A fast and sensitive high-pressure liquid chromatographic method was developed for the quantitation of doxorubicin, daunorubicin, and their aglycones in pharmaceutical preparations. Because its higher pH extends column life while permitting determination of impurities, this system represents an improvement over previously published methods. It utilizes a C18 bonded silica gel column and a solvent system consisting of methanol-0.01 M monobasic ammonium phosphate aqueous solution (65:35) at pH 4.0 and 1600 psi of pressure. The accuracy of the doxorubicin and daunorubicin determinations, expressed as the coefficient of variation, is 1.65 and 1.27% respectively. The aglycones can be determined with a precision of less than 1.3%.