Preparation and characterization of magnetic metal-organic framework nanocomposite as solid-phase microextraction fibers coupled with high-performance liquid chromatography for determination of non-steroidal anti-inflammatory drugs in biological fluids an

A novel solid-phase microextraction (SPME) fiber based on a capillary glass tube coated with magnetic Fe3O4/Cu3(BTC)2 metal organic frameworks nanocomposite was prepared by sol-gel technique. The magnetic Fe3O4/Cu3(BTC)2 metal organic frameworks nanocomposite were synthesized by a simple hydrothermal reaction and the resultant powder was mixed with sol-gel precursors to prepare sol-gel solution of the magnetic Fe3O4/Cu3(BTC)2 coating material. In this study, glass tubes with a specific diameter were used as substrates. The magnetic Fe3O4/Cu3(BTC)2 MOF nanocomposites coating was characterized using Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). Then, the synthesized fiber as novel solid-phase microextraction (SPME) fiber combined with high-performance liquid chromatography (SPME-HPLC) was applied for the determination and quantification of non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen, diclofenac, naproxen and nalidixic acid) in real samples including human urine, serum, plasma, and tablet formulation. To found optimum microextraction conditions, the influences of effective variables were investigated using one-factor-at-a-time experiments and the significant variables were optimized using a Box-Behnken design (BBD) combined with desirability function. Under optimized conditions, calibration graphs of analytes were linear in a concentration range of 0.1-400 μg L−1 with correlation coefficients >0.9966. Limits of detection and quantification were in the ranges of 0.03-0.0 5 μg L−1 and 0.12-0.18 μg L−1, respectively. This procedure was successfully employed in determining target analytes in spiked human urine, serum, plasma, and tablet samples with recoveries ranged from 94.0 to 102.0%.