A new sensitive method for rapid and accurate determination of benzocaine via hydroxamic acid formation is described. The solution of hydroxylamine hydrochloride is reacted with benzocaine in alkaline medium to give corresponding hydroxamic acid (II) which forms the purple coloured complex with FeCl3in acidic medium, having a maximum absorbance at 530 nm. The commonly present additives such as Tyrothricin, Propylene glycol, Glycerin do not show any interference except Quiniodochlor whose interference was eliminated by extracting it with alcohol and removal of waxy substances with a mixture of water and HCL (17.5 :2.5).