Abstract

The objective of current study was to develop a validated, specific stability indicating normal-phase high performance thin layer chromatographic method for simultaneous estimation of flupentixol and melitracen in their combined dosage form. The forced degradation studies were performed on pure flupentixol and melitracen and also on their combined dosage form using acid, base, neutral, oxidation, thermal and photo stress to show the stability indicating capability of the developed method. The chromatographic method was optimized using samples generated in forced degradation studies. Good separation between the peaks corresponding to the flupentixol and melitracen and degradation products from the analyte were achieved on silica gel 60F254TLC plate using toluene: chloroform: methanol: ammonia (4.5: 4.5: 1: 0.3 v/v) as mobile phase. Densitometric quantification was performed at 295 nm by reflectance scanning. The RF value of flupentixol and melitracen were 0.45 ± 0.03 and 0.65 ± 0.03 respectively. Validation of the developed method was conducted as per ICH requirements. Response were a linear function of concentration of flupentixol over the range 50-250 ng/band by peak area with correlation coefficient 0.98174 and losartan over the range 1000–5000 ng/band by peak area with correlation coefficient 0.99107. LOD values were found to be 2.95 and 5.48 ng/band by area for flupentixol and melitracen respectively. LOQ values were 8.95 and 16.62 ng/band by area for flupentixol and melitracen respectively. Results from analysis of a commercial tablet formulation were 100.38 ± 0.1959 % and 100.03 ± 0.3214 % by peak area for flupentixol and melitracen respectively. Recoveries were 99.16 ± 0.8177 % and 99.63 ± 0.9331 % by peak area for flupentixol and melitracen respectively. The conditions used also enabled separation and detection of degradation products from acidic, basic, oxidation stress. No degradation products of FLUP and MELI were obtained after neutral, photo and heat stress conditions applied on both drugs individually or in combination

Description