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@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.

Automated summary

A simple, effective and selective magnetic solid-phase extraction method was developed for the separation and quantitative determination of atrazine from spices and water samples. The optimized MSPE-LC procedure achieved a high extraction efficiency under pH 7, 0 mg adsorbent amount, 5 minutes total adsorption-desorption time, and a 20 enrichment factor. The recovery values for the magnetic solid-phase extraction method in spices and water samples were between 91% and 94%. The HPLC-DAD method determined the limit of detection (LOD) and limit of quantification (LOQ) for atrazine as 0.5 ng mL(-1) and 1.7 ng mL(-1), respectively.