Piplartine and piperine were extracted from Piper chaba by matrix solid-phase dispersion (MSPD) and determined by high-performance liquid chromatography (HPLC) with diode array detection (DAD). The experimental conditions for the MSPD were optimized. Silica gel was selected as dispersion adsorbent and methanol as elution solvent. The calibration curve showed good relationship (r>0.9998) in the concentration range of 5-100 μgmL^-1 for piplartine and piperine. The recoveries were between 90.6% and 100.9%. The proposed method consumed less sample, time and solvent compared with conventional methods, including ultrasonic and soxhlet extraction.