<p>A novel approach combining a cold probe with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) was developed to simplify the retrieval of organic solvents from aqueous sample surfaces. Custom-designed cooled probes containing a 1:1 water-ethylene glycol mixture enabled efficient and rapid solvent collection without the need for cooling the sample. The method was applied to quantify propargite in fruit samples using the gas chromatography-mass spectroscopy technique. Extraction parameters were optimized using both one-variable-at-a-time and simplex methods, yielding optimal conditions (1 mL dispersing solvent, 200 µL extraction solvent, 2 min extraction time, 5 min centrifugation, 50 °C, no salt addition). The method achieved a limit of detection of 0.051 µg mL⁻¹, a relative standard deviation of 8.6%, and an average extraction recovery of 103.9% across six replicate analyses. The technique demonstrated robust applicability for determining propargite in real fruit samples, offering a simple and effective approach for trace-level pesticide analysis.</p>