Author: Venkata Sai Suresh Kumar Sista, Anjali Jha, V. L. H. HaranA. and G.V. S. Prasad

DOI: http://doi.org/10.31788/RJC.2026.1919472

This research outlines the development and validation of a reliable analytical method for determining residual solvents—methanol, acetone, dichloromethane (DCM), and toluene—in Sunitinib Cyclamate, a newsalt formof theanticancer drug Sunitinib. This method employs headspace gas chromatography (GC-HS), a precise and efficient technique for analysing volatile organic impurities. Validation followed ICH Q2(R1) guidelines, covering essential parameters such as specificity, accuracy, precision, linearity, range, robustness, ruggedness, and solution stability. The results demonstrated excellent specificity, with no interference from the drug matrix or excipients. Systemsuitability parameters, including resolution and %RSD, consistently satisfied the acceptance limits. The methodshowed high precision (%RSD < 2%), satisfactory recovery (85–115%), and strong linearity (R² ≥ 0.996) across thetested concentration range. Moreover, the procedure-maintained robustness under intentional variations in analytical conditions and showed consistent ruggedness among different analysts and instruments. Overall, the validatedGC- HS method provides a sensitive, accurate, and regulatory-compliant approach for residual solvent determinationinSunitinib Cyclamate, supporting its dependable use in routine quality control and pharmaceutical batch release.

Keywords: Gas Chromatography-Headspace (GC-HS), Residual Solvents, Sunitinib Cyclamate, Method Validation, ICH Q2(R1), Pharmaceutical Analysis.