STABILITY INDICATING HPTLC METHOD FOR ESTIMATION OF BUDESONIDE AND FORMOTEROL FUMARATE DIHYDRATE IN PHARMACEUTICAL FORMULATION

Abstract

A sensitive, selective, precise and accurate stability-indicating high-performance thin layer chromatographic method for analysis of budesonide (BUD) and formoterol fumarate dihydrate (FFD) was developed along with forced degradation study and validated according to ICH guidelines. Densitometry analysis of BUD and FFD was carried out in the absorbance mode at 234 nm using toluene: methanol: ethyl acetate: ammonia (8:2:2.5:0.1,% V/V/V/V) as solvent system. This system was found to give compact spots for BUD at Rf value of 0.34 ± 0.06 and FFD at Rf value of 0.67± 0.05. It was found that besides oxidative, thermal and photo stability studies, acid and base induced degradation of drugs were more with resultant degradation product. 32 factorial design was used to predict base induced degradation. The drug undergoes degradation under mainly acidic and basic conditions. Also, the degraded products were well resolved from the pure drugs with significantly different Rf values. Linearity was found to be in the range of 1800-10600 and 1000-6000 ng band-1 for BUD and FFD, respectively. The LOQ for BUD and FFD were 392.48 ng band-1 and 1189.36 ng band-1 and LOD for BUD and FFD was115.79 ng band-1 and 350.88 ng band-1, respectively. ‘‘Bartlett’s test’’ applied on peak area for linearity, additionally proved validity of the developed method. Good accuracy and precision were obtained as revealed from percentage RSD value less than 2. Similarly, no interference was observed from common excipients in tablet formulation as well as degradation product, indicating specificity of the method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one.