Abstract 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%.

中文翻译：

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磁性金属-有机骨架纳米复合材料作为固相微萃取纤维的制备和表征结合高效液相色谱法测定生物体液和片剂配方样品中的非甾体抗炎药

摘要 采用溶胶-凝胶技术制备了一种新型固相微萃取（SPME）纤维，其基于毛细玻璃管，表面涂覆有磁性Fe3O4/Cu3(BTC)2金属有机骨架纳米复合材料。通过简单的水热反应合成磁性 Fe3O4/Cu3(BTC)2 金属有机骨架纳米复合材料，并将所得粉末与溶胶-凝胶前驱体混合，制备磁性 Fe3O4/Cu3(BTC)2 涂层材料的溶胶-凝胶溶液。在这项研究中，具有特定直径的玻璃管被用作基板。使用傅里叶变换红外 (FTIR) 光谱、粉末 X 射线衍射 (XRD) 和扫描电子显微镜 (SEM) 对磁性 Fe3O4/Cu3(BTC)2 MOF 纳米复合涂层进行了表征。然后，将合成的纤维作为新型固相微萃取 (SPME) 纤维结合高效液相色谱 (SPME-HPLC) 用于非甾体抗炎药 (NSAID)（布洛芬、双氯芬酸、萘普生和萘啶酸）在真实样品中，包括人尿、血清、血浆和片剂配方。为了找到最佳微萃取条件，使用一次一个因素的实验研究了有效变量的影响，并使用 Box-Behnken 设计 (BBD) 结合合意性函数优化了重要变量。在优化条件下，分析物的校准图在 0.1–400 μg L-1 的浓度范围内呈线性，相关系数 >0.9966。检测限和定量限在 0.03–0 的范围内。0 5 μg L-1 和 0.12–0.18 μg L-1，分别。该程序已成功用于测定加标人尿、血清、血浆和片剂样品中的目标分析物，回收率范围为 94.0% 至 102.0%。