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

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.

Ecofriendly and Facile One‐Pot Multicomponent Synthesis of 5‐Phenyl‐5,10‐dihydropyrido[2,3‐d : 6,5‐d′]dipyrimidine‐2,4,6,8(1H,3H,7H,9H)‐tetraone Derivatives Catalyzed by CuII Immobilized on Functionalized Magnetic Mesoporous MCM‐41 (Fe3O4@MCM‐41‐GPTMS‐Gu‐CuII)

“…H1‐type hysteresis loop [45a] (which is a characteristic of ordered mesoporous materials) (Figure 4 a). The specific surface area, pore‐volume, and mean pore diameter of Fe 3 O 4 @MCM‐41 ( II ) and Fe 3 O 4 @MCM‐41‐GPTMS‐Gu‐Cu II ( V ) are shown in Table 1.…”

Magnetic mesoporous Fe3O4@nSiO2@mSiO2 nanoparticles for high-throughput mass spectrometry detection of hydrolyzed products of organophosphorus nerve agents

“…11,12 Among them, magnetic mesoporous materials is advantageous due to their large specic surface area, high chemical stability, fast magnetic separation speed, and easy surface modication, 13,14 and they are widely used as adsorption materials for the QuEChERS method. Nur Husna Zainal Abidin et al 13 synthesized magnetic mesoporous Fe 3 O 4 @MCM-41 as purication materials to construct a rapid analysis method for organophosphorus pesticide residues in environmental substrates. Three organophosphorus pesticides (chlorpyrifos, diazinon, and methyl parathion) in grape and strawberry samples were analyzed.…”

“…A series of new purification materials, such as activated carbon nanofibers, 9 magnetic composite carbon nanotubes, 10 magnetic metal–organic framework materials, and magnetic mesoporous materials, have also been developed and utilized. 11,12 Among them, magnetic mesoporous materials is advantageous due to their large specific surface area, high chemical stability, fast magnetic separation speed, and easy surface modification, 13,14 and they are widely used as adsorption materials for the QuEChERS method. Nur Husna Zainal Abidin et al 13 synthesized magnetic mesoporous Fe 3 O 4 @MCM-41 as purification materials to construct a rapid analysis method for organophosphorus pesticide residues in environmental substrates.…”