Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 2015-04-05

Compatible validated spectrofluorimetric and spectrophotometric methods for determination of vildagliptin and saxagliptin by factorial design experiments.

Omar Abdel-Aziz, Miriam F Ayad, Mariam M Tadros

文献索引：Spectrochim. Acta. A. Mol. Biomol. Spectrosc. 140 , 229-40, (2015)

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摘要

Simple, selective and reproducible spectrofluorimetric and spectrophotometric methods have been developed for the determination of vildagliptin and saxagliptin in bulk and their pharmaceutical dosage forms. The first proposed spectrofluorimetric method is based on the dansylation reaction of the amino group of vildagliptin with dansyl chloride to form a highly fluorescent product. The formed product was measured spectrofluorimetrically at 455 nm after excitation at 345 nm. Beer's law was obeyed in a concentration range of 100-600 μg ml(-1). The second proposed spectrophotometric method is based on the charge transfer complex of saxagliptin with tetrachloro-1,4-benzoquinone (p-chloranil). The formed charge transfer complex was measured spectrophotometrically at 530 nm. Beer's law was obeyed in a concentration range of 100-850 μg ml(-1). The third proposed spectrophotometric method is based on the condensation reaction of the primary amino group of saxagliptin with formaldehyde and acetyl acetone to form a yellow colored product known as Hantzsch reaction, measured at 342.5 nm. Beer's law was obeyed in a concentration range of 50-300 μg ml(-1). All the variables were studied to optimize the reactions' conditions using factorial design. The developed methods were validated and proved to be specific and accurate for quality control of vildagliptin and saxagliptin in their pharmaceutical dosage forms.Copyright © 2015. Published by Elsevier B.V.