This chapter deals with the synergistic effect of ultrasound and microwaves on the extraction of bioactives from plant materials. Extraction using solvent has been the method of choice for bioactive substances since a long time. Other methods of bioactives recovery include mechanical expression, supercritical fluid extraction, and microwave extraction. These techniques have constraints, such as an excess usage of solvents in the case of solvent extraction, unsatisfactory yield while applying mechanical pressing, high capital cost of supercritical fluid extraction, and the requirements of an aqueous medium in microwave aided extraction. Sonication or ultrasonic extraction offers benefits such as using fewer time and energy, extracting at a lower temperature, and retaining the extract's quality. This method is also ecofriendly and economical, as the requirements for solvents and additives are less. This is also a rapid method with a better separation and recycling of constituents. Pressure created during the application of ultrasound creates cavitation that is responsible for the better yield of the bioactives. This chapter discusses the factors affecting ultrasound assisted microwave extraction, construction of the device and also its application in plant systems.