A high- performance liquid chromatographic procedure was established for the estimation of procaine hydrochloride as a bulk material or in injection. Li Chrocart C18 (Merck) column and a mobile phase consisting of 0.02 M sodium acetate containing 0.1% trimethylamine and 15% acetonitrile, adjusted with glacial acetic acid to PH 4.5, was used. Detection made at 254 nm with a fixed wavelength absorbance detector. The drug content can be quantitated with or without internal standard when a precision loop injector (Rheodyne 7010) is used. Keywords :