A new method, involving the application of PMR spectrometry for the assay of chlorpropamide and its tablets, is proposed. The PMR spectrum of chlorpropamide has a well-defined triplet (around 0.8 ppm) and quartet (near 7.8 ppm), which are chosen for quantitative analysis. The method is based on comapring the integral of these signals to that of the sharp singlet of maleic acid at 6.3 ppm which is used as internal standard. The proposed method is simple and rapid, also it gives accurate and reproducible results when applied for the analysis of both authentic chlorproparaide and its tablets. In addition, the PMR spectrum obtained helps in confirming identity and purity of the drug.