Yolk-shell structure magnetic metal–organic framework nanoparticles were prepared via post solvothermal method and employed as a magnetic solid-phase extraction adsorbent for selective pre-concentration of 5′-ribonucleotides by π stacking interaction, hydrogen bonding, and the strong interaction between titanium ions (Ti⁴⁺) and phosphate group. The properties of the materials were confirmed by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectrometry, vibrating sample magnetometer, infrared spectroscopy, thermogravimetric analysis, and Brunauer–Emmett–Teller analysis. The main parameters affecting the adsorption–desorption process, including adsorbent amount, incubation time, incubation temperature, sample pH, shaking speed, elution solution, and elution time, were systematically optimized. Finally, 1.0?mg of adsorbent mixed with 1.0?mL sample solution (10.0?mmol?L^?1 NaCl, pH 3.0) and shaken at 135?rpm for 5?min at?40?°C, washed with 1.0?mL Na₃PO₄-NH₃?H₂O under vortex for 5?min were selected as optimized adsorption–desorption conditions. The binding performance of adsorbent towards five nucleotides was evaluated by static adsorption experiments. The data are well-fitted to the Langmuir isotherm model and the maximum adsorption capacity is 27.8?mg?g^?1 for adenosine 5′-monophosphate. The limit of detection of the method is 19.44–38.41?ng?mL^?1. Under the optimal conditions, the adsorbent was successfully applied to?magnetic solid-phase extraction and high performance liquid chromatography determination of five nucleotides in octopus, chicken, fish, and pork samples.

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