Increasingly attention has been paid to the active substances in grapefruit peel. In this study, insoluble bound phenolic compounds (BP) were released from grapefruit peel insoluble dietary fiber (GP-IDF) by microwave extraction (M-BP), enzymatic hydrolysis (E-BP) and combined microwave and enzymatic treatment (ME-BP). The results showed that the yield of ME-BP was the highest (148.856 +/- 0.620 GAE mg/100 g), and conditions of microwave treatment (microwave power, temperature, time) were 600 W, 85 degrees C, and 37 min, while that of enzymatic treatment were 8% addition, 60 degrees C, and 2 h. Scanning electron microscopy displayed that GP-IDF became looser by ME. ME mainly resulted in the removal of lignin in IDF from X-ray diffraction, which was consistent with FT-IR. Twenty seven BP were identified by UPLC-ESI-QTOF-MS/MS. The high content of gallic acid (42.50 + 3.21 mu g/g DW), ferulic acid (18.46 +/- 1.65 mu g/g DW) and protocatechuic acid (6.16 + 0.72 mu g/g DW) was quantified by LC-ESI-QqQ-MS/MS. Furthermore, ME-BP showed stronger antioxidant capacities than that of others (ABTS, oxygen and DPPH free radical scavenging ability), and showed good inhibition of alpha-glucosidase. Our results demonstrated that combined microwave and enzymatic treatment was an effective treatment for improving the release of BP.