Solvent‐assisted dispersive solid‐phase extraction (SA‐DSPE) approach was developed to measure triazole fungicides (TFs). In the SA‐DSPE technique, the addition of 1000 μL of ethanol as a disperser solvent, along with a small quantity of benzil as a sorbent to the sample solution, led to a cloudy solution. After completion of the extraction, the mixture was subjected to centrifugation to isolate benzil. Next, benzil was dissolved in ethanol, and the resulting solution was subsequently analyzed by a gas chromatography‐flame ionization detector. This method demonstrated high linearity (R2 > 0.9963) and repeatability (relative standard deviation % < 4.3) for the quantification of TFs under the optimal conditions (sorbent: benzil, amount of benzil: 2% w/v, pH of solution: 7.0, disperser solvent: ethanol, volumes of ethanol: 1000 μL, centrifuge time: 3 min, extraction temperature: 25°C, and ionic strength: without salt addition). The proposed SA‐DSPE yielded detection limits, quantification limits, and preconcentration factors within the ranges of 0.3–0.9 ng/mL, 1.0–3.0 ng/mL, and 419–426, respectively. Finally, the validated method was employed to determine TFs in a diverse range of real samples, encompassing waters, fruits, vegetables, and agricultural soils, with relative recoveries ranging from 93.0% to 104%.