Browsing by Author "Junaid, A. M."

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    Determination of pesticide residues in beans using QuEChERS technique coupled to gas chromatography-mass spectrometry: Multivariate optimization of CEN and AOAC methods
    (Elsevier, 2025) Abdulra’uf, L. B.; Junaid, A. M.; Lawal, A. R.; Ibrahim, H. B.; Tan, G. H.
    The use of pesticides has led to environmental pollution and posed a global health risk, since they remain as residues on foods. Beans one of the most widely cultivated crop in Africa, and susceptible to attack by insects both on field and during storage, leading to the application of pesticides to control pests’ infestation. However, misuse of these chemicals by farmers on beans has resulted in the rejection of beans exported to European countries, due to the presence of pesticide residues at concentrations higher than the maximum residues levels (MRLs). In this study, the effectiveness of the Association Official Analytical Chemists (AOAC) Official Method and the European Committee of Standardization (CEN) Standard Method, were determined using multivariate approach for the analysis of organochlorine pesticide residues in 6 varieties of beans samples. The significance of factors (mass of sample, volume of acetonitrile, mass of magnesium sulphate, sample pH, centrifugation time and speed) affecting the efficiency of extraction was estimated using Plackett-Burman design, while central composite design was used to optimize the significant factors. The following optimum factors were subsequently used for method validation, recovery tests, and real sample analysis: 4 g of sample sludge (1:1 v/v), 10 mL of acetonitrile, 4.45 g of MgSO4, and 5 min of centrifugation at 5000 rpm. The figure of merit of analytical methodology estimated using matrix-matched internal standard calibration method gave linearity ranging from 0.25 to 500 μg/kg, with correlation coefficient (R2) greater than 0.99, the recovery ranged from 75.55 to 110.41 (RSD = 0.70–16.65), with LOD and LOQ of 0.23–1.77 μg/kg and 0.76–5.88 μg/kg, respectively.
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    Dispersive liquid-liquid microextraction/HPLC techniques for determination of oxytetracycline and doxycycline residues in beef samples: method developments and statistical analysis
    (Nigerian Society of Physical Sciences, 2023-04-10) Aliu, M. A.; Junaid, A. M.; Ibraheem, A.; Ishaq, A.; Lawal, A.; Ayeni, K. E.; Lawal, A. R.; Abdulrauf, L. B.
    A rapid, cost-effective and environment-friendly sample pre-treatment method involving dispersive liquid-liquid microextraction (DLLME) and high-performance liquid chromatography (HPLC) was developed and applied for the extraction of oxytetracycline and doxycycline residues in beef samples (liver, kidney and muscle). Several influencing factors associated with the extraction and separation of these antibiotics residues, such as sample size, type and volume of disperser and extraction solvents, centrifugation speed and time, were optimized using Plackett-Burman design and central composite design, while insignificant factors were fixed at values determined using univariate analysis. Figures of merit of the analytical methodology including the limit of detection (LOD), the limit of quantification (LOQ), accuracy (in terms of average recoveries), precision and calibration functions were established according to the European Union commission decision 2002/657/EC. Linearity, in the range of 5–500 µg/kg, was obtained with regression coefficients ranging from 0.9983 – 0.9999. Inter-day repeatability, intra-day precision, LODs and LOQs obtained were 3.81 – 14.90%, 3.80 – 8.70%, 4.21 – 4.69 µg/kg and 14.02 – 15.65 µg/kg respectively. Samples with detectable drug residues have oxytetracycline being the most commonly detected. The developed method was successfully established and the concentration levels of drug residues detected were lower than the European Union set maximum residue level (MRL).