title: Multiple dual mode counter-current chromatography with variable duration of alternating phase elution steps.
abstract: The multiple dual mode (MDM) counter-current chromatography separation processes consist of a succession of two isocratic counter-current steps and are characterized by the shuttle (forward and back) transport of the sample in chromatographic columns. In this paper, the improved MDM method based on variable duration of alternating phase elution steps has been developed and validated. The MDM separation processes with variable duration of phase elution steps are analyzed. Basing on the cell model, analytical solutions are developed for impulse and non-impulse sample loading at the beginning of the column. Using the analytical solutions, a calculation program is presented to facilitate the simulation of MDM with variable duration of phase elution steps, which can be used to select optimal process conditions for the separation of a given feed mixture. Two options of the MDM separation are analyzed: 1 - with one-step solute elution: the separation is conducted so, that the sample is transferred forward and back with upper and lower phases inside the column until the desired separation of the components is reached, and then each individual component elutes entirely within one step; 2 - with multi-step solute elution, when the fractions of individual components are collected in over several steps. It is demonstrated that proper selection of the duration of individual cycles (phase flow times) can greatly increase the separation efficiency of CCC columns. Experiments were carried out using model mixtures of compounds from the GUESSmix with solvent systems hexane/ethyl acetate/methanol/water. The experimental results are compared to the predictions of the theory. A good agreement between theory and experiment has been demonstrated.
authors.affiliation: Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia. Electronic address: kost@igic.ras.ru.
authors.forename: Artak E
authors.initials: AE
authors.lastname: Kostanyan
authors.affiliation: Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia.
authors.forename: Andrey A
authors.initials: AA
authors.lastname: Erastov
authors.affiliation: Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia.
authors.forename: Oleg N
authors.initials: ON
authors.lastname: Shishilov
mesh_terms: D001241:Aspirin / Q000032:analysis; D002110:Caffeine / Q000032:analysis; D003374:Coumarins / Q000032:analysis; D003377:Countercurrent Distribution / Q000379:methods*; D008962:Models, Theoretical; D020156:Salicylic Acid / Q000032:analysis
chemical_list: D003374:Coumarins; D002110:Caffeine; C030123:coumarin; D020156:Salicylic Acid; D001241:Aspirin
keywords: Impulse and non-impulse sample loading; Multi-dimensional liquid chromatography; Multiple dual mode counter-current chromatography; One- and multi-step solute elution