LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano

Exarchou, V.; Godejohann, M.; van Beek, T. A.; Gerothanassis, I. P.; Vervoort, J.

LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano

dc.contributor.author	Exarchou, V.	en
dc.contributor.author	Godejohann, M.	en
dc.contributor.author	van Beek, T. A.	en
dc.contributor.author	Gerothanassis, I. P.	en
dc.contributor.author	Vervoort, J.	en
dc.date.accessioned	2015-11-24T16:40:59Z
dc.date.available	2015-11-24T16:40:59Z
dc.identifier.issn	0003-2700	-
dc.identifier.uri	https://olympias.lib.uoi.gr/jspui/handle/123456789/8345
dc.rights	Default Licence	-
dc.subject	magnetic-resonance-spectroscopy	en
dc.subject	performance liquid-chromatography	en
dc.subject	high-resolution nmr	en
dc.subject	tandem mass-spectrometry	en
dc.subject	to-noise ratio	en
dc.subject	hplc-nmr	en
dc.subject	solvent-suppression	en
dc.subject	natural-products	en
dc.subject	plant-extracts	en
dc.subject	constituents	en
dc.title	LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano	en
heal.abstract	Structure elucidation of natural products usually relies on a combination of NMR spectroscopy with mass spectrometry whereby NMR trails MS in terms of the minimum sample amount required. In the present study, the usefulness of on-line solid-phase extraction (SPE) in LC-NMR for peak storage after the LC separation prior to NMR analysis is demonstrated. The SPE unit allows the use of normal protonated solvents for the LC separation and fully deuterated solvents for flushing the trapped compounds to the NAIR probe. Thus, solvent suppression is no longer necessary. Multiple trapping of the same analyte from repeated LC injections was utilized to solve the problem of low concentration and to obtain 2D heteronuclear NMR spectra. In addition, a combination of the SPE unit with a recently developed cryoflow NMR probe and an MS was evaluated. This on-line LC-UV-SPE-NMR-MS system was used for the automated analysis of a Greek oregano extract. Combining the data provided by the UV, MS, and NMR spectra, the flavonoids taxifolin, aromadendrin, eriodictyol, naringenin, and apigenin, the phenolic acid rosmarinic acid, and the monoterpene carvacrol were identified. This automated technique is very useful for natural product analysis, and the large sensitivity improvement leads to significantly reduced NAIR acquisition times.	en
heal.access	campus	-
heal.fullTextAvailability	TRUE	-
heal.identifier.primary	Doi 10.1021/Ac0347819	-
heal.identifier.secondary	<Go to ISI>://000186601500036	-
heal.identifier.secondary	http://pubs.acs.org/doi/pdfplus/10.1021/ac0347819	-
heal.journalName	Anal Chem	en
heal.journalType	peer reviewed	-
heal.language	en	-
heal.publicationDate	2003	-
heal.publisher	American Chemical Society	en
heal.recordProvider	Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας	el
heal.type	journalArticle	-
heal.type.el	Άρθρο Περιοδικού	el
heal.type.en	Journal article	en

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