A new ultra-high performance teicoplanin-based stationary phase was prepared starting from sub-2μm totally porous silica particles of narrow size distribution. Columns of different lengthswere 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/meter in Hydrophilic Interaction (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/meter (at the optimum flow rate) was obtained in the separation of the enantiomers of chiral probes under HILIC/POM conditions. N27 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 one minute. The enantiomers of N-BOC-D,L-methionine were successfully baseline separated in only 11 seconds 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.

Ultra-fast high-efficiency enatioseparations by means of a teicoplanin-based chiral stationary phase made on sub-2μm totally porous silica particles of narrow size distribution / Ismail, OMAR HABIB; Ciogli, Alessia; Villani, Claudio; DE MARTINO, Michela; Pierini, Marco; Cavazzini, Alberto; Bell, David S.; Gasparrini, Francesco. - In: JOURNAL OF CHROMATOGRAPHY A. - ISSN 0021-9673. - STAMPA. - 1427:(2016), pp. 55-68. [10.1016/j.chroma.2015.11.071]

Ultra-fast high-efficiency enatioseparations by means of a teicoplanin-based chiral stationary phase made on sub-2μm totally porous silica particles of narrow size distribution

ISMAIL, OMAR HABIB;CIOGLI, Alessia;VILLANI, Claudio;DE MARTINO, MICHELA;PIERINI, MARCO;GASPARRINI, Francesco
2016

Abstract

A new ultra-high performance teicoplanin-based stationary phase was prepared starting from sub-2μm totally porous silica particles of narrow size distribution. Columns of different lengthswere 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/meter in Hydrophilic Interaction (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/meter (at the optimum flow rate) was obtained in the separation of the enantiomers of chiral probes under HILIC/POM conditions. N27 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 one minute. The enantiomers of N-BOC-D,L-methionine were successfully baseline separated in only 11 seconds 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.
2016
1.9μm titan particles, high efficiency and ultra-fast chiral separations, short/ultra short columns.
01 Pubblicazione su rivista::01a Articolo in rivista
Ultra-fast high-efficiency enatioseparations by means of a teicoplanin-based chiral stationary phase made on sub-2μm totally porous silica particles of narrow size distribution / Ismail, OMAR HABIB; Ciogli, Alessia; Villani, Claudio; DE MARTINO, Michela; Pierini, Marco; Cavazzini, Alberto; Bell, David S.; Gasparrini, Francesco. - In: JOURNAL OF CHROMATOGRAPHY A. - ISSN 0021-9673. - STAMPA. - 1427:(2016), pp. 55-68. [10.1016/j.chroma.2015.11.071]
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11573/844729
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