Photo-degradation of two drugs, Carbamazepine and Ciprofloxacin Hydrochloride was investigated in dark and sunlight. Following the degradation of Carbamazepine spectrophotometrically in sunlight, shows a regular decrease with time. The two peaks appeared in its HPLC chromatograms were identified by GC-MS to give compounds of molecular weights 196 and 256 respectively, having a half-life 693 h., while in the dark, there is an up and down decrease in absorbance, indicating a rapid cleavage of the compound. Ciprofloxacin hydrochloride in sunlight shows a sharp decrease in absorbance but the degraded compound shown in its HPLC chromatogram was not identified, and the degraded compound has a half-life of 31.5 h. For ciprofloxacin hydrochloride, no degradation was noticed in the dark. This proves that carbamazepine is more stable than ciprofloxacin hydrochloride.