Podili, Bhavani  <br/><br/>
Simple reversed phase high performance liquid chromatography method for the estimation of related substances, assay of cabozantinib and nivolumab and its application to issolution studies 

 - Vol.83(4), July-Aug 
 - Mumbai  Indian Journal of Pharmaceutical Science  2021 
 - 701-713p. 
<br/><br/> The present work describes the development and subsequent validation of a novel, simple, selective and<br/>stability indicating gradient reversed phase high performance liquid chromatography method for the<br/>quantitative determination of related substances, assay of cabozantinib and nivolumab and its application<br/>to dissolution studies. The chromatographic method was optimized using the impurity-spiked solution.<br/>A good resolution between the peaks was achieved under selected chromatographic conditions. The<br/>separation was accomplished on an X-Bridge C18, 150×4.6 mm, 3.5 μ column connected to a photo diode<br/>array detector using 0.1 % orthophosphoric acid in water as mobile phase A and acetonitrile as mobile<br/>phase B, under gradient elution. The mobile phase flow rate was maintained at 1.0 ml/min. The detection<br/>of the constituents was done at 216 nm using a ultra-violet detector. Recovery studies were satisfactory<br/>and the correlation coefficient for two active pharmaceutical ingredients and their related substances,<br/>0.999 indicates the linearity of the method within the limits. Limit of detection and limit of quantification<br/>for all impurities and cabozantinib and nivolumab were established with respect to the test concentration.<br/>Specificity, accuracy, precision, ruggedness and robustness were determined as part of the method<br/>validation. The performance of the method was validated according to the current International Council<br/>for Harmonisation requirements. Moreover, the dissolution study was performed on active pharmaceutical<br/>ingredients to estimate the recovery using the same method. Validation of the developed reversed phase<br/>high performance liquid chromatography procedure revealed that all the degradation products formed<br/>during stress conditions and related impurities were well separated from their active pharmaceutical<br/>ingredients and peaks were well resolved from each other with appropriate retention time. The method<br/>was characterized by good linearity, specificity, low values of limit of detection and quantisation, accuracy,<br/>precision, ruggedness and robustness. All statistical results were within the acceptance criteria and the<br/>proposed method is simple, fast, accurate, precise and reproducible. Hence, it can be applied for routine<br/>dissolution analysis and employed for quality control of drug samples during stability studies. 
<br/><br/><label>Subjects--Topical Terms: </label><br/>PHARMACEUTICS