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  • Intermittent counter-current extraction--effect of the key operating parameters on selectivity and throughput.

Intermittent counter-current extraction--effect of the key operating parameters on selectivity and throughput.

Journal of chromatography. A (2011-05-17)
Peter Hewitson, Svetlana Ignatova, Ian Sutherland
ABSTRACT

Intermittent counter-current extraction (ICcE) has proved itself as a method for splitting compounds into streams and/or concentrating compounds in the column. In this paper a model mixture sample based on a modified GUESSmix (containing salicin, caffeine, aspirin, coumarin, salicylic acid, carvone, ionone and biphenyl) was separated into two eluant streams across a range of HEMWat phase system polarities from the polar system 11 through to non-polar system 23. ICcE could provide throughput of over 1 kg/day with this model sample, at the preparative scale, Changing the time cycle to adjust where the sample mixture is split into two streams was demonstrated. It is established that for the continuous running of ICcE, on a conventional twin bobbin counter-current chromatograph instrument, it is necessary to adjust the dead volumes of the flying leads to maintain similar phase retention in each column so the instrument does not become hydrodynamically and mechanically unbalanced due to the difference in densities between the upper and lower phases.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
L-Carvone, natural, 99%, FG
Sigma-Aldrich
L-Carvone, ≥97%, FCC, FG
Supelco
(+)-Carvone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
(S)-(+)-Carvone, 96%
Sigma-Aldrich
D-Carvone, ≥96%, FG
Sigma-Aldrich
(R)-(−)-Carvone, 98%
Supelco
(+)-Carvone, analytical standard
Supelco
(−)-Carvone, analytical standard
Sigma-Aldrich
D-(−)-Salicin, ≥99% (GC)