In this study, the fungus species Aspergillus niger was used to produce as a single cell protein by using sugarcane molasses and effluent of sago industry. The substrates were pre analyzed to evaluate the quantity of nutritional contents. As per that result, the reducing sugar, total sugar, proteins, aminoacids and soluble carbohydrates were 1.27 gm/10gm & 2.3 gm/10gm; 2.07 gm/10gm & 2.65 gm/10gm; 2.06 & 2.23 gm/10gm; 1.65 & 2.05 gm/10gm; 2.25 & 3 gm/10gm in sugarcane molasses and sago waste respectively. The optimization results shows that the highest biomass content of was recorded on 4th and 5th day of fermentation at 5% concentration of each substrate (molasses and sago waste). The utilization of reducing sugar, total sugar, protein, amino acid, and carbohydrates was decreased with the increase in the concentration of biomass with the 5gm & 6gm concentration of molasses and sago wastes respectively. Further, the suitable pH were also recorded as, A. niger was effectively grown at pH 5.5 on sugarcane molasses and 7.5 on sago wastes. The post analysis report states that the ingredient content in the substrate was gradually decreased as compared to the quantity present in pre analysis. Finally the biomass of A. niger obtained from optimized condition the nutritional values were analysed. The results states that, the all the nutritional ingredients such as the reducing sugar, total sugar, proteins, aminoacids and soluble carbohydrates of molasses and sago wastes were 2.66 & 2.93, 3.67 & 3.65, 4.78 & 3.96, 2.81 & 2.94 and 3.71 & 3.49mg/1gm respectively at optimized pH and concentration. The present findings reveals that sugarcane molasses waste can be used as effective alternate carbon source for SCP production.