Investigation of polar stationary phases for the separation of sympathomimetic drugs with nano-liquid chromatography in hydrophilic interaction liquid chromatography mode |
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Authors: | Aturki Zeineb D'Orazio Giovanni Rocco Anna Si-Ahmed Kahina Fanali Salvatore |
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Institution: | aIstituto di Metodologie Chimiche, Consiglio Nazionale delle Ricerche, Via Salaria km 29.300, Area della Ricerca di Roma 1, Monterotondo Scalo 00015, Rome, Italy;bLaboratoire d’Analyse Organique Fonctionelle, Faculté di Chimie, USTHB. B.P. 32, El Alia Bab Ezzouar 16111, Alger, Algeria |
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Abstract: | In this study, the retention and selectivity of a mixture of basic polar drugs were investigated in hydrophilic interaction chromatographic conditions (HILIC) using nano-liquid chromatography (nano-LC). Six sympathomimetic drugs including ephedrine, norephedrine, synephrine, epinephrine, norepinephrine and norphenylephrine were separated by changing experimental parameters such as stationary phase, acetonitrile (ACN) content, buffer pH and concentration, column temperature. Four polar stationary phases (i.e. cyano-, diol-, aminopropyl-silica and Luna HILIC, a cross-linked diol phase) were selected and packed into fused silica capillary columns of 100 μm internal diameter (i.d.). Among the four stationary phases investigated a complete separation of the all studied compounds was achieved with aminopropyl silica and Luna HILIC stationary phases only. Best chromatographic results were obtained employing a mobile phase composed by ACN/water (92/8, v/v) containing 10 mM ammonium formate buffer pH 3. The influence of the capillary temperature on the resolution of the polar basic drugs was investigated in the range between 10 and 50 °C. Linear correlation of ln k vs. 1/T was observed for all the columns; ΔH° values were negative with Luna HILIC and positive with aminopropyl- and diol-silica stationary phases, demonstrating that different mechanisms were involved in the separation.To compare the chromatographic performance of the different columns, Van Deemter curves were also investigated. |
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Keywords: | Nano-liquid chromatography Hydrophilic interaction liquid chromatography Polar stationary phases Sympathomimetic drugs |
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