Plackett–Burman and face-centered composite designs for development and optimization of chromatographic method for the simultaneous determination of glycopyrronium, indacaterol and mometasone in their fixed dose combination inhaler – Green profile assessment

• Published in: Journal of pharmaceutical and biomedical analysis 2023-09, Vol.234, p.115553-115553, Article 115553
• Main Authors: Youssef, Yasmin M., Mahrouse, Marianne A., Mostafa, Eman A.
• Format: Article
• Language: English
• Subjects: Face-centered composite; Glycopyrronium bromide; Indacaterol acetate; Mometasone furoate; Plackett–Burman; RP-HPLC/UV
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2023.115553

A novel simple, specific, sensitive, accurate and precise reversed phase high performance liquid chromatographic method (RP-HPLC/UV) was developed and validated for the simultaneous estimation of Glycopyrronium bromide (GLY), Indacaterol acetate (IND) and Mometasone furoate (MOF) in pure form, in laboratory prepared mixtures and in pharmaceutical dosage form. Experimental design methodology was applied by using Plackett–Burman and face-centered composite designs to achieve the best resolution with minimum experimental trials. The designed model was statistically analyzed, graphically presented by surface plots and the relationships between coefficients of the derived polynomial equations were interpreted. Chromatographic separation was achieved on Inertsil ODS C18 column (250 ×4.6 mm, 5 µm) at ambient temperature using a mobile phase composed of methanol: 0.1% glacial acetic acid (pH4) in a gradient elution at a flow rate 1 mL /min. UV detection was carried out at 233 nm. Response was found to be linear in the concentration range of 20–120 µg /mL with regression coefficient (r2 = 0.999) for GLY, 50–300 µg /mL with regression coefficient (r2 = 0.9995) for IND and 50–300 µg /mL with regression coefficient (r2 = 0.9998) for MOF. The method was validated as per ICH guidelines and satisfactory results were achieved. The method was successfully applied for the analysis of the cited drugs in their fixed dose combination (FDC) pharmaceutical formulation. Statistical comparison between the results obtained by the proposed method and the reference methods for GLY, IND and MOF showed no significant difference. The developed method could be implemented in quality control aspects of the cited drugs. Four green metrics were used to evaluate the new RP-HPLC/UV method's greenness and compare it to other published techniques. [Display omitted] •RP-HPLC/UV for estimation of Glycopyrronium, Indacaterol & Mometasone in inhaler.•Experimental designs applied using Plackett–Burman & face-centered composite designs.•The proposed method was fully validated according to ICH guidelines.•The proposed method recorded highest AGREE & ESA scores among compared methods.