Thin Layer Chromatography‒spectrodensitometric Determination of a Three-Component Mixture of Propyphenazone, Caffeine, Ergotamine Tartrate, and Two of Their Impurities with Application to Tablets, Spiked Human Plasma, and Green Profile Assessment

A novel, green, and cost-effective thin-layer chromatography (TLC)‒spectrodensitometric method was designed and validated for the simultaneous determination of a five-component mixture. The analyzed mixture is composed of three active ingredients: propyphenazone (PRO), caffeine (CAF), and ergotamine tartrate (ERG), along with two official impurities which are PRO impurity: phenazone (PHN) and CAF impurity: theophylline (THEO). The suggested method was used for the quantitation of the three coformulated active ingredients in their marketed tablet and in human plasma. The studied compounds were separated on TLC silica gel 60F 254 plates using a mobile phase consisting of methanol–ethyl acetate–glacial acetic acid (1:9:0.1, V/V ) with diprophylline (DPP) as internal standard. Densitometric scanning was carried out at 210.0 nm. Method validation was assessed according to the International Council for Harmonisation (ICH) guidelines. The greenness profile for the proposed method was evaluated using the National Environmental Method Index (NEMI), analytical eco-scale, and Green Analytical Procedure Index (GAPI) tools. The proposed method offers the advantages of being simple, rapid, economic, and ecofriendly. It is a successful choice for the routine analysis of the studied drugs in pharmaceutical and biological samples.