Fast RPLC analysis of pharmaceutical compounds at moderately elevated temperatures by using a conventional instrument. Comparison between particulated and monolithic columns

JAVIER GOTTA; JAIVER OSORIO GRISALES; MARIO RETA; CECILIA CASTELLS

JOURNAL OF SEPARATION SCIENCE

WILEY-V C H VERLAG GMBH

Año: 2010 vol. 33 p. 2645 - 2653

1615-9306

Recent developments in high-performance liquid chromatographic 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 ultrahigh-pressure liquid chromatographic instruments is not uncommon. Another strategy consisted in heating thermally resistant columns to temperatures well above of 100ºC 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 60ºC. 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  β-blockers, was achieved with the three columns at 60ºC by using acetonitrile/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.