title: Improving the productivity of a multidimensional chromatographic preparative system by collecting pure chemicals after each of three chromatographic dimensions.
abstract: The enhanced sample collection capability of a heart-cutting three-dimensional GC-prep system is reported. In its original configuration, a highly pure component can be usually collected after the last (3D) column outlet by means of a dedicated preparative station. The latter is located after the last chromatographic column, and this poses the requirement for multiple heart cuts even for those components showing satisfactory degree of purity after the first (or second) separation dimension. The feasibility to collect pure components after each chromatographic dimension is here described, employing a three-dimension MDGC system equipped with high-temperature valves, located inside the first and second GC ovens, with the aim to improve the productivity of the collection procedure. In addition to a commercial preparative collector located at the 3D outlet, two laboratory-made collection systems were applied in the first and second dimension, reached by the effluent to be collected trough a high-temperature valve switching the heart-cut fraction between either the detector (FID), or the collector. Highly pure sesquiterpene components were collected, namely: patchouli alcohol after the first column [poly(5% diphenyl/95% dimethylsiloxane)], α-bulnesene after a second column coated with high molecular weight polyethylene glycol, and α-guaiene after an ionic-liquid based column (SLB-IL60), used as the third dimension. Purity levels ranging from 85 to 95% were achieved with an average collection recovery of 90% (n=5). The following average amounts were collected per run: 160μg for α-guaiene, 295μg for α-bulnesene, and 496μg for patchouli alcohol.
authors.affiliation: Dipartimento di "Scienze Chimiche, Biologiche, Farmaceutiche ed Ambientali", University of Messina, Polo Annunziata-viale Annunziata, 98168, Messina, Italy.
authors.forename: Danilo
authors.initials: D
authors.lastname: Sciarrone
authors.affiliation: Chromaleont s.r.l., c/o University of Messina, Polo Annunziata-viale Annunziata, 98168, Messina, Italy.
authors.forename: Sebastiano
authors.initials: S
authors.lastname: Pantò
authors.affiliation: Dipartimento di "Scienze Biomediche, Odontoiatriche e delle Immagini Morfologiche e Funzionali", University of Messina, via Consolare Valeria, 98125, Messina, Italy.
authors.forename: Paola
authors.initials: P
authors.lastname: Donato
authors.affiliation: Dipartimento di "Scienze Chimiche, Biologiche, Farmaceutiche ed Ambientali", University of Messina, Polo Annunziata-viale Annunziata, 98168, Messina, Italy; Chromaleont s.r.l., c/o University of Messina, Polo Annunziata-viale Annunziata, 98168, Messina, Italy; University Campus Bio-Medico of Rome, Via Álvaro del Portillo 21, 00128 Rome, Italy. Electronic address: lmondello@unime.it.
authors.forename: Luigi
authors.initials: L
authors.lastname: Mondello
mesh_terms: D052176:Azulenes / Q000302:isolation & purification; D002849:Chromatography, Gas / Q000379:methods*; D004129:Dimethylpolysiloxanes; D011092:Polyethylene Glycols; D012717:Sesquiterpenes / Q000302:isolation & purification*; D045789:Sesquiterpenes, Guaiane / Q000302:isolation & purification
chemical_list: D052176:Azulenes; D004129:Dimethylpolysiloxanes; D012717:Sesquiterpenes; D045789:Sesquiterpenes, Guaiane; C512113:alpha-bulnesene; D011092:Polyethylene Glycols; C019408:guaiene; C052983:patchouli alcohol
keywords: Heart-cutting; Patchouli essential oil; Preparative GC; Three-dimensional configuration