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-solidphase
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