Fabrication and characterization of magnetic metal–organic framework nanocompositeas solid-phase microextraction fibers coupled with high-performance liquid chromatography for determination of non-steroidal anti-inflammatory drugs in biological fluids and tablet formulation samples.

A novel solid-phase microextraction (SPME) fiber based on a glass tube coated with Fe3O4/Cu3(BTC)2 magnetic metal –organic formwork nanoparticle nanocomposite was prepared by sol–gel technique. The Fe3O4/Cu3(BTC)2nanocomposite were synthesized by a simple hydrothermal reaction and the resultant powder was mixed with sol–gel precursors to prepare sol–gel solution of the Fe3O4/Cu3(BTC)2 coating material. The prepared Fe3O4/Cu3(BTC)2 was deposited on surface of glass tubes as new substrate with a simple method. The results revealed that this procedure was a simple and reproducible technique for the preparation of SPME fibers coated with magnetic nanoparticles. The Fe3O4/Cu3(BTC)2nanocomposites was characterized using fourier transform infrared (FTIR) spectroscopy, powder x-ray diffraction (XRD)and scanning electronmicroscopy (SEM). Than this nanocomposite as novel solid-phase microextraction (SPME) fiber combined with high-performance liquid chromatography(SPME–HPLC) was applied for the determination and quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) (nalidixic acid, diclofenac, naproxen and ibuprofen) in biological fluids including serum, plasma and human urine. To found optimum extraction condition, the influences of effective variables were investigated using one-factor-at-a-time experimentsand then, the significant variables were optimized by using a Box–Behnken design (BBD) combined with desirability function. Under optimized conditions, calibration graphs of NAL, DIC, NAPand, IBUwere linear in a concentration range of 0.1-400μg L-1 with correlation coefficients more than 0.9966. Limits of detection and quantification were in the ranges of 0.03-0.05μg L-1 and 0.12-0.18μg L-1, respectively. This procedure was successfully employed in determining target analytes in spiked plasma, serum samplesandhuman urine samples; the relative mean recoveries ranged from 94.0 to 99.0%. The new approach offers an attractive alternative for the analysis of selected drugs from biological samples, providing several advantages including fewer sample preparation steps, faster sample throughput and ease of performance compared to traditional methodologies.