Organic volatile impurities by Headspace GC method was developed and validated for Diphenoxylate hydrochloride bulk drug for its seven residual solvents. Analysis was performed on Perkin Elmer HS 40 system with auto injector. Carrier gas Helium was used with constant flow rate of 2.5mL/min as carrier gas and the separation of residual solvents were achieved on DB-5 column. The thermostat temperature was 125 °C for 20 minute for each vial and after the equilibration the vials were pressurized and injected on GC column. FID detector was used for detection. The parameter for which the method was validated included specificity, limit of detection and quantification, linearity, precision, accuracy and robustness. The method was successfully used to quantify the levels of specified limit for residual solvents in Diphenoxylate hydrochloride bulk drug.