In order to take full advantage of black wheat bran in the development of whole grain functional food, the crude polyphenols extracted from black wheat bran by ultrasonic-assisted method were purified, and the macroporous resin purification process was optimized to determine the optimal purification conditions. Moreover, liquid chromatography and mass spectrometry (LC-MS) technology were used to analyse the components of purified polyphenols in black wheat bran. The results indicated that when the concentration of sample solution was 1.20 mg/mL, and the concentration of elution solvent was 60%, with the injection flow rate of 1.50 mL/min, and the elution rate of 1.50 mL/min, the purification effect was better. The purity of polyphenols in black wheat bran before and after purification was 2.60%±0.28% and 14.27%±0.13%, respectively. The purity of polyphenols after purification was about 5.48 times of that before purification. Nine polyphenols contained probably in the purified black wheat bran were speculated. The above research showed that the macroporous resin purification process could purify the crude polyphenol extract of black wheat bran in an effective way, and maintain the diversity of polyphenols to some extent.