title: Transition from enantioselective high performance to ultra-high performance liquid chromatography: A case study of a brush-type chiral stationary phase based on sub-5-micron to sub-2-micron silica particles.
abstract: Three brush-type chiral stationary phases (CSPs) differing in the particle size of the starting silica particles have been prepared by covalent grafting of the pi-acidic bis-(3,5-dinitrobenzoyl)-derivative of trans-1,2-diaminocyclohexane (DACH-DNB). Starting silica particles of 4.3, 2.6 and 1.9micron were used to generate the final CSPs using an improved, highly reproducible synthetic methodology, that allowed to assemble and surface-graft the whole chiral selector in only two steps. The different CSPs have been packed in columns of various length and diameters, and fully characterized in terms of flow permeability, kinetic performances and enantioselectivity using a set of test solutes. Very high speed and high resolution applications together with stereodynamic HPLC examples are demonstrated on the columns with reduced particle diameters, on which separations of several enantiomeric pairs are routinely obtained with analysis times in the 15-40s range.
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Giovanna
authors.initials: G
authors.lastname: Cancelliere
authors.forename: Alessia
authors.initials: A
authors.lastname: Ciogli
authors.forename: Ilaria
authors.initials: I
authors.lastname: D'Acquarica
authors.forename: Francesco
authors.initials: F
authors.lastname: Gasparrini
authors.forename: Jelena
authors.initials: J
authors.lastname: Kocergin
authors.forename: Domenico
authors.initials: D
authors.lastname: Misiti
authors.forename: Marco
authors.initials: M
authors.lastname: Pierini
authors.forename: Harald
authors.initials: H
authors.lastname: Ritchie
authors.forename: Patrizia
authors.initials: P
authors.lastname: Simone
authors.forename: Claudio
authors.initials: C
authors.lastname: Villani
mesh_terms: D002725:Chloroform / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D004355:Drug Stability; D006586:Hexanes / Q000737:chemistry; D007700:Kinetics; D008958:Models, Molecular; D010316:Particle Size; D012822:Silicon Dioxide / Q000737:chemistry*; D013237:Stereoisomerism; D013454:Sulfoxides / Q000737:chemistry
chemical_list: D006586:Hexanes; D013454:Sulfoxides; D012822:Silicon Dioxide; D002725:Chloroform