Bulk and precipitation polymerization methods were used to prepare ibuprofenmolecularly imprinted polymers. Molecularly imprinted polymer-bulk and -precipitation were synthesized in acetonitrile, likewise molecularly imprinted polymer-bulk (mixture) and molecularly imprinted polymer-precipitation (mixture) in a mixture of acetonitrile/toluene (75:25 v/v). N 2 adsorption-desorption analysis data revealed that molecularly imprinted polymer-precipitation (mixture) has the highest specific surface area (200.74 m 2 /g). The surface chemistry and morphology of the synthesized sorbents were investigated by Fouriertransform infrared analysis and scanning electron microscope micrographs respectively. The prepared sorbents in the mixture of solvents were used in a dispersive solid-phase extraction process for selective extraction and preconcentration of ibuprofen from urine and human plasma samples. The detection limits were 62.91 and 7.89 ng/ml using molecularly imprinted polymer-bulk (mixture) and molecularly imprinted polymer-precipitation (mixture), respectively. Also, the sorbents showed selective behavior to extract ibuprofen in the presence of naproxen, fenoprofen, and ketoprofen. Overall, the results showed that the precipitation method in the mixture of acetonitrile/toluene resulted in the preparation of a sorbent with the highest extraction efficiency. Furthermore, a pharmacokinetic study was done. The maximum plasma concentration, the time required for maximum plasma concentration, and plasma half-life were 28.95 μg/ml, 2, and 2.39 h, respectively.