AbstractWe describe a method for measuring adriamycin and its metabolites, adriamycinol and adriamycinone in plasma, using reversed phase HPLC and fluorescence detection. The lower limit of detection is approximately 1 ng/mL for each compound. An extraction technique for serum is described which is capable of an almost equal recovery (>93%) of adriamycin and metabolites without interference from endogenous components of plasma and from other common drugs. Within‐day and day to day coefficients of variation are estimate