Method developers present a novel approach for simultaneous determination of melatonin and resveratrol with an optimized microextraction protocol. With the discovery of melatonin in wines, a new interest emerged in the health benefits of wine consumption, which are usually attributed to trans-resveratrol. In this context, a dispersive liquid–liquid microextraction for the analysis of melatonin and resveratrol in wines by LC-FLD was developed. A 26-1 factorial design was used to identify the significant variables (p < 0.05) and Central Composite Design was used to achieve the optimal conditions: 300 µL of chloroform (extracting solvent), 1500 µL of acetonitrile (disperser solvent) and 1500 mg of NaCl (ionic strength). Excellent linearity (R2 > 0.9999), repeatability (<3.55%), and accuracy (<7.18%) were obtained using a blank matrix and recoveries (>91.9%) using wines. The method was successfully applied to the analyses of different wine varieties; authors discuss advantages of the new method.
