Departamento de Química, Unidad Departmental de Química Analítica, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain.
Departamento de Física, Laboratorio de Rayos X y Materiales Moleculares, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain.
Talanta. 2020 May 1;211:120723. doi: 10.1016/j.talanta.2020.120723. Epub 2020 Jan 7.
Core-shell SiO@CIM-80(Al) microspheres were synthesized, characterized, and used as novel sorbent in a dispersive miniaturized solid-phase extraction (D-μSPE) method for the determination of fourteen polycyclic aromatic hydrocarbons (PAHs) in wastewaters by ultra-high performance liquid chromatography coupled to a fluorescence detector (UHPLC-FD). A Doehlert experimental design permitted to optimize the main parameters affecting the microextraction procedure, intending the obtaining of a simple approach. Optimized extraction conditions include 13 mg of SiO@CIM-80(Al) microparticles (~2 mg CIM-80(Al)), 2.5 min of extraction time, 0.125 mL of acetonitrile (ACN) as desorption solvent and 0.5 min of desorption time. The entire method showed adequate analytical performance with limits of detection down to 5 ng L, and inter-day precision lower than 14.1% for a concentration level of 0.5 μg L. The extraction capability of SiO@CIM-80(Al) microspheres was compared to that obtained with commercially available silica microspheres and the neat MOF CIM-80(Al), demonstrating the advantages of the use of MOF core-shell sorbents in D-μSPE.
核壳结构的 SiO@CIM-80(Al) 微球被合成、表征，并被用作一种新型的固相萃取剂，用于分散微型固相萃取（D-μSPE）方法，以超高效液相色谱-荧光检测（UHPLC-FD）测定废水中的 14 种多环芳烃（PAHs）。采用 Doehlert 实验设计优化了影响微萃取过程的主要参数，旨在获得一种简单的方法。优化的萃取条件包括 13mg 的 SiO@CIM-80(Al) 微球（~2mg CIM-80(Al)）、2.5 分钟的萃取时间、0.125mL 的乙腈（ACN）作为洗脱溶剂和 0.5 分钟的洗脱时间。整个方法表现出良好的分析性能，检测限低至 5ng L，0.5μg L 浓度水平下的日内精密度低于 14.1%。SiO@CIM-80(Al) 微球的萃取能力与市售硅胶微球和纯 MOF CIM-80(Al) 的萃取能力进行了比较，证明了在 D-μSPE 中使用 MOF 核壳吸附剂的优势。
