The aim of this study was to develop a novel surfactant-assisted ultrasound pretreatment of sugarcane tops as well as to optimize the effect of various operational parameters on pretreatment and hydrolysis. A novel surfactant-assisted ultrasound pretreatment was developed which could effectively remove hemicelluloses and lignin and improve the reducing sugar yield from sugarcane tops. Operational parameters for pretreatment and hydrolysis were studied and optimized. Under optimal hydrolysis conditions, 0.661 g of reducing sugar was produced per gram of pretreated biomass. The structural changes of native and pretreated biomass were investigated by Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared analysis (FTIR). The results indicate that surfactant-assisted ultrasound pretreated sugarcane tops can be used as a potential feed stock for bioethanol production.