A fully automated sugaring-out assisted liquid-liquid extraction procedure was suggested. The procedure was based on the separation of the acetonitrile phase, containing a target analyte from the homogeneous sample solution after injection of sugaring-out reagent (glucose) into a mixing chamber of the flow system. Air bubbling was used to promote the extraction process and phase separation. After the fast phase separation in the mixing chamber, the acetonitrile phase containing the target analyte was transferred to an HPLC-UV system. Under the optimal conditions, the detector response of procainamide was linear in the concentration range of 6×10⁻⁷–4×10⁻⁵ mol L⁻¹. The limit of detection, calculated from a blank test based on 3σ, was 2×10⁻⁷ mol L⁻¹. The proposed method was successfully applied for the determination of procainamide in human urine samples and the analytical results agreed fairly well with the results obtained by reference CE method.