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An accurate, simple, reproducible, and sensible liquid chromatographic method was developed and validated for the determination of chlorpheniramine maleate and dexamethasone in a tablet formulation. The analysis was performed at room temperature on a reversed-phase C18 column with UV detection at 254 nm. The mobile phase consisted of 7.5 mM monobasic potassium phosphate in methanol–water (62.5 + 37.5) at a constant flow rate of 1 mL/min. The method was validated in terms of linearity, precision, accuracy, and specificity by forced decomposition of chlorpheniramine maleate and dexamethasone initiated by using acid, base, water, hydrogen peroxide, heat, and light. The response was linear in the ranges of 0.04–0.12 and 0.006–0.016 mg/mL for chlorpheniramine maleate (r2 = 0.9999) and dexamethasone (r2 = 0.9994), respectively. The relative standard deviation values for intra- and interday precision studies were 2.39 and 2.02, respectively, for chlorpheniramine maleate and 2.39 and 1.25, respectively, for dexamethasone. Recoveries ranged from 95.07 to 101.95% for chlorpheniramine maleate and from 97.75 to 102.10% for dexamethasone.

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