The titled paper discloses a novel methodology for study and analysis of active pharmaceutical ingredients extracted using the High-Performance Liquid Chromatography techniques. Performance of the proposed novel method is evaluated by targeting the one of the active pharmaceutical ingredients Zipracidone HCl which is used to treat the psychotic disorders like schizophrenia, mania, or bipolar disorder and other similar diseases. The process is carried out through early-stage chromatography preparations, sample solution preparations, linearity preparations, accuracy level preparation and Robustness assessment. The experimental results show 99.73% (as such basis) functional activity of drug and 99.97% (on anhydrous basis) functional activity with average accuracy of 99.57% (as such basis) and 99.88 (on anhydrous basis). Other outcomes are disclosed through the result and discussion section.