A simple, sensitive and inexpensive method was developed using solid-phase extraction, together with high performance liquid chromatographic method with UV detection for determination of hydrogen cyanamide residues. The evaluated parameters include the type of column (CHEM ELUTTM), the nature of eluent (hexane, ethyl acetate, methanol and water) and procedure of derivatization. The method was validated using grape juice samples spiked with hydrogen cyanamide at different concentration levels (0.03 and 0.3 μg/mL). Average recoveries (using each concentration six replicates) ranged 89-92%, with relative standard deviations less than 2%, calibration solutions concentration in the range 0.01-10.0 μg/mL and limit of detection (LOD) and limit of quantification (LOQ) were 0.01 μg/mL and 0.03 μg/mL respectively.