A magnetic supramolecular solvent microextraction strategy for sensitive HPLC determination of triazoles in fruits and vegetables

In this study, a green, and rapid sample preparation method based on magnetic supramolecular solvent microextraction (M-SUPRA) was developed for the preconcentration and high-sensitivity determination of trace triazole residues in fruit and vegetable matrices prior to high-performance liquid chromatography (HPLC) analysis. The magnetic supramolecular solvent was synthesized via the self-assembly of amphiphilic coacervates integrated with functionalized magnetic nanoparticles (Fe 3 O 4 ). This system offers multi-interaction binding sites (hydrophobic, hydrogen bonding, and π − π interactions) and enables rapid phase separation via an external magnetic field without requiring high-speed centrifugation or toxic organic dispersants. Key experimental parameters affecting extraction efficiency, including M-SUPRA composition, solvent volume, sample pH, ionic strength, and extraction time, were systematically optimized. Under optimal conditions, the method exhibited excellent linearity with coefficients of determination (R 2 > 0.99). The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 1.0 µg L –1 to 7.0 µg L –1 and 3.0 µg L –1 to 20.0 µg L –1 , respectively, with high enrichment factors (4 – 57). The proposed M-SUPRAS-ME protocol provides a sustainable, highly sensitive, and practical tool for routine monitoring of pesticide residues in complex food matrices. Additionally, the environmental impact and analytical practicality of the developed method were evaluated.