Reduced graphene oxide decorated NiCo2(OH)6 nanoflowers for vortexed assisted dispersive µ-solid-phase extraction of organophosphorus pesticides in baby food cereal, rice and wheat flour

J Chromatogr A. 2024 Sep 27:1733:465277. doi: 10.1016/j.chroma.2024.465277. Epub 2024 Aug 15.

Abstract

Food safety is an important issue to protect humane health and improve the life quality. Hence, analysis of the possible contaminants in food samples is essential. A rapid and efficient vortexed-assisted dispersive µ-solid-phase extraction coupled with gas chromatography-mass spectrometry was proposed for simultaneous separation/preconcentration and determination of five commonly used organophosphorus pesticides. Reduced graphene oxide decorated NiCo2(OH)6 nanoflowers as a novel nanostructure was synthetized and introduced for separation of the target pesticides from the wheat flour, rice flour, and baby food cereal samples. The characterization of the nanoflowers was accomplished by SEM-EDX, XRD, and FT-IR techniques. The main factors including pH, the amount of nanoflower, the volume of sample solution, salt concentration (ionic strength), desorption conditions (i.e. desorption solvent type and volume, and desorption time) on the pesticides extraction efficiencies were inquired using matrixed match method. Applying the optimum conditions, the linearity of 0.100-500.000 µg kg-1, LODs and LOQs in the range of 0.03-0.04 µg kg-1 and 0.1 µg kg-1 for the studied food samples were obtained. The repeatability (intra-day precision (n = 5)) of ≤ 2.0 % and reproducibility (inter-day precision, days = 5, n = 3) of ≤3.1 % and were appraise at three concentration levels (10, 50 and 100 μg kg-1 of each analyte). High relative recoveries of 90.0-99.3 % ascertained high potential of the presented method for complex matrix analysis.

Keywords: Baby food cereal; Dispersive µ-solid-phase organophosphorus pesticides; NiCo(2)(OH)(6) nanoflowers; Reduced graphene oxide; Rice flour; Vortexed assisted; Wheat flour.

MeSH terms

  • Edible Grain* / chemistry
  • Flour* / analysis
  • Food Contamination / analysis
  • Gas Chromatography-Mass Spectrometry / methods
  • Graphite* / chemistry
  • Infant Food / analysis
  • Limit of Detection
  • Nanostructures / chemistry
  • Nickel / chemistry
  • Organophosphorus Compounds* / analysis
  • Organophosphorus Compounds* / chemistry
  • Organophosphorus Compounds* / isolation & purification
  • Oryza* / chemistry
  • Pesticide Residues / analysis
  • Pesticide Residues / isolation & purification
  • Pesticides / analysis
  • Pesticides / chemistry
  • Pesticides / isolation & purification
  • Reproducibility of Results
  • Solid Phase Extraction* / methods
  • Solid Phase Microextraction / methods
  • Triticum / chemistry

Substances

  • Graphite
  • graphene oxide
  • Organophosphorus Compounds
  • Pesticides
  • Nickel
  • Pesticide Residues