title: Analytical Stability-Indicating Methods for Alogliptin in Tablets by LC-CAD and LC-UV.
abstract: Stability-indicating LC methods using a UV detector and a charged aerosol detector (CAD) simultaneously were validated for the assessment of alogliptin (ALG) in tablets. The analysis was performed on a C8 column (250 × 4.6 mm, 5 μm) at a flow of 0.8 mL/min, using acetonitrile-10 mM ammonium acetate buffer (pH 3.5; 90 + 10, v/v) as mobile phase and UV detection at 275 nm. Validation followed the International Conference on Harmonization guidelines. The method was linear over the range of 25-200 μg/mL. Normality of the residuals showed a normal distribution, no autocorrelation, and homoscedasticity. LODs were 6.25 and 2.65 µg/mL and LOQs were 20.85 and 8.84 µg/mL for the CAD and the UV detector, respectively. The methods were precise and accurate. Excipients and degradation products did not interfere in the methods in studies of specificity. None of the factors studied in the analysis of robustness had a significant effect on the quantification of the ALG by the Pareto chart. The results of the assay obtained with LC-CAD and LC-UV were similar. The methods could be considered interchangeable and stability-indicating, and can be applied as an appropriate QC tool for analysis of ALG in tablets.
authors.affiliation: Universidade Federal do Rio Grande do Sul, Faculdade de Farmácia, Laboratório de Produção de Substâncias Químicas de Referência, Ave Ipiranga No. 2752, CEP 90610-000, Porto Alegre/RS, Brazil.
authors.forename: Charise Dallazem
authors.initials: CD
authors.lastname: Bertol
authors.affiliation: Universidade de Passo Fundo, Centro de Pesquisa em Alimentação, Laboratório de Cromatografia, Campus I, Km 292, BR 285, Bairro São José, CEP 99052-900, Passo Fundo/RS, Brazil.
authors.forename: Maria Tereza
authors.initials: MT
authors.lastname: Friedrich
authors.affiliation: Universidade Federal do Rio Grande do Sul, Faculdade de Farmácia, Laboratório de Produção de Substâncias Químicas de Referência, Ave Ipiranga No. 2752, CEP 90610-000, Porto Alegre/RS, Brazil.
authors.forename: Graciela
authors.initials: G
authors.lastname: Carlos
authors.affiliation: Universidade Federal do Rio Grande do Sul, Faculdade de Farmácia, Laboratório de Produção de Substâncias Químicas de Referência, Ave Ipiranga No. 2752, CEP 90610-000, Porto Alegre/RS, Brazil.
authors.forename: Pedro Eduardo
authors.initials: PE
authors.lastname: Froehlich
mesh_terms: D019817:Benzoic Acid / Q000032:analysis; D002853:Chromatography, Liquid; D004355:Drug Stability; D005079:Excipients / Q000032:analysis; D057230:Limit of Detection; D008353:Mannitol / Q000032:analysis; D010880:Piperidines / Q000008:administration & dosage / Q000032:analysis*; D013607:Tablets; D014498:Uracil / Q000008:administration & dosage / Q000031:analogs & derivatives* / Q000032:analysis
chemical_list: D005079:Excipients; D010880:Piperidines; D013607:Tablets; D008353:Mannitol; D014498:Uracil; D019817:Benzoic Acid; C520853:alogliptin