Insights in the analytical performance of neat metal-organic frameworks in the determination of pollutants of different nature from waters using dispersive miniaturized solid-phase extraction and liquid chromatography
Five metal-organic frameworks (MOFs), specifically HKUST-1, MOF-5(Zn), MIL-53(Al), UiO-64 and MOF-74(Zn) are synthesized, characterized, and utilized in a miniaturized solid-phase extraction method under dispersive mode (D-µSPE) for the determination of six pollutants of different nature, including...
| Autores: | , , , , , , |
|---|---|
| Formato: | artículo |
| Estado: | Versión borrador |
| Fecha de publicación: | 2018 |
| País: | España |
| Recursos: | Universidad de Jaén |
| Repositorio: | RUJA. Repositorio Institucional de la Producción Científica de la Universidad de Jaén |
| OAI Identifier: | oai:ruja.ujaen.es:10953/4592 |
| Acesso em linha: | https://hdl.handle.net/10953/4592 |
| Access Level: | acceso abierto |
| Palavra-chave: | Metal-organic frameworks Sample perparation Dispersive micro solid-phase extraction Pollutants Environmental waters |
| Resumo: | Five metal-organic frameworks (MOFs), specifically HKUST-1, MOF-5(Zn), MIL-53(Al), UiO-64 and MOF-74(Zn) are synthesized, characterized, and utilized in a miniaturized solid-phase extraction method under dispersive mode (D-µSPE) for the determination of six pollutants of different nature, including one polycyclic aromatic hydrocarbon, two hormones, two drugs, and one disinfectant, from environmental waters (tap water and wastewater). A discussion of possible interactions justifying the partitioning of target analytes to the MOFs is included, considering not only the analytes’ physicochemical characteristics but also those of MOFs: metal nature, structural environment of MOF pores, pore size and pore aperture widths, among others. MIL-53(Al) is selected for its versatility and high extraction efficiency for the target compounds. The D-µSPE method using MIL-53(Al) is optimized and used in combination with high-performance liquid chromatography (HPLC) with diode array detector (DAD) or liquid-chromatography with time-of-flight mass spectrometric detector (LC-TOF). Under optimum conditions, only 5 mg of MIL-53(Al) are required for 10 mL of water, with the aid of 5 min of vortex and 5 min of centrifugation. Elution is accomplished with 200 µL of acetonitrile (3 times), and evaporation down to 100 µL before LC injection. Detection limits down to 0.040 μg L−1 for triclosan and 0.013 μg L−1 for atrazine are obtained for the entire method using HPLC-DAD and LC-TOF, respectively. The method, operating at low spiked levels (2 µg L−1 for HPLC-DAD and 0.7 µg L−1 for LC-TOF), is also characterized for average relative recoveries of 109% and 105%; relative standard deviation values lower than 8.7% and 7.5%; and average extraction efficiencies of 41.2% and 49.1%; using HPLC-DAD and LC-TOF, respectively; while demonstrating adequate analytical performance with complex samples such as wastewaters. |
|---|