AbstractA sensitive, selective, precise and stability‐indicating thin‐layer chromatographic (TLC) method was developed and validated for the analysis of noscapine, both as a bulk drug and in its formulation. The method employed TLC aluminium plates precoated with silica gel 60F‐254 as the stationary phase. The solvent system consisted of chloroform‐methanol (10:0.5 v/v). Densitometric analysis of noscapine and its degradation products was carried out in the absorbance mode at 254 nm. This system was found to give compact symmetrical spots for noscapine (Rf value 0.85 ± 0.04). Noscapine was subjected to acid and alkali hydrolysis, oxidation and photo degradation.The drug undergoes photo degradation and also degrades under acidic and basic conditions. The prepared degradation products were identified and verified through infrared (IR) and mass spectral analyses. The degraded products were also well resolved from the pure drug with significantly different Rf values and they were quantitatively determined. The method was validated for linearity, precision, robustness, limit of detection (LOD), limit of quantitation (LOQ), specificity and accuracy. Linearity was found to be in the 1.0–10.0 µg, 0.4–3.2 µg, 1.0–9.0 µg and 0.5–5.0 µg/band ranges for noscapine, cotarnine, meconine and opionic acid, respectively. The polynomial regression analysis for the calibration plots showed a good polynomial relationship with r2 of 0.9998, 9989, 9996 and 0.9997 for noscapine and its three degradation products, cotarnine, meconine and opionic acid, respectively. Statistical analysis proves that the method is repeatable and specific for the estimation of noscapine. As this approach could effectively separate the drug from its degradation products it can be employed as a stability‐indicating method in Quality Control laboratories. Copyright © 2009 John Wiley & Sons, Ltd.