This study investigated the effects of particle size and ultrasonic parameters on the yields of bioactive compounds extracted from the leaves and inflorescences of hemp. The total flavonoid and anthocyanin contents were determined using the spectrophotometric method. The response surface methodology (RMS) was employed to optimize the yield of bioactive substances. On the basis of the developed model, the highest flavonoid yield was obtained under the following extraction conditions: particle size, 0.59 mm; extraction time, 10.71 min; ultrasound intensity, 7.13 W∙cm−2; extraction yield, 9.28 mg QE∙g−1; determination coefficient, R2 = 0.97. The optimal conditions for extracting anthocyanins were as follows: particle size, 0.25 mm; extraction time, 15 min; ultrasound intensity, 8.60 W∙cm−2; extraction efficiency, 20.27 mg Cy-GE∙100 g−1; determination coefficient, R2 = 0.87. This study helped confirm the importance of pulsed ultrasound-assisted extraction in obtaining bioactive compounds from hemp. Keywords: Box–Behnken design; pulsed ultrasound-assisted extraction; hemp; flavonoids; anthocyanins; response surface methodology