Mesoporous silica sorbent with gold nanoparticles for solid-phase extraction of organochlorine pesticides in water samples

• Published in: Journal of Chromatography A 2022-01, Vol.1662, p.462729, Article 462729
• Main Authors: Pellicer-Castell, Enric, Belenguer-Sapiña, Carolina, Amorós, Pedro, El Haskouri, Jamal, Herrero-Martínez, José Manuel, Mauri-Aucejo, Adela R.
• Format: Article
• Language: English
• Subjects: Gas chromatography; Gold; Mesoporous silica; Organochlorine pesticides; Solid-phase extraction; Water analysis
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2021.462729

•A silica mesoporous material (UVM-7) doped with Au nanoparticles was synthesized.•Au/Ti-UVM-7 was applied to organochlorine pesticides extraction from water samples.•The material was characterized and the interaction of Au with analytes was proved.•Quantitative recoveries and good repeatability and sensitivity were achieved.•Real samples were analyzed in comparison with a C18 reference method. In this work, a novel sorbent, based on UVM-7 mesoporous silica doped with Au, has been proposed for organochlorine pesticides extraction. Cartridges containing this material have been applied to the preconcentration of 20 pesticides from water samples, through a solid-phase extraction (SPE) protocol, with their later determination by gas chromatography with an electron capture detector. First, UVM-7 materials were properly characterized by X-ray diffraction, N2 adsorption-desorption, electron microscopy techniques, and UV–Vis spectroscopy, thus confirming their structure and Au incorporation. After optimization of main extraction parameters, recoveries in the range of 80–110% were obtained for most of the analytes, with enrichment factors comprised between 275 and 430. The obtained sensitivity was comparable with other reported methods, with limits of quantification in the range of 0.3–20 ng L−1, thus allowing the determination of these compounds according to European legislation. The developed method has been successfully applied to the analysis of real spiked samples in comparison with a reference method, thus being this sorbent an alternative for organochlorine pesticide enrichment, through a simple, reusable, cheap, and environmentally friendly SPE procedure.