Roselle (Hibiscus sabdariffa L.) is a comestible plant known for its fleshy red calyces that are used in making a wide range of foods such as wine, juice, jam, syrup, pudding, cakes, ice cream, and herbal tea. The anti- bacterial, diuretic, antioxidant, and anti-mutagenic effects of the roselle calyces are also well known. It is high in vitamins, minerals and bioactive substances such as organic acids, phytosterols, and polyphenols, and because of its extensive phar-macological potential, it has long been used as folk medicine to treat common cold. Gas chromatography-mass spectroscopy (GC-MS) is the best technique to identify the compounds present in the sample by mass spectra data obtained from purely available standards injected under the same conditions. In this study, the GC-MS technique was used to validate the pharmacological potential of Hibiscus sabdariffa by identifying the chemicals found in its calyces. The maximum cyanidin-3-glucoside was found to be the highest in PKM (Periyakulam) HS 04 1784.65 mg/100 g in cyanidin-3-glucoside equivalents, total flavonoid content (28.01 mg QE/g), and DPPH (2-diphenyl-1-picrylhydrazyl) activity % (93.17), and in PKM HS 02 total phenolic content (1.29 GA mg/g). The extract was prepared by soaking a dry calyx powder sample in methanol overnight and the ethanolic extract was then analyzed using GC-MS. Flavonoids, tannins, phenols, saponins, alkaloids, glycosides, terpenoids, and steroids were found in the ethanolic extract of Hibiscus sabdariffa calyces. The existence of 26 bioactive chemicals was discovered by GC-MS analysis, including phthalic acid, astaxanthin, lutein, lycoxanthin, 3-Pyridinecarboxylic acid, rhodoxanthin, molybdenum, and hexadecenoic acid. The presence of some of these bioactive chemicals has been used to support scientific evidence for the plant’s anti-aging, anti-oxidant, anti-hypertensive, and anti-inflammatory capabilities, which constitute valuable preliminary information in pharma industries.