CIDEPINT   05376
CENTRO DE INVESTIGACIONES EN TECNOLOGIA DE PINTURAS
Unidad Ejecutora - UE
artículos
Título:
Fast RPLC analysis of pharmaceutical compounds at intermediate temperatures by using a conventional instrument
Autor/es:
JAVIER GOTTA; JAIVER OSORIO GRISALES; MARIO R. RETA; CECILIA B. CASTELLS
Revista:
JOURNAL OF SEPARATION SCIENCE
Editorial:
WILEY-V C H VERLAG GMBH
Referencias:
Año: 2010 vol. 33 p. 2645 - 2653
ISSN:
1615-9306
Resumen:
Recent developments in HPLC methods have focused on various strategies in order to increase the speed of analysis. One area of impressive growing is column technology. Today, analytical methods that propose the use of short columns packed with sub-2 m particles installed in ultra high-pressure LC instruments are not uncommon. Another strategy consisted of heating thermally resistant columns to temperatures well above of 100°C in order to reduce eluent viscosities and, therefore, column backpressure. We discuss experimental conditions for achieving high-throughput analysis using standard instruments with a few simple modifications. The chromatographic performance of two particulated and a silica-based monolithic column operated at moderate temperatures and flow rates are compared. The monolithic column proved to be stable over several thousands column volumes at 60°C. More important, its resistance to mass transfer at this temperature was significantly reduced. Very fast separations of two different mixtures of pharmaceutical compounds, anti-inflammatory drugs and -blockers, were achieved with the three columns at 60°C by using ACN/buffer at 5 mL/min. Excellent peak shapes of basic solutes and quite reasonable resolutions were achieved in very short analysis times with columns operated at temperatures moderately higher than the usual room temperature.