Synthesis of magnetic Cu/CuFe2O4@MIL-88A(Fe) nanocomposite and application to dispersive solid-phase extraction of chlorpyrifos and phosalone in water and food samples

Herein, a novel Cu/CuFe2O4@iron-based metal-organic framework 88 A (Cu/CuFe2O4@MIL-88A(Fe)) was developed through a scalable hydrothermal strategy for the magnetic dispersive solid-phase extraction of chlorpyrifos and phosalone from water, fruit juice, and vegetable samples prior to corona discharge ion mobility spectrometry analysis. The resulting nanocomposite was characterized in detail, and thus the investigation indicated that the magnetic nanocomposite had good adsorption capacity, high surface area, dispersion, and superparamagnetic properties. In addition, the fabricated sorbent provided different interactions with the target analytes, (hydrogen bonding, hydrophobic contacts, and 7C-7C stacking interactions) resulting in the improvement of extraction efficiency. The applied method based on Cu/CuFe2O4@ MIL-88A(Fe) was validated by investigating the affecting parameters, including the amount of magnetic nanocomposite (10.0 mg), sample pH (7.0), salt content (7.5 % w/v), extraction time (5 min), type of elution (150 mu L of methanol), and desorption time (2 min). The linearity of the method was found to be in the range of 0.6-300.0 ng mL-1 and 1.5-500.0 ng mL-1, for chlorpyrifos and phosalone with the coefficient of determination of >= 0.9991. The limits of detections (LODs) of 0.2 and 0.5 ng mL- 1 were obtained for the determination of chlorpyrifos and phosalone, respectively. The relative standard deviation values (RSDs %) were calculated in the range of 4.4 %-6.1 % (intra-day, n = 5) and 6.3 %-8.0 % (inter-day, n = 3) for three days. Ultimately, the developed method was successfully applied for the extraction of the desired analytes from various spiked samples with acceptable recoveries (88.3-100.4 %).

Automated summary

A novel Cu/CuFe2O4@iron-based metal-organic framework was developed for magnetic dispersive solid-phase extraction of chlorpyrifos and phosalone from various samples. The method showed good adsorption capacity and high surface area, resulting in improved extraction efficiency through different interactions with the target analytes. Additionally, the method was validated and successfully applied for the extraction of desired analytes with acceptable recoveries.