Abstract: TLC and HPLC were applied to the analysis (both qualitative and quantitative) of husk of aloe (which was disposed of as waste from aloe food factory) for the constituents of emodin and aloe-emodin. Kromasil-C18 column was used as stationary phase, the mixture of methanol and H3PO4 (85+15) was used as mobile phase for emodin and mixture of methanol and water (80+20) for aloe-emodin. UV-detection was made at the wavelength of 254nm. Linear relationships between values of peak area and mass were kept in the ranges of 3.75-300 mg for emodin and 2.5-200 mg for aloe-emodin. Values of recovery and RSD′s (n=5) were found 96.3% and 1.3% for emodin, 98.5% and 1.9% for aloe-emodin respectively. Husk of aloe obtained as waste from aloe food factory, was pre-treated and analyzed by HPLC for contents of emodin and aloe-emodin as described by the proposed method, average contents of emodin and aloe-emodin found were 71 mg·kg-1 and 28 mg·kg-1 respectively.