title: Development of an improved online comprehensive hydrophilic interaction chromatography × reversed-phase ultra-high-pressure liquid chromatography platform for complex multiclass polyphenolic sample analysis.
abstract: In this study, an improved online comprehensive two-dimensional liquid chromatography platform coupled to tandem mass spectrometry was developed for the analysis of complex polyphenolic samples. A narrowbore hydrophilic interaction chromatography column (150 × 2.0 mm, 3.0 μm, cross-linked diol) was employed in the first dimension, while a reversed-phase column based on monodisperse sub-2 μm fully porous particles (50 × 3.0 mm, 1.9 μm d.p.) with high surface area (410 m2/g) was employed in the second dimension. The combination of a trapping column modulation interface with the high retentive fully porous monodisperse reversed-phase column in the second dimension resulted in higher peak capacity values (1146 versus 867), increased sensitivity, sharper and more symmetrical peaks in comparison with a conventional loop-based method, with the same analysis time (70 min). The system was challenged against a complex polyphenolic extract of a typical Italian apple cultivar, enabling the simultaneous separation of multiple polyphenolic classes, including oligomeric procyanidins, up to degree of polymerization of 10. Hyphenation with an ion trap time-of-flight mass spectrometer led to the tentative identification of 121 analytes, showing how this platform could be a powerful analytical tool for the accurate profiling of complex polyphenolic samples.
authors.affiliation: Laboratory of Food Chemistry, Dipartimento di Agraria (QuaSic. A. Tec.), Università Mediterranea di Reggio Calabria, Reggio Calabria, Italy.|Department of Pharmacy, University of Salerno, Salerno, Italy.
authors.forename: Eduardo
authors.initials: E
authors.lastname: Sommella
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, Roma, Italy.
authors.forename: Omar H
authors.initials: OH
authors.lastname: Ismail
authors.affiliation: Laboratory of Food Chemistry, Dipartimento di Agraria (QuaSic. A. Tec.), Università Mediterranea di Reggio Calabria, Reggio Calabria, Italy.|Department of Pharmacy, University of Salerno, Salerno, Italy.
authors.forename: Francesco
authors.initials: F
authors.lastname: Pagano
authors.affiliation: Laboratory of Food Chemistry, Dipartimento di Agraria (QuaSic. A. Tec.), Università Mediterranea di Reggio Calabria, Reggio Calabria, Italy.|Department of Pharmacy, University of Salerno, Salerno, Italy.
authors.forename: Giacomo
authors.initials: G
authors.lastname: Pepe
authors.affiliation: Department of Pharmacy, University of Naples Federico II, Napoli, Italy.
authors.forename: Carmine
authors.initials: C
authors.lastname: Ostacolo
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, Roma, Italy.
authors.forename: Giulia
authors.initials: G
authors.lastname: Mazzoccanti
authors.affiliation: Laboratory of Food Chemistry, Dipartimento di Agraria (QuaSic. A. Tec.), Università Mediterranea di Reggio Calabria, Reggio Calabria, Italy.
authors.forename: Mariateresa
authors.initials: M
authors.lastname: Russo
authors.affiliation: Department of Pharmacy, University of Naples Federico II, Napoli, Italy.
authors.forename: Ettore
authors.initials: E
authors.lastname: Novellino
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, Roma, Italy.
authors.forename: Francesco
authors.initials: F
authors.lastname: Gasparrini
authors.affiliation: Department of Pharmacy, University of Salerno, Salerno, Italy.|European Biomedical Research Institute of Salerno, Salerno, Italy.
authors.forename: Pietro
authors.initials: P
authors.lastname: Campiglia
keywords: comprehensive two-dimensional liquid chromatography; monodisperse particles; polyphenols