Multiresidue Determination of Fungicides in Wine by Solvent Demulsification-Dispersive Liquid-Liquid Microextraction and Ultra-High Performance Liquid Chromatography–Tandem Mass Spectrometry

Fungicides are applied from plant development to grape production, transport, and storage. Even after fruit processing, residues of these compounds can be present in grape by-products such as wine and juice. In this way, a fast and straightforward method based on solvent demulsification-dispersive liquid-liquid microextraction (SD-DLLME) sample preparation was developed, validated, and applied for the multiresidue determination of 30 fungicides in wine using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The evaluated SD-DLLME parameters were agitation types, extraction and dispersive solvent type, extraction and dispersive solvent volume, sample pH, and salt types. Sample preparation using SD-DLLME avoids the centrifugation step. Validation was performed using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 70 to 117% and precision in terms of relative standard deviation ≤20%, except for three compounds at the lowest spiked level. For most of the compounds, the practical method limits of detection and quantification were 0.03 and 0.1 μg L−1, respectively. The method was successfully applied in commercial wine samples in which several pesticides were found at concentrations ranging from 0.109 to 10.6 μg L−1.