A simple, precise, accurate and rapid Reverse phase liquid chromatographic method has been developed and validated for the analysis of Terbutaline and Guaiphenesin in Bulk as well as in Tablet dosage form. The analysis was carried out using Hexon C18 (250mm x 4.6ID, Particle size: 5 micron) column with UV-3000-M Detector by using the Gradient system. The mobile phase used was Methanol and Water in the ratio of 60:40 containing phosphate buffer adjusted with pH 3 was pumped at a flow rate of 0.8 ml/min with UV-detection at 275 nm. The retention time for Terbutaline and Guaiphenesin was found to be 2.278 and 4.414 minutes respectively. The method has been validated in accordance with the ICH guidelines such as Linearity, Accuracy, Precision, LOD, LOQ, and Robustness. The method was found to be linear over a concentration range of 1-5μg/ml and 40-200μg/ml with R2 value 0.994 and 0.998 for Terbutaline and Guaiphenesin Respectively. The present work shows that this RP-HPLC method is useful for the routine analysis of Terbutaline and Guaiphenesin in bulk as well as its Tablet dosage form.