Canthium dicoccum is a shrub belongs to the family Rubiaceae. Ethnomedicine has evident the medicinal properties of different parts of this plant. During the present investigation, qualitative phytochemical analysis was carried out on the leaf extract of C. dicoccum and the results revealed the presence of carbohydrates, glycosides, saponins, alkaloids, phenols, flavonoids, tannins, steroids and volatile oils. HPTLC analysis showed the presence of useful compound i.e., Beta sitosterol. Further, investigation is been focused on the separation of phytochemical constituents by GC-MS technique using Perkin Elmer gas chromatogram and mass spectrometer. The mass spectra of the compounds found in three different extracts (Methanol, chloroform and petroleum ether) were matched with NIST 11 and Wiley 8 library. Sixteen compounds were identified in the methanolic extract, twenty four in petroleum ether and twenty in chloroform extract respectively. These compounds may be medicinally valuable and have wide applications in the pharmaceutical industry. The identified compound needs further research on toxicological aspects to develop safe drugs.