A sensitive, accurate, and reproducible high-performance liquid chromatographic procedure for the analysis of indapamide in human whole blood is reported. After a single-step liquid-liquid extraction at pH 6.6 using diethyl ether, indapamide was eluted from a Nucleosil C18 5-microns column with 80 mM ammonium acetate, pH 3.5-acetonitrile-2-propanol (65:30:5, v/v/v). The peak height versus whole blood concentration was linear over the range 10.0-500 ng/ml using ultraviolet detection. The mean absolute recovery of indapamide using the described assay was 87.4%. The inter- and intra-day accuracy and precision were within 9.6% of the actual values for all concentrations investigated. Furthermore, this procedure was applied to the analysis of whole blood samples from healthy subjects receiving a single 2.5-mg oral dose of indapamide.