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This study aims to develop a dispersive liquid-liquid micro-extraction (DLLME) method for simultaneous determination of triazole fungicides (TFs). A hydrophobic molecular deep eutectic solvent (DES), composed of diphenylamine (DPA) and benzophenone (BZP) in a 1:1 molar ratio, was prepared as an extraction solvent for the adsorption of TFs. The rapid injection of a dispersion solvent containing the extraction solvent (DES) facilitated the extraction process, and phase separation was further accelerated through centrifugation. Under the optimal conditions, the proposed method provided a correlation coefficient greater than 0.993, with intra-day and inter-day RSDs ranging from 2.5% to 4.8% and 5.5% to 7.1%, respectively. The limits of detection and quantitation were found to be in the range of 0.5-1.0 ng mL − 1 and 1.6–3.3 ng mL − 1 , respectively. Enrichment factors ranged from 593 to 1380. Ultimately, the proposed extraction method successfully detected residual TFs, achieving relative recoveries between 84.6% and 109.6% in water, wheat, and rice samples. Furthermore, this study provides comparative insights into the presence of TFs in bran compared to hulled wheat samples. The findings demonstrate that the proposed DLLME method, based on a tailored hydrophobic DPA–BZP-1:1 DES, provides a simple, low-solvent, and selective sample preparation strategy, offering an effective methodological alternative for the routine monitoring of triazole fungicide residues in agricultural products and environmental samples.

A polybenzidine-modified Fe 3 O 4 @SiO 2 nanocomposite was successfully synthesized through a chemical oxidation method and employed as a novel sorbent in dispersive magnetic solid phase extraction (DMSPE) for the preconcentration and determination of three triazole fungicides (TFs), namely diniconazole, tebuconazole, and triticonazole in river water, rice paddy soil, and grape samples. The synthesis method involved a polybenzidine self-assembly coating on Fe 3 O 4 @SiO 2 magnetic composite. Characterization techniques such as FT-IR, XRD, FESEM, EDX, and VSM were used to confirm the correctness of the synthesized nano-sorbent. The target TFs were determined in actual samples using the synthesized nanocomposite sorbent in combination with gas chromatography–flame ionization detection (FID). Several variables were carefully optimized , including the sample pH, sorbent dosage, extraction time, ionic strength, and desorption condition (solvent type, volume, and time). Under the optimized experimental conditions, the method exhibited linearity in the concentration range 5–1000 ng mL −1 for triticonazole and 2–1000 ng mL −1 for diniconazole and tebuconazole. The limits of detection (LOD) for the three TFs were in the range 0.6–1.5 ng mL −1 . The method demonstrated acceptable precision with intra-day and inter-day relative standard deviation (RSD) values of less than 6.5%. The enrichment factors ranged from 248 to 254. Finally, the method applicability was evaluated by determining TFs in river water, rice paddy soil, and grape samples with recoveries in the range 90.5–106, indicating that the matrix effect was negligible in the proposed DMSPE procedure. Graphical Abstract