A method using reversed-phase high-performance liquid chromatography with electrochemical detection for the assay of hydroxyurea in capsules was developed. Chromatographic conditions included an octadecyl column, a mobile phase containing sodium acetate-acetonitrile buffer of 95:5(v/v), pH 6.5 using 2-thiouracil as internal standard, and amperometric electrochemical detection at +700 mV. Linear detector response was found in the range 0.05~2.00 μM, and each run took 6 nun for method validation. The correlation coefficient (r) of the calibration curve was found to be 0.9999. The precision and accuracy tests revealed that RSD and RE of intra- and inter-day measurements were all well below 3.5%. Absolute recovery of hydroxyurea from capsules was averaged greater than 96.0%. A significant correlation on the assay of capsules was shown with the USP XXV method by two-tailed test. This method provides an alternative way of assay of hydroxyurea in capsules.