This paper describes the results of thermal stability studies of polybutadiene-coated zirconia reversed phases and application to fast HPLC separations at elevated temperatures and high flow rates. The thermal stability of the material was evaluated at temperatures up to 200 °C, and the rapid analyses of polyaromatic hydrocarbons and typical reversed-phase test mixtures were carried out at 100 °C and a flow rate of 5 mL/min. We found that the material is completely stable at 200 °C for at least 1300 column volumes. Analysis time can be decreased about 18-fold at high temperatures and flow rates without any significant loss in resolution relative to that at conventional temperatures and normal flow rates. For the separation of a five-component reversed-phase test mixture, the analysis time was only 50 s.