Ultrasound-assisted dispersive solid phase microextraction followed by UV-Vis spectrophotometry (UA-DSPME UV-Vis) was designed for the extraction and preconcentration of Carbaryl using nano-sized molecularly-imprinted polymer (MIP-NP). Nano-sized Carbaryl-imprinted polymer was characterized by scanning electron microscopy. A preliminary Plackett-Burman design was applied for screening. Subsequently, central composite design under response surface methodology was used to investigate and model the Carbaryl adsorption as response as well as to optimize this response versus variables such as Carbaryl MIP-NP mass, sonication time, temperature, eluent volume, pH and vortex time. At optimum experimental conditions, UAMSPE-UV-Vis exhibited a linear range of 0.1-1.2 mg L-1. The enhancement and preconcentration factors were obtained to be 30.6 and 25.0, respectively, for the extraction of Carbaryl by MIP-NP. In addition, the values of 0.033 and 0.11 mg L-1 were obtained for limit of detection and limit of quantification, respectively. The value of 4.3% determined for relative standard deviation for the separation and preconcentration of Carbaryl after 5 repetitions shows the acceptable repeatability of the process. Finally, the developed method was successfully applied for the determination of Carbaryl in water samples. (C) 2017 Elsevier Inc. All rights reserved.