Separation of phenolic compounds by centrifugal partition chromatography


Phenolic compounds are ubiquitous biomolecules exhibiting a wide range of physiological properties, with application in the pharmaceutical and nutraceutical fields. In this work, aqueous biphasic systems (ABS) formed by polyethylene glycol and sodium polyacrylate, and inorganic salts or ionic liquids as electrolytes, were applied for the purification of caffeic, ferulic and protocatechuic acids (CA, FA, and PA, respectively), vanillin (VN) and syringaldehyde (SA), followed by the use of centrifugal partition chromatography (CPC) to reinforce the fractionation process scale-up. In single-step experiments in ABS, high selectivities and adequate partition coefficients (K-CA = 2.78 +/- 0.20; K-PA = 0.44 +/- 0.04; K-FA = 0.23 +/- 0.01; K-VN = 1.12 +/- 0.05 and K-SA = 1.23 +/- 0.02) were achieved using ABS formed by sodium chloride as the electrolyte. This system was further applied in CPC, allowing an efficient separation of the five phenolic compounds after the optimization of the equipment operational conditions, while demonstrating the potential of polymer-based ABS to be used in liquid-liquid chromatography. Finally, the recovery of the phenolic compounds (between 65 and 87%) with high purity from the ABS phases was demonstrated, allowing the reuse of the ABS phase-forming components, which was proved to be of low environmental impact. In fact, in a scenario where the polymeric phases are reused, the carbon footprint is decreased to 36%, as the consumption of new chemicals and water reduces considerably.




Chemistry; Science & Technology - Other Topics


Santos, JHPM; Almeida, MR; Martins, CIR; Dias, ACRV; Freire, MG; Coutinho, JAP; Ventura, SPM

nossos autores


This work was developed within the scope of the project CICECO-Aveiro Institute of Materials, POCI-01-0145-FEDER-007679 (FCT Ref. UID/CTM/50011/2013), financed by national funds through the FCT/MEC and when appropriate co-financed by FEDER under the PT2020 Partnership Agreement. The authors are grateful for the financial support of the Portuguese Foundation for Science and Technology (FCT) for the doctoral grant of SFRH/BD/102915/2014 of J. H. P. M. Santos. S. P. M. Ventura acknowledges for contract IF/00402/2015. M. G. F. acknowledges the European Research Council (ERC) for the grant ERC-2013-StG-337753. The authors acknowledge the FCT funding through the project "Multipurpose strategies for broadband agro-forest and fisheries by-products valorisation: a step forward for a truly integrated biorefinery (PAC - Programa de atividades Conjuntas) ref: SAICTPAC/0040/2015. A. C. R. V. Dias acknowledges FCT/MCTES for a contract under Investigador FCT 2013 contract number IF/00587/2013, and for the financial support to CESAM (UID/AMB/50017), through national funds, and the co-funding by FEDER, within the PT2020 Partnership Agreement and Compete 2020.

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