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Sorghum and millet are important food staples in semi-arid tropics of Asia and Africa. Sorghum and millet are cereal grains that have prospective to be used as substitute to wheat flour for celiac patients. These are considered as the good source of many important and essential fatty acids. The volatile profiling of these two important crops is comparable to other cereals as well. The present study was an effort to explore biochemical composition of commercially available sorghum and millet varieties with special reference to their fatty acid and volatile profiling. Chemical composition of sorghum and millet was determined according to respective methods. Fatty acid methyl esters were prepared and then subjected to GC-FID for fatty acids analysis. The results indicated that both sorghum and millet oils are rich in essential fatty acids comprising mono and polyunsaturated fatty acids. Main fatty acids that are identified in current study includes palmitic acid, oleic acid, palmitoleic acid, behenic acid, linoleic acid, linoleic acid, stearic acid, myristic acid, etc. On the other hand volatile compounds from sorghum and millet were determined by preparing their respective volatile samples by using calvenger apparatus with suitable volatile extracting solvent. Volatile samples were then subjected to GC-MS analysis and respected results were compared with NIST library. About 30 different volatiles were identified in millet varieties while 35 different compounds were discovered in sorghum varieties belonging to aldehydes, ketones, benzene derivatives, esters, alcohols, sulphur compounds.