Rapid isolation and characterization of crocins, picrocrocin, and crocetin from saffron using centrifugal partition chromatography and LC-MS.

Journal of Separation Science
Evangelia KarkoulaAlexios-Leandros Skaltsounis

Abstract

This study demonstrates a simple method for one-step isolation of the main secondary metabolites of a hydroalcoholic extract of Crocus sativus stigmas (saffron) using step-gradient centrifugal partition chromatography. The analysis was performed in dual and elution-extrusion mode, using five biphasic systems of the solvents heptane/ethyl acetate/butanol/ethanol/water in ratios of 4:10:0:4:10, 1:13:0:4:10, 1:12:1:4:10, 1:10:3:4:10, and 1:7:6:4:10. Five major crocins, picrocrocin, and crocetin were directly isolated in one step. Scaling up to preparative level, allowed the recovery of significantly high quantities of pure compounds, especially trans-crocin-4, saffron's principal crocin. Comparing dual-mode and elution-extrusion, in dual-mode, the trans-crocin-4 containing fractions were co-eluted with a high amount of free β-d-glucose. In contrast, absence of free β-d-glucose was observed in the corresponding trans-crocin-4 fractions obtained by the second method denoting its superiority against dual-mode. Initiating analysis with the 4th solvent-system afforded selective isolation of trans-crocin-4, with reduction in experimental time and solvent consumption. Structure elucidation was performed by nuclear magnetic resonance spec...Continue Reading

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Citations

Dec 4, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Nikolaos Pitsikas, Petros A Tarantilis
Jan 28, 2021·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Nikolaos Pitsikas, Petros A Tarantilis
Jan 31, 2021·Metabolites·Georgios TheodoridisOn Behalf Of The FoodOmicsGR Ri Consortium

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