Liquid chromatography of polymers is traditionally a slow technique with analysis times of typically 30 min per sample. To adapt liquid chromatographic techniques to combinatorial materials research the sample throughput must be significantly increased. Preferably, the analysis time per sample is to be reduced to a few minutes. Short analysis times can be achieved using high resolution stationary phases, high flow rates, and fast gradients. The present work demonstrates that gradient HPLC of polymethacrylates can be accomplished in less than 2 min. The fast separation of poly(methyl methacrylate), poly(i-propyl methacrylate), poly(n-butyl methacrylate), poly(tbutyl methacrylate), and poly(n-decyl methacrylate) is conducted on a short monolithic stationary phase using a flow rate of up to 7 mL/min. The optimization of the gradient is conducted by running a number of linear gradients and by simulating an optimum step gradient. Further modification of the simulated gradient results in the desired short analysis times.