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

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@NiCo 2 O 4 @Fe...

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Bibliographic Details
Published in:	Separation science and technology 2023-03, Vol.58 (5), p.916-928
Main Authors:	Ozalp, Ozgur, Gumus, Z. Pinar, Soylak, Mustafa
Format:	Article
Language:	eng
Subjects:	Activated carbon activated carbon cloth Adsorbents Adsorption Analytical methods Atrazine Chromatography Cloth Desorption Electron microscopy Energy distribution Fourier transforms Herbicides High performance liquid chromatography HPLC Infrared spectroscopy Ions Iron oxides Liquid chromatography Magnetic solid phase extraction Mass spectrometry Mass spectroscopy Nanocomposites Nickel compounds Parameters pesticides Photoelectron spectroscopy Photoelectrons Quadrupoles Recovery Scanning electron microscopy Scientific imaging Solid phases Spices spinel oxides Trace levels water Water analysis Water sampling X ray detectors X ray photoelectron spectroscopy X rays X-ray diffraction
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Summary:	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@NiCo 2 O 4 @Fe 3 O 4 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@NiCo 2 O 4 @Fe 3 O 4 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.
ISSN:	0149-6395 1520-5754