Core-shell microparticles formed by the metal-organic framework CIM-80(Al) (Silica@CIM-80(Al)) as sorbent material in miniaturized dispersive solid-phase extraction

Adrián Gutiérrez-Serpa; Ana I Jiménez-Abizanda; Francisco Jiménez-Moreno; Jorge Pasán; Verónica Pino

doi:10.1016/j.talanta.2020.120723

Core-shell microparticles formed by the metal-organic framework CIM-80(Al) (Silica@CIM-80(Al)) as sorbent material in miniaturized dispersive solid-phase extraction

Talanta. 2020 May 1:211:120723. doi: 10.1016/j.talanta.2020.120723. Epub 2020 Jan 7.

Authors

Adrián Gutiérrez-Serpa¹, Ana I Jiménez-Abizanda², Francisco Jiménez-Moreno³, Jorge Pasán⁴, Verónica Pino⁵

Affiliations

¹ Departamento de Química, Unidad Departmental de Química Analítica, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain. Electronic address: agutiers@ull.edu.es.
² Departamento de Química, Unidad Departmental de Química Analítica, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain. Electronic address: aijimene@ull.edu.es.
³ Departamento de Química, Unidad Departmental de Química Analítica, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain. Electronic address: fjimenez@ull.edu.es.
⁴ Departamento de Física, Laboratorio de Rayos X y Materiales Moleculares, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain. Electronic address: jpasang@ull.edu.es.
⁵ Departamento de Química, Unidad Departmental de Química Analítica, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain; Instituto Universitario de Enfermedades Tropicales y Salud Pública de Canarias, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206, Spain. Electronic address: veropino@ull.edu.es.

PMID: 32070617
DOI: 10.1016/j.talanta.2020.120723

Abstract

Core-shell SiO₂@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 SiO₂@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^-1, and inter-day precision lower than 14.1% for a concentration level of 0.5 μg L^-1. The extraction capability of SiO₂@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.

Keywords: Core-shell microparticles; Metal-organic frameworks; Miniaturized dispersive solid-phase extraction; Novel sorbent material; Silica-based materials; Water analysis.