A hybrid nanocomposite containing a moisture-resistant surface based on MOF-199 and carbon nanotubes (CNTs) was synthesized. Characterization was undertaken using powder X-ray diffraction (PXRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The adsorption behavior of the MOF-199/CNTs composite to ibuprofen was then investigated at room temperature. Experimentation revealed that the hybrid absorbent had excellent adsorption capacity for the nonsteroidal anti-inflammatory drug (NSAID), ibuprofen, with maximum adsorption up to 40.8 mg/g. The adsorbent was able to be recycled several times without deactivation. Finally, the MOF-199/CNTs composite was used as the extraction sorbents for selective extraction of ibuprofen, ketoprofen and naproxen in human urine. The results showed successful application of the nanocomposite to NSAID analysis in spiked human urine samples. Recoveries at three concentrations were 89.7-96.8%, 79.3-85.5% and 95.6-97.5% for ibuprofen, ketoprofen and naproxen, respectively. The relative standard deviations (RSDs) were within the range of 2.9-5.3%. The results demonstrated that the MOF-199/CNTs composite is an excellent adsorbent for determination of NSAIDs in spiked urine samples.