275785 Pilot Scale Chromatographic Separation of Poly Unsaturated Ethyl Esters Using Liquefied Gases and Supercritical Fluids

Wednesday, October 31, 2012: 4:45 PM
Washington (Westin )
Steve J. Tallon, Fernando Montanes, Kevin Mitchell and Paul Rose, Industrial Research Ltd, Lower Hutt, New Zealand

This paper describes the scale-up, development and commissioning of a pilot scale preparative chromatography plant suitable for use with liquefied gases and supercritical fluids as the mobile phase, including the use of flammable gases. The pilot plant has 2 by 10L columns capable of operation up to 350 bar pressure and 85°C temperature. The columns can be operated in series or independently, and in single or semi-continuous automated operation. A UV-Vis detection system is used, and up to 4 fractions can be separately recovered. A co-solvent gradient can also be applied.

A laboratory scale process for separation of the polyunsaturated fatty acids EPA and DHA from mixtures of ethyl esters derived from fish and algal sources has been developed, and a comparison of results between laboratory and pilot scale is given. Very good separation, exceeding 90% concentration of EPA and DHA, and very good recovery was able to be achieved in a single pass operation using CO2 as the mobile phase and a silica column. Conditions were optimised over the range 150 to 250 bar pressure, temperatures from 40 to 60°C, and using a range of ethyl ester and CO2 flow rates. Results were able to be reproduced on the pilot scale using loadings between 10g and 100g of ethyl esters.

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