A stability-indicating HPLC method was developed to simultaneously determine cisatracurium besylate and propofol in mixtures. The effects of organic modifier, ionic strength and the pH of the mobile phase on resolution and retention were investigated. A baseline separation was achieved on an octadecylsilane column with an isocratic mobile phase of acetonitrile-ammonium formate (pH 5.2; 0.3 M) (50:50, v/v). Cisatracurium and propofol were confirmed by both retention time and mass-to-charge ratio using LC-MS. The degradation products of cistracurium were identified by ESI positive-ion detection as Hofmann elimination and ester hydrolysis products of cisatracurium. There were no propofol degradation products observed. The quantitation of the two drugs was accomplished using UV detection at 280 nm. This method showed linearity for cisatracurium besylate and propofol in the 9-128 and 37-592 micrograms ml-1 ranges, respectively. Accuracy and precision were in the 0.4-1.4 and 0.4-2.9% ranges respectively, for both analytes.