In this study, a comparison study between two recent extraction methods, namely ultrasound-assisted molecularly imprinted polymeric nanoparticles solid-phase extraction (US-MIPNPs-SPE) and the solidification of floating organic drop-assisted dispersive liquid–liquid microextraction (SFOD-DLLME), for the preconcentration and separation of morin is presented. The morin-MIP NPs, with an average particle size of 57 nm, were synthesized using a precipitation polymerization strategy using methacrylic acid (MAA) and ethyleneglycoldimethacrylate (EGDMA) as functional and cross-linking monomers, respectively. After the synthesis and characterization, the prepared MIP was used as an efficient nano-scale sorbent in the ultrasound-SPE procedure. The effects of various parameters on the extraction efficiency of the morin, including the pH of the sample solution, adsorption and desorption times, initial sample volume, and volume and type of eluent, were investigated in batch experiments. After optimization, isotherm and kinetic models for the adsorption of morin onto morin-MIP NPs were evaluated and fitted. In the SFOD-DLLME procedure, the affecting parameters on morin recovery, such as the type, the volume of extraction and dispersive solvents, pH of the initial sample solution, extraction time, and ionic strength, were studied too.