A new approach to determination of good correlations between in vivo and in vitro dissolution was studied using the optimization technique. Ibuprofen, which exhibits dissolution rate-limiting absorption, was used as a model drug. Ibuprofen capsules of two different release types were prepared, and their in vivo dissolution profiles were obtained from measurements of plasma concentration following oral administration of the capsules to beagle dogs by the mathematical deconvolution method using solution data of oral administration as a weight function. For the dissolution test to correspond to the in vivo dissolution profiles, the test was carried out at 12 levels (9 different sets of conditions) and results were analyzed with the optimization technique to deal with two factors. The first-order rate constant (k_d) and the dissolution time at 50% (t₅₀%) of the in vivo dissolution were selected for use as the response variables. Regression analysis was performed to describe the in vitro dissolution characteristics as functions of the pH of dissolution medium and paddle rotation speed in the paddle method. The in vivo/in vitro correlation obtained from the k_d was better than that obtained from the t₅₀%. The optimum conditions for dissolution testing corresponding to the in vivo k_d were determined to be a pH 6.6 for the dissolution medium and a 56 rpm paddle rotation rate. The experimental data obtained by dissolution testing was well fit by the predicted curve derived from in vivo and in vitro dissolution profiles. This dissolution test is applicable to the formulations containing ibuprofen of particle size within the experimental range.