INTERNATIONAL JOURNAL OF ADVANCE RESEARCH
IN MULTIDISCIPLINARY

The analytical characterisation of gastrointestinal tract (GIT)-based oral drug formulations presents several challenges because formulation excipients, modified-release technologies, pH-dependent drug behaviour and degradation processes can influence extraction, chromatographic separation and mass-spectrometric response. The present study describes the proposed development and validation of a sensitive and selective ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) procedure for the quantitative analysis of selected active pharmaceutical ingredients (APIs), related impurities and degradation products in GIT-based oral formulations. The analytical strategy incorporated sample-preparation optimisation, chromatographic screening, mass-spectrometric optimisation, matrix-effect assessment, forced degradation and analytical procedure validation. Reversed-phase UPLC was optimised using small-particle columns, while electrospray ionisation and multiple-reaction monitoring were investigated for selective MS/MS detection. Validation was designed around specificity/selectivity, range, accuracy, precision, lower-range performance and robustness, consistent with the current ICH Q2(R2) framework. ICH Q14 further supports a science- and risk-based approach to analytical procedure development, linking analytical performance to the intended purpose of the procedure. (ICH Database) The proposed procedure is expected to provide improved selectivity for complex oral formulations compared with single-wavelength UV detection and to support stability-indicating assessment through separation and detection of degradation-related components. The work provides a framework for application of UPLC-MS/MS in pharmaceutical quality control, impurity profiling and stability assessment of GIT-based dosage forms.