Off-line coupling of new generation centrifugal partition chromatography device with preparative high pressure liquid chromatography-mass spectrometry triggering fraction collection applied to the recovery of secoiridoid glycosides from Centaurium erythraea Rafn. (Gentianaceae).

Autor: Mandova T; Laboratory of Pharmacognosy, UMR CNRS 8638, Faculty of Pharmacy, Paris Descartes University, Sorbonne Paris Cité, 4 avenue de l'Observatoire, 75006 Paris, France; Gilson Purification SAS, 22 rue Bourseul, ZA du Poteau, 56890 Saint-Avé, France., Audo G; Gilson Purification SAS, 22 rue Bourseul, ZA du Poteau, 56890 Saint-Avé, France., Michel S; Laboratory of Pharmacognosy, UMR CNRS 8638, Faculty of Pharmacy, Paris Descartes University, Sorbonne Paris Cité, 4 avenue de l'Observatoire, 75006 Paris, France., Grougnet R; Laboratory of Pharmacognosy, UMR CNRS 8638, Faculty of Pharmacy, Paris Descartes University, Sorbonne Paris Cité, 4 avenue de l'Observatoire, 75006 Paris, France. Electronic address: raphael.grougnet@parisdescartes.fr.
Jazyk: angličtina
Zdroj: Journal of chromatography. A [J Chromatogr A] 2017 Sep 01; Vol. 1513, pp. 149-156. Date of Electronic Publication: 2017 Jul 08.
DOI: 10.1016/j.chroma.2017.07.023
Abstrakt: A purification sequence including a Gilson CPC 250 PRO device coupled to PrepHPLC hyphenated with a MS triggering fraction collector was applied to isolate secoiridoid glycosides from a complex methanolic extract of Centaurium erythraea. This species is widely used for ethnomedicinal purposes around the Mediterranean Sea. The solvent system ethyle acetate/ethanol/water 7.5/3/5 was determined using shake-flask method targeting swertiamarin, the major secoiridoid of the extract. Optimization of CPC experimental parameters enabled the injection of 4g of extract with a flow rate of 40mL/min at 3000rpm to provide a secoiridoid glycosides enriched fraction. 130mg of this latter was submitted to a second step of purification by preparative HPLC (gradient water/formic acid (19:1) (A) and methanol (B) as follows: 0min, 85% A; 8min, 60% A; 12min, 55% A; 35min, 55% A; 40min, 10% A; 50min, 10% A; 52min, 85% A; 55min, 85% A) to give swertiamarin (36mg, yield 27.7%, purity 98.2%). Other secoiridoid glycosides (sweroside, gentiopicroside, secologanol, secoxyloganin) were also isolated in minor amounts. As these monoterpene derivatives are responsible for several biological activities, their quick recovery with high yield and purity may serve as a model for further scale-up and industrial development.
(Copyright © 2017 Elsevier B.V. All rights reserved.)
Databáze: MEDLINE
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