Synthesis and characterization of NiO nanoflower for dispersive micro solid phase extraction of zinc from water and food samples

Abstract

This study introduces a dispersive micro solid phase extraction (DµSPE) method utilizing NiO nanoflowers for the analysis of zinc in food, environmental, and wastewater samples, employing Inductively Coupled Plasma- Optical Emission Spectrometry (ICP-OES). The synthesized NiO nanoflower-like nanoparticle was characterized through Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), and Scanning Electron Microscopy (SEM). Additionally, various parameters including pH, sample volume, adsorbent quantity, and extraction time were investigated to optimize the NiO nanoflower-based SPME (NiO nanoflower-SPME) method. The analytical performance metrics, specifically the limit of detection (LOD), limit of quantification (LOQ), and relative standard deviation (RSD), were determined to be 0.77 µg L−1, 2.56 µg L−1, and 3.9 %, respectively. Furthermore, addition-recovery studies conducted on real samples, along with analyses of standard reference materials, were performed to validate the accuracy of the method. With these results, it was concluded that the NiO nanoflower-SPME method is crucial for the analysis of zinc in real samples due to the fact that the complex matrix environment complicates the analysis. © 2025 Elsevier Inc.