Magnetic Mesoporous Silica Composite for Enhanced Preconcentration of Selected Organophosphorus Pesticides in Fruits

Nur Husna Zainal Abidin; Wan Nazihah Wan Ibrahim; Nor Suhaila Mohamad Hanapi; Nor’ashikin Saim

doi:10.22146/ijc.42935

Magnetic Mesoporous Silica Composite for Enhanced Preconcentration of Selected Organophosphorus Pesticides in Fruits

https://doi.org/10.22146/ijc.42935

Nur Husna Zainal Abidin⁽¹⁾, Wan Nazihah Wan Ibrahim^(2*), Nor Suhaila Mohamad Hanapi⁽³⁾, Nor’ashikin Saim⁽⁴⁾

(1) Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(2) Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(3) Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(4) Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia
(*) Corresponding Author

Abstract

In the present work, MCM-41 coated magnetic particles (Fe₃O₄-MCM-41) composite was synthesized and employed as an effective adsorbent in magnetic solid phase extraction (MSPE) of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from grape and strawberry samples prior to high performance liquid chromatography with UV detection (HPLC-UV). The synthesized sorbent was physicochemically and morphologically characterized via Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and N₂ adsorption analysis. The main parameters on the extraction efficiency of selected OPPs, including extraction time, desorption solvent, desorption time, and sorbent dosage, were thoroughly optimized. Compared to MCM-41 sorbent, the newly synthesized Fe₃O₄-MCM-41 adsorbent shows a linear response (0.1-5.00 mg L^–1) with good determination coefficients ranging from 0.9900 to 0.9980, low limits detection (LODs), 0.02-0.15 mg L^–1 and low limit quantifications (LOQs), 0.06-0.40 mg L^–1. The precision as relative standard deviation (%RSD) of the proposed MSPE method was studied at low and high concentration (0.1-5.0 mg L^–1) based on intra-day (1.0 to 6.0%, n = 3) and inter-day (1.0 to 7.0%, n = 3), respectively. Fruit matrices were used to assess the field applicability of the sorbents. Comparatively, Fe₃O₄-MCM-41 achieved excellent percent recovery (85–120%) compared to the MCM-41 (70–110%). The result revealed that the Fe₃O₄-MCM-41 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from fruit samples.

Keywords

MCM-41; Fe3O4-MCM-41; organophosphorus pesticides; magnetic solid phase extraction

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References

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DOI: https://doi.org/10.22146/ijc.42935