title: Compatible validated spectrofluorimetric and spectrophotometric methods for determination of vildagliptin and saxagliptin by factorial design experiments.
abstract: 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.
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Abbassia, Cairo 11566, Egypt.
authors.forename: Omar
authors.initials: O
authors.lastname: Abdel-Aziz
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Abbassia, Cairo 11566, Egypt.
authors.forename: Miriam F
authors.initials: MF
authors.lastname: Ayad
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Ain Shams University, Abbassia, Cairo 11566, Egypt. Electronic address: mariam.tadros@hotmail.com.
authors.forename: Mariam M
authors.initials: MM
authors.lastname: Tadros
mesh_terms: D000218:Adamantane / Q000031:analogs & derivatives* / Q000032:analysis; D016227:Benzoquinones / Q000737:chemistry; D002703:Chloranil / Q000737:chemistry; D004151:Dipeptides / Q000032:analysis*; D054873:Dipeptidyl-Peptidase IV Inhibitors / Q000032:analysis*; D057230:Limit of Detection; D009570:Nitriles / Q000032:analysis*; D011759:Pyrrolidines / Q000032:analysis*; D013050:Spectrometry, Fluorescence / Q000379:methods; D013053:Spectrophotometry / Q000379:methods; D013607:Tablets; D000077597:Vildagliptin
chemical_list: D016227:Benzoquinones; D004151:Dipeptides; D054873:Dipeptidyl-Peptidase IV Inhibitors; D009570:Nitriles; D011759:Pyrrolidines; D013607:Tablets; D002703:Chloranil; C004532:quinone; C502994:saxagliptin; D000077597:Vildagliptin; D000218:Adamantane
keywords: Charge transfer reaction; Dansylation; Experimental design; Hantzsch reaction; Saxagliptin; Vildagliptin