ICH Q14 Inspired-Qbd Mediated Development and Validation of Innovative Stability- Indicating HPLC Method For Estimating Melatonin From Sleep-Enhancing Tablet Formulation.

This research investigates the implementation of the recently published ICH Q14 guidance in the development of an AQbD-based HPLC method for the quantification of Melatonin in sleep-enhancing tablet formulations. An advanced Quality by Design (QbD) approach was employed, systematically examining each component of the process. Initial evaluations led to the identification of basic Analytical Target Product Profiles (ATPPs) and Quality Target Product Profiles (QTPPs). Subsequently, a risk assessment was conducted to determine the Critical Method Parameters (CMPs) and Critical Performance Attributes (CPAs). This was followed by a Design of Experiments (DOE) study utilizing an innovative mixed design to derive the Method Operating Design Region (MODR). The control strategy was defined by establishing limits within the system suitability parameters. Potential risk factors were thoroughly examined during the validation process. The developed method demonstrated rapid performance (with a run time of 10 minutes), high sensitivity (exhibiting broad linearity), and accuracy, as confirmed by recovery studies of Melatonin at three different concentration levels, all of which fell within acceptable limits. The method's stability-indicating capability was validated through forced degradation studies, establishing peak purity criteria using Empower software. In nutshell, the research successfully developed an efficient HPLC method for Melatonin, providing valuable insights into the variables affecting method performance. This method is proposed for use in quality control laboratories for routine and stability testing.