A new method is developed using PMR for the assay of chloramphenicol and its pharmaceutical forms. The method is rapid, accurate, precise and helps in confirming the identity and purity of the drug. The principle of the method involves comparing the integral of the well-defined doublet system of chloramphenicol spectrum (positioned at 7.6 δ and 7.5 δ) to that of the sharp singlet (positioned at 6.25 δ) of maleic acid which is used as internal standard.