Abstract: Pectin of pomelo peel was extracted with microwave-supercritical CO2 extraction. The factors of microwave power, extraction time, extraction pressure, extraction temperature and CO2 flow rate were discussed. The process was optimized with orthogonal experiment. The results showed that average yield of pectin was 22.63 % under the conditions of pomelo peel 5 g, microwave power 450 W, extraction time 15 min, extraction pressure 8.5 MPa, extraction temperature 40 ℃ and CO2 flow rate 12 L/h. The yield had been increased 6.50 % compared with the methods of conventional water bath heating under the same conditions.