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模板导向合成三维金属有机骨架 199 衍生的高多孔铜纳米泡沫纤维,用于高效液相色谱法测定一些抗生素前的固相微萃取。

Template-directed synthesis of three-dimensional metal organic framework 199-derived highly porous copper nano-foam fiber for solid-phase microextraction of some antibiotics prior to their quantification by High performance liquid chromatography.

机构信息

Electroanalytical Chemistry Research Laboratory, Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran.

Electroanalytical Chemistry Research Laboratory, Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran.

出版信息

J Chromatogr A. 2021 Dec 20;1660:462677. doi: 10.1016/j.chroma.2021.462677. Epub 2021 Nov 8.

DOI:10.1016/j.chroma.2021.462677
PMID:34818591
Abstract

The in-situ preparation of three-dimensional MOF-199 (3D MOF-199) derived from the electrochemically prepared highly porous nano Cu foam on the surface of a flexible copper wire is reported. The 3D-Cu foam coating was used as a precursor and template for fabrication of MOF-199. The microextraction ability of the in-situ prepared 3D-MOF-199 fiber was evaluated using the prepared fiber for solid phase microextraction (SPME) of selected antibiotics including amoxicillin, azithromycin, ciprofloxacin, cefixime and gentamicin coupled to high-performance liquid chromatography with UV detection. Under the optimized condition, the calibration curves were linear in the range of 1-100 µg L   (r above 0.9921) for both water and urine matrices. Limits of detection and limits of quantification were 0.14-0.62 µg L   and 0.53-2.17 µg L   in the selected matrices, respectively. In addition, the repeatability of the method was evaluated by considering the relative standard deviation (RSD%). The intra-day and inter-day RSDs of the method with the single fiber was in the range of 2.8% to 4.9% and from 3.1% to 4.9%, respectively. Furthermore, the fiber-to-fiber reproducibility ranged from 2.9% to 5.5%. The enrichment factors were also in the range of 32 to 55. Finally, the method was successfully used for analysis of amoxicillin, azithromycin, ciprofloxacin, cefixime and gentamicin in urine samples. Relative recoveries for spiked urine samples were in the range of 90-105%.

摘要

本文报道了在柔性铜丝表面通过电化学制备的高多孔纳米 Cu 泡沫原位制备三维 MOF-199(3D MOF-199)。3D-Cu 泡沫涂层被用作制备 MOF-199 的前体和模板。通过使用制备的纤维进行固相微萃取(SPME),评估了原位制备的 3D-MOF-199 纤维的微萃取能力,所选抗生素包括阿莫西林、阿奇霉素、环丙沙星、头孢克肟和庆大霉素与高效液相色谱法与紫外检测相结合。在优化条件下,在水和尿液基质中,校准曲线在 1-100µg L-1范围内呈线性(r 均大于 0.9921)。在选定的基质中,检测限和定量限分别为 0.14-0.62µg L-1和 0.53-2.17µg L-1。此外,通过考虑相对标准偏差(RSD%)评估了该方法的重复性。该方法的日内和日间 RSD 分别在单纤维 2.8%-4.9%和 3.1%-4.9%的范围内。此外,纤维之间的重现性在 2.9%-5.5%的范围内。富集因子也在 32-55 的范围内。最后,该方法成功用于尿液样品中阿莫西林、阿奇霉素、环丙沙星、头孢克肟和庆大霉素的分析。加标尿液样品的相对回收率在 90-105%的范围内。

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