To produce xylo-oligosaccharides (XOS) from the agriculture waste, which included, green coconut and vegetable cocktail. The two pretreatment – hydrogen peroxide-acetic acid (HP-AC) and sodium hypochlorite-sodium hydroxide (SH-SH) – were used for this study. The optimal conditions for the pretreatment were 80 °C, 4.0 % NaClO, and 2 h, followed by 0.08 % NaOH, 55 °C, and 1 h. Further enzymatic hydrolysis of green coconut (GC) and vegetable cocktail (VC) were performed and found in case of GC, the best outcomes were observed. Different types of XOS were obtained from the treated biomass whereas a single type of XOS xylo-pentose was obtained in high quantity (96.44 % and 93.09 % from CG and VC respectively) with the production of other XOS < 2 %. This study presents a reasonably secure and economical method for turning secondary crop residue into XOS and fermentable sugars.