State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, China.
Department of Environmental Science & Engineering, Tan Kah Kee College, Zhangzhou 363105, China.
Talanta. 2019 Jul 1;199:499-506. doi: 10.1016/j.talanta.2019.03.019. Epub 2019 Mar 2.
In this study, a new metal-organic framework-monolith composite for in-tube solid phase microextraction phase (IT-SPME) of fluoroquinolones (FQs) was prepared. 4-Vinylbenzoic acid was copolymerized with ethylenedimethacrylate in a fused silica capillary to form porous monolith. After that, zeolitic imidazolate frameworks (ZIF-8) were synthesized in situ within the pores and the surface of the monolith by controlled layer-by-layer self-assembly of Zn and imidazole. The introduction of ZIF-8 enhanced the surface area of monolith composite, and thus, improving the extraction performance of IT-SPME for FQs obviously. Under the optimized conditions, a highly sensitive method for the monitoring of FQs residue in water and honey samples was developed by the on-line combination of IT-SPME with high-performance liquid chromatography with fluorescence detection (HPLC-FLD). The limits of detection (S/N = 3) for the targeted FQs in water and honey samples were as low as 0.14-0.61 ng/L and 0.39-1.1 ng/L, respectively. The relative standard deviations (RSDs) for intra-day and inter-day assay variability were less than 10% in all samples. The established on-line IT-SPME-HPLC-FLD was successfully used to detect ultra-trace FQs in environmental water and honey samples. Recoveries at different spiked concentrations ranged from 80.1% to 119% and 80.2-117% for water and honey samples, respectively, with satisfactory reproducibility. Compared to up-to-date reported methods, the proposed approach exhibits some features such as high sensitivity, convenience, partial automation, low consumptions of sample and solvent.
在这项研究中，制备了一种用于氟喹诺酮（FQs）的管内固相微萃取（IT-SPME）的新型金属有机骨架-整体复合材料。4-乙烯基苯甲酸与二乙烯基苯在熔融石英毛细管中共聚形成多孔整体。之后，通过 Zn 和咪唑的逐层控制自组装，原位合成沸石咪唑酯骨架（ZIF-8）。ZIF-8 的引入增强了整体复合材料的比表面积，从而显著提高了 IT-SPME 对 FQs 的萃取性能。在优化条件下，通过在线结合 IT-SPME 和高效液相色谱荧光检测（HPLC-FLD），开发了一种用于监测水中和蜂蜜样品中 FQs 残留的高灵敏度方法。在水中和蜂蜜样品中，目标 FQs 的检测限（S/N=3）低至 0.14-0.61ng/L 和 0.39-1.1ng/L。所有样品的日内和日间测定变异性的相对标准偏差（RSD）均小于 10%。建立的在线 IT-SPME-HPLC-FLD 成功用于检测环境水样和蜂蜜样品中的痕量 FQs。在不同浓度下的回收率范围为 80.1%-119%和 80.2%-117%，水和蜂蜜样品的重现性良好。与最新报道的方法相比，该方法具有灵敏度高、方便、部分自动化、样品和溶剂消耗低等特点。
