title: Ultra-fast high-efficiency enantioseparations by means of a teicoplanin-based chiral stationary phase made on sub-2 μm totally porous silica particles of narrow size distribution.
abstract: A new ultra-high performance teicoplanin-based stationary phase was prepared starting from sub-2 μm totally porous silica particles of narrow size distribution. Columns of different lengths were packed at high pressure and a deep and systematic evaluation of kinetic performance, in terms of van Deemter analysis, was performed under different elution conditions (HILIC, POM, RP and NP) by using both achiral and chiral probes. For the achiral probes, the efficiency of the columns at the minimum of the van Deemter curves were very high leading to some 278,000, 270,000, 262,000 and 232,000 plates/m in hydrophilic interaction liquid chromatography (HILIC), polar organic mode (POM), normal phase (NP) and reversed phase (RP) respectively. The lowest plate height, Hmin=3.59 μm (h(/)=1.89), was obtained under HILIC conditions at a flow rate of 1.4 mL/min. Efficiency as high as 200,000-250,000 plates/m (at the optimum flow rate) was obtained in the separation of the enantiomers of chiral probes under HILIC/POM conditions. N-protected amino acids, α-aryloxy acids, herbicides, anti-inflammatory agents were baseline separated on short (2-cm) and ultra-short (1-cm) columns, with analysis time in the order of 1 min. The enantiomers of N-BOC-d,l-methionine were successfully baseline separated in only 11s in HILIC mode. Several examples of fast and efficient resolutions in sub/supercritical fluid chromatography were also obtained for a range of chiral carboxylic acids.
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Omar H
authors.initials: OH
authors.lastname: Ismail
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Alessia
authors.initials: A
authors.lastname: Ciogli
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Claudio
authors.initials: C
authors.lastname: Villani
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Michela
authors.initials: M
authors.lastname: De Martino
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Marco
authors.initials: M
authors.lastname: Pierini
authors.affiliation: Dipartimento di Scienze Chimiche e Farmaceutiche, Università di Ferrara, via L. Borsari 46, 44121 Ferrara, Italy.
authors.forename: Alberto
authors.initials: A
authors.lastname: Cavazzini
authors.affiliation: Sigma-Aldrich/Supelco, 595 North Harrison Road, Bellefonte, PA 16823, USA.
authors.forename: David S
authors.initials: DS
authors.lastname: Bell
authors.affiliation: Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Università di Roma, P.le Aldo Moro 5, 00185 Roma, Italy. Electronic address: francesco.gasparrini@uniroma1.it.
authors.forename: Francesco
authors.initials: F
authors.lastname: Gasparrini
mesh_terms: D000596:Amino Acids / Q000302:isolation & purification; D000893:Anti-Inflammatory Agents / Q000302:isolation & purification; D002264:Carboxylic Acids / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods; D025924:Chromatography, Supercritical Fluid / Q000379:methods; D006540:Herbicides / Q000302:isolation & purification; D057927:Hydrophobic and Hydrophilic Interactions; D007700:Kinetics; D008715:Methionine / Q000031:analogs & derivatives / Q000302:isolation & purification; D008958:Models, Molecular; D016062:Porosity; D011312:Pressure; D012822:Silicon Dioxide / Q000737:chemistry*; D013237:Stereoisomerism; D017334:Teicoplanin / Q000737:chemistry*
chemical_list: D000596:Amino Acids; D000893:Anti-Inflammatory Agents; D002264:Carboxylic Acids; D006540:Herbicides; D017334:Teicoplanin; D012822:Silicon Dioxide; D008715:Methionine
keywords: 1.9μm Titan particles; High efficiency and ultra-fast chiral separations; Short/ultra short columns; UHPC-Titan120-T(ZWIT)-1.9; UHPC-chiral separations