Magnetic solid-phase extraction of atrazine with ACC@NiCo₂O₄@Fe₃O₄ nanocomposite in spice and water samples

ABSTRACT

A simple, environmentally friendly, effective and selective magnetic solid-phase extraction method (MSPE) has been developed for the separation and quantitative determination of atrazine from spices and water samples before liquid chromatographic (LC) analysis. Activated carbon cloth@NiCo₂O₄@Fe₃O₄ was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction spectrometry (XRD), Brunauer–Emmett–Teller (BET), and scanning electron microscopy with energy distribution X-Ray detector (SEM-EDX) techniques. The developed MSPE-LC procedure was optimized in terms of pH, adsorbent amount, adsorption time, eluent type and volume, interference parameters and the pre-concentration factor and extraction efficiency at optimum conditions were determined. In the determination of atrazine, it was observed that the activated carbon cloth@NiCo₂O₄@Fe₃O₄ nanocomposite could be reused at least 25 times by applying the adsorption-desorption cycle. According to best extraction efficiency of parameters for the extraction and determination of atrazine from spices and water samples were determined as pH 7, adsorbent amount of 0 mg, total adsorption-desorption time of 5 minutes, and enrichment factor of 20. The recovery values of the magnetic solid-phase extraction method in spices and water samples under optimum conditions are between 91% and 94%. Analysis of trace levels of atrazine, limit of detection (LOD) and limit of quantification (LOQ) were determined by HPLC-DAD method with 0.5 ng mL⁻¹ and 1.7 ng mL⁻¹, respectively. Sample applications with high recovery values performed with the MSPE-LC method were confirmed by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) for spices and water samples.

GRAPHICAL ABSTRACT

KEYWORDS:

• Magnetic solid phase extraction
• activated carbon cloth
• spinel oxides
• atrazine
• spices
• water
• pesticides
• liquid chromatography

Acknowledgments

The authors thank to the Unit of the Scientific Research Projects of Erciyes University (FBG-2020-10013). The authors also thank to chromatography laboratories of Ege University, Central Research Testing and Analysis Laboratory Research and Application Center (EGE-MATAL).

Disclosure statement

No potential conflict of interest was reported by the authors.

Supplemental data

Supplemental data for this article can be accessed online at https://doi.org/10.1080/01496395.2023.2168203

Additional information

Funding

The work was supported by the Erciyes Üniversitesi [FBG-2020-10013].