In this study, a sensitive analytical method was developed to determine some pesticides (cyprodinil, trifloxystrobin, prometryn, propachlor, fenitrothion, chlorpyrifos, profenofos, and phosalone) in molasses samples. Pesticides were extracted from samples by dispersive liquid‐liquid microextraction method combined with sugaring‐out homogeneous liquid‐liquid extraction and determined by gas chromatography–mass spectrometry analysis. In this method, pesticides in molasses samples were first extracted using a water‐miscible solvent (acetonitrile) in the sugaring‐out homogeneous liquid‐liquid extraction stage. The sugar in the ratio of 84–88% naturally contained in the molasses sample enabled phase separation in the acetonitrile‐water homogeneous mixture. Then acetonitrile phase containing pesticides was used as dispersing solvent in the second step of the process. Under the specified optimum conditions, the limit of detection was calculated between 0.8–6.1 ng/g and the limit of quantification was in the range of 2.5–20 ng/g. The relative standard deviation values of molasses samples containing 150 ng/g of each analyte were found to be lower than 4.9% intra‐day and 5.6% for inter‐day. This validated method has been successfully applied to different types of molasses.