<p>A new magnetic dispersive micro-solid-phase extraction method was developed for the detection of Pb(II) ions, using hierarchical nanocomposite (mMWCNTs@CoNiFe-LDH). This adsorbent synergistically combines magnetic multi-walled carbon nanotubes with flower-like CoNiFe-layered double hydroxide (LDH), providing rapid extraction within 3&#xa0;min and simple&#xa0;magnetic separation. The extensive characterization validated its porous core–shell design, elevated surface functioning, and thermal stability. Under optimal conditions, this method demonstrated good sensitivity (LOD: 0.142&#xa0;µg L⁻<sup>1</sup>, LOQ: 0.431&#xa0;µg L⁻<sup>1</sup>), and precision (RSD ≤ 4.2%). The nanocomposite exhibited high reusability and selectivity in the presence of significant concentrations of interfering ions. The approach, validated with certified reference materials (90–94% recovery) and used for several matrices (water, food and tobacco), indicated worrisome Pb concentrations in curry powder (22.1&#xa0;µg&#xa0;kg⁻<sup>1</sup>) and tobacco (71.8&#xa0;µg&#xa0;kg⁻<sup>1</sup>). Evaluations of greenness confirmed environmental sustainability. This method provides a fast and dependable&#xa0;option for analyzing&#xa0;Pb(II) in food and water samples.</p>

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Magnetic Dispersive Micro-Solid Phase Extraction of Pb(II) Using Core–Shell mMWCNTs@CoNiFe-LDH Nanoflowers From Food and Water Samples

  • Hassan Elzain Hassan Ahmed,
  • Ali Mohammednour Ali Mohammed,
  • Mustafa Soylak

摘要

A new magnetic dispersive micro-solid-phase extraction method was developed for the detection of Pb(II) ions, using hierarchical nanocomposite (mMWCNTs@CoNiFe-LDH). This adsorbent synergistically combines magnetic multi-walled carbon nanotubes with flower-like CoNiFe-layered double hydroxide (LDH), providing rapid extraction within 3 min and simple magnetic separation. The extensive characterization validated its porous core–shell design, elevated surface functioning, and thermal stability. Under optimal conditions, this method demonstrated good sensitivity (LOD: 0.142 µg L⁻1, LOQ: 0.431 µg L⁻1), and precision (RSD ≤ 4.2%). The nanocomposite exhibited high reusability and selectivity in the presence of significant concentrations of interfering ions. The approach, validated with certified reference materials (90–94% recovery) and used for several matrices (water, food and tobacco), indicated worrisome Pb concentrations in curry powder (22.1 µg kg⁻1) and tobacco (71.8 µg kg⁻1). Evaluations of greenness confirmed environmental sustainability. This method provides a fast and dependable option for analyzing Pb(II) in food and water samples.