Abstract-Sodium hydroxide pretreatment of oil palm mesocarp fiber (OPMF) was carried out with NaOH from 2% to 10% (w/v) at temperature 50 0 C and 70 0 C. The performances of pretreatments were evaluated based on total carbohydrate and reducing sugar including glucose, xylose and arabinose after enzymatic hydrolysis on the pretreated biomass. It was found that the enzymatic hydrolysis had significantly improved when 6% NaOH in 70 0 C applied in the pretreatment process. The highest total reducing sugars produced by means of commercial enzymes was achieved with the overall conversions of glucan and xylan of 87% and 60.73% respectively. The compositions of OPMF in this study are as follows (% g/g dry biomass): glucan, 28.8, xylan, 25.3, arabinan, 1.91, ethanol extractive, 6.32 and ash, 2.60.Index Terms-Enzymatic hydrolysis, glucose, NaOH pretreatment, oil palm mesocarp fiber.