In this study, pressurized liquid extraction (PLE) was used with methanol as extraction solvent to extract bioactive compounds from Ananas comosus (pineapple) flesh. Response surface methodology (RSM) was used to evaluate the correlative effects of temperature (60 – 150°C) and extraction time (10 – 30 min) on the yield of selected bioactive compounds. In this model, the R2 obtained was 0.8788 for selected bioactive compounds for Ananas comosus suggesting a satisfactory agreement between the predicted and experimental values. Two-dimensional high-performance liquid chromatography (2D-HPLC) with a diode array detector (DAD) was used for the separation and detection of the bioactive compounds. Extraction temperature was found to significantly increase the yield of three selected bioactive compounds following which the optimum operating extraction conditions for PLE for Ananas comosus was determined to be 105°C and a static time of 20 min.