A simple and sensitive method for the determination of methylene chloride as residual solvent was developed and validated on gas liquid chromatograph fitted with flame ionization detector. The carrier gas was nitrogen, and separation was carried out on BP 5 capillary column consisting of 5% phenyl and 95% dimethyl polysiloxane stationary phase. The retention time for methylene chloride was 5.4 min. The method was extended for determination of the methylene chloride organic volatile impurity in the marketed formulations of ciprofloxacin hydrochloride, norfloxacin, pefloxacin and ofloxacin.