This article proposed an optimal hydrolysis condition and a chromatographic method for the analysis of polyphenol glycosides in aloe extract and its hydrolysates, The aglycones assayed were aloin and aloe-emodin, The linearity (r > 0.9997) and validation (< 10%) of the calibration curves were excellent. The amounts of aloin were 76.1 ± 5.9 and 77.7 ± 2.8 μmol/g in decoction and hydrolysate, respectively, while those of aloe-emodin were 8.3 ± 0.5 and 8.1 ± 0.3 μmol/g, The contents of aloin and aloe-emodin in aloe showed no significant difference before and after hydrolysis, This may be due to that aloe sold in Chinese medicine retailer was processed and the glycosides have already been transferred to aglycones. In addition, the components may be decomposed during processing. The method developed here can be applied to determine aglycones and their glycosides in aloe for the quality control.