title: Rapid collection and identification of a novel component from Clausena lansium Skeels leaves by means of three-dimensional preparative gas chromatography and nuclear magnetic resonance/infrared/mass spectrometric analysis.
abstract: The present research reports the use of a three-dimensional preparative gas chromatography (prep GC) system, equipped with three Deans-switch devices and 5%diphenyl/wax/mid-polarity ionic liquid stationary phases, for the isolation of volatile components from a complex natural source, namely wampee essential oil (derived from Clausena lansium Skeels leaves). Collection was performed by using a simple and effective lab-constructed trapping device. Initially, an unknown (and abundant) wampee oil constituent was erroneously identified as α-sinensal, through an MS database search (a low similarity match was attained), performed after a GC-quadMS experiment., The unknown compound was then the isolated by using the novel prep GC system, in a highly pure form (at the mg level), and was correctly identified by using nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FTIR) and mass spectrometry (MS). Both FTIR and MS data were used to confirm the NMR information. The name given to the molecule was (2E,6E)-2-methyl-6-(4-methylcyclohex-3-enylidene)hept-2-enal. The results herein described will demonstrate the need for a high-resolution GC step, prior to analyte collection, in the prep GC analysis of complex samples.
authors.affiliation: Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Messina, Italy.
authors.forename: Danilo
authors.initials: D
authors.lastname: Sciarrone
authors.forename: Sebastiano
authors.initials: S
authors.lastname: Pantò
authors.forename: Archimede
authors.initials: A
authors.lastname: Rotondo
authors.forename: Laura
authors.initials: L
authors.lastname: Tedone
authors.forename: Peter Quinto
authors.initials: PQ
authors.lastname: Tranchida
authors.forename: Paola
authors.initials: P
authors.lastname: Dugo
authors.forename: Luigi
authors.initials: L
authors.lastname: Mondello
mesh_terms: D000447:Aldehydes / Q000032:analysis* / Q000302:isolation & purification; D002849:Chromatography, Gas; D054700:Clausena / Q000737:chemistry*; D053138:Cyclohexenes / Q000032:analysis* / Q000302:isolation & purification; D008401:Gas Chromatography-Mass Spectrometry; D009682:Magnetic Resonance Spectroscopy; D009822:Oils, Volatile / Q000737:chemistry* / Q000302:isolation & purification; D018515:Plant Leaves / Q000737:chemistry; D017550:Spectroscopy, Fourier Transform Infrared
chemical_list: C585680:(2E,6E)-2-methyl-6-(4-methylcyclohex-3-enylidene)hept-2-enal; D000447:Aldehydes; D053138:Cyclohexenes; D009822:Oils, Volatile