Chinese Journal of Chromatography ›› 2018, Vol. 36 ›› Issue (9): 858-865.DOI: 10.3724/SP.J.1123.2018.04018

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Separation of eicosapentaenoic acid ethyl ester and docosahexaenoic acid ethyl ester by simulated moving bed chromatography

DONG Qing, LI Min, YANG Yiwen, BAO Zongbi, YANG Qiwei, ZHANG Zhiguo, REN Qilong   

  1. Key Laboratory of Biomass Chemical Engineering of Ministry of Education, College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, China
  • Received:2018-04-17 Online:2018-09-08 Published:2014-08-05
  • Supported by:

    National Natural Science Foundation of China (No. 21776240); National Natural Science Foundation of China (No. 21436010); Program for Zhejiang Province Leading Team of S&T Innovation Key (No. 2011R50002).

Abstract:

Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are important ω -3 polyunsaturated fatty acids. Their physiological effects on humans are not exactly the same; therefore, the production of products with high-purity EPA or DHA monomers is significant. In this work, EPA ethyl ester (EPA-EE) and DHA ethyl ester (DHA-EE) were first separated using HPLC with poly(styrene-co-divinylbenzene) (PS/DVB) as the stationary phase. The effects of the mobile phase, PS/DVB particle diameter, and column temperature were systematically evaluated. The results showed that methanol is a suitable mobile phase, having a resolution of 2.75. By comparing resolutions, a PS/DVB particle diameter of 10 μ m was chosen; however, when the pressure drop of PS/DVB is considered, PS/DVB with a particle diameter of 20 μ m is more favorable for large-scale preparations. A column temperature of 40℃ was found to be the most feasible for maintaining efficient separation. Second, eight semi-preparative columns (150 mm×10 mm) of PS/DVB polymer were prepared for the simulated moving bed (SMB) chromatography; the homogeneity of these columns was perfect, with a relative total column porosity error of less than 1%. Finally, an EPA-EE and DHA-EE mixture was separated using the SMB chromatography, and the contents of the extract and the raffinate were determined using GC-FID. The effects of the flow rate of Zone Ⅱ and Zone Ⅲ, the flow rate of the feed, and the feed concentration were investigated. Under optimal conditions, EPA-EE and DHA-EE with favorable purities of 91.6% and 93.6%, respectively, were achievable. The recovery of the EPA-EE was 97.0% and the recovery of the DHA-EE was 91.6%. The productivity and solvent requirements were 5.97 g/(L\5h) and 1.52 L/g, respectively. Therefore, SMB chromatography is an attractive technology for the production of high-value products.

Key words: docosahexaenoic acid ethyl ester (DHA-EE), eicosapentaenoic acid ethyl ester (EPA-EE), liquid chromatography (LC), separation, simulated moving bed (SMB) chromatography

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