸(DHA)均为 人体必需的ω-3型多烯不饱和脂肪酸，近年来大量实验 和临床研究表明，DHA具有健脑作用，EPA具有降血 脂、抗血小板聚集、延缓血栓形成的作用 。 [1-2] 在鱼体
处理[3]，将EPA和DHA甘油酯分别转化为二十碳五烯酸 乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)，再进 行精制纯化。目前对于EPA-EE和DHA-EE纯化技术研 究的报道主要有机溶剂萃取、尿素络合、超临界萃取以
食品科学
※工艺技术
鱼油中二十碳五烯酸乙酯和二十二碳六烯酸 乙酯的超临界流体色谱分离技术
陈伟珠1,2，洪 专1,*，赵 敏1，张怡评1，谢全灵1，易瑞灶1
(1.国家海洋局第三海洋研究所，福建 厦门 361005； 2. 厦门大学化学化工学院化学系，化学生物学福建省重点实验室，福建 厦门 361005)
Keywords：supercritical fluid chromatography (SFC)；eicosapentaenoic acid ethyl ester (EPA-EE)； docosahexae (DHA-EE)；separation
中图分类号：O657.74
rate of 2 mL/min. Under these conditions, baseline separation of EPA-EE and DHA-EE was achieved. The developed method was
simple, rapid, highly reproducible and suitable for the separation of EPA-EE and DHA-EE from fish oil.
摘 要：建立鱼油中二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)的超临界流体色谱纯化方法。比 较Luna 5u Silica、Hedera ODS-BP、Hypersil ODS2、ZORBAX SB-C8和Hypersil C8等色谱柱对EPA-EE和DHA-EE的 分离效果，确定以Hedera ODS-BP作为优选色谱柱，进一步以容量因子、选择性和分离度为考核指标，考察改性 剂、流动相比例、背压及温度对分离效果的影响。得到的优化分离条件为：以Hedera ODS-BP为色谱柱，10%甲醇 为改性剂，总流速2mL/min、柱温40℃、背压100bar。在此条件下，鱼油中EPA-EE和DHA-EE可以达到基线分离。 结论：本法简便、快速、重现性好，可用于鱼油中EPA-EE和DHA-EE的分离。 关键词： 超临界流体色谱(SFC)；二十碳五烯酸乙酯(EPA-EE)；二十二碳六烯酸乙酯(DHA-EE)；分离
were investigated. The optimum conditions forthese factors were found to be separation on Hedera ODS-BP column at a column temperature of 40 ℃ an a back pressure of 100 bar using a mobile phase containing 10% methanol as a modifier at a total flow
Xiamen University, Xiamen 361005, China)
Abstract：A supercritical fluid chromatographic method to separate eicosapentaenoic acid ethyl ester (EPA-EE) and
Supercritical Fluid Chromatographic Separation of Eicosapentaenoic Acid Ethyl Ester and Docosahexaenoic Acid Ethyl Ester from Fish Oil
CHEN Wei-zhu1,2，HONG Zhuan 1,*，ZHAO Min1，ZHANG Yi-ping1，XIE Quan-ling 1，YI Rui-zao 1
docosahexaenoic acid ethyl ester (DHA-EE) from fish oil was established. Hedera ODS-BP was found to be the most effective
column for separating EPA-EE and DHA-EE from fish oil as demonstrated by a comparison with Luna 5u Silica, Hypersil ODS2,
(1. The Third Institute of Oceanography of the State Oceanic Administration, Xiamen 361005, China； 2. Key Laboratory for Chemical Biology of Fujian Province, Department of Chemistry, College of Chemistry and Chemical Engineering,
ZORBAX SB-C8, and Hypersil C8. The effects of mobile phase modifier type, methanol percentage in mobile phase, back pressure and column temperature for the separation of both esters by Hedera ODS-BP on capacity factor, diastereoselectivity and resolution
文献标识码：A
文章编号：1002-6630(2012)24-0082-04
二十碳五烯酸(EPA) 、二十二碳六烯酸(DHA)均为 人体必需的ω-3型多烯不饱和脂肪酸，近年来大量实验 和临床研究表明，DHA具有健脑作用，EPA具有降血 脂、抗血小板聚集、延缓血栓形成的作用 。 [1-2] 在鱼体
处理[3]，将EPA和DHA甘油酯分别转化为二十碳五烯酸 乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)，再进 行精制纯化。目前对于EPA-EE和DHA-EE纯化技术研 究的报道主要有机溶剂萃取、尿素络合、超临界萃取以