A simple and sensitive electrochemical method has been developed for the determination of acetyl salicylic acid (ASA) and caffeine (CAF) using edge plane pyrolytic graphite electrode (EPPGE). At pH 7.2, two well defined peaks with peak potential (E(p)) of similar to 1225 mV and similar to 1335 mV were appeared for the oxidation of ASA and CAF, respectively. Anodic peaks for ASA and CAF showed a systematic increase in peak current with increase in concentration in the range 0.02-100 mu M with sensitivity of 0.16 and 0.17 mu A/mu M, respectively. Detection limits (3 sigma/slope) for ASA and CAF were found to be 0.01 and 0.008 mu M, respectively whereas, the limit of quantifications were found to be 0.032 and 0.026 mu M, respectively. The proposed sensor has been utilized for the simultaneous determination of ASP and CAF in human urine samples, pharmaceutical preparations and coffee beverages. (C) 2011 Elsevier B.V. All rights reserved.