title: A degradation study of cefepime hydrochloride in solutions under various stress conditions by TLC-densitometry.
abstract: A rapid, accurate and sensitive thin-layer chromatography (TLC) method with densitometric detection has been developed and validated for the determination of cefepime in pharmaceuticals. Chromatographic separation was achieved on a silica gel TLC F254 plates with a mobile phase consisting of ethanol-2-propanol-glacial acetic acid 99.5%-water (4:4:1:3, v/v). Densitometric detection was carried out at wavelength of 266 nm in reflectance/absorbance mode. The validation of the method was found to be satisfactory with high accuracy (from 99.24 to 101.37%) and precision (RSD from 0.06 to 0.36%). Additionally, the stability of cefepime in solution was investigated, including the effect of pH, temperature and incubation time. Favorable retention parameters (Rf , Rs, α) were obtained under the developed conditions, which guaranteed good separation of the studied components. The degradation process of cefepime hydrochloride was described by kinetic and thermodynamic parameters (k, t0.1 , t0.5 and Ea ). Moreover, the chemical properties of degradation products were characterized by the Rf values, absorption spectra, HPLC-MS/MS and TLC-densitometry analysis. As the method could effectively separate the active substance from its main degradation product (1-methylpyrrolidine), it can be employed as a method to indicate the stability of this drug.
authors.affiliation: Department of Inorganic and Analytical Chemistry, Faculty of Pharmacy, Collegium Medicum, Jagiellonian University, 9 Medyczna Str, 30-688, Kraków, Poland.
authors.forename: Monika
authors.initials: M
authors.lastname: Dąbrowska
authors.forename: Małgorzata
authors.initials: M
authors.lastname: Starek
authors.forename: Jan
authors.initials: J
authors.lastname: Krzek
authors.forename: Elżbieta
authors.initials: E
authors.lastname: Papp
authors.forename: Piotr
authors.initials: P
authors.lastname: Król
mesh_terms: D000077723:Cefepime; D002511:Cephalosporins / Q000032:analysis* / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D002855:Chromatography, Thin Layer / Q000379:methods*; D003720:Densitometry / Q000379:methods*; D004355:Drug Stability; D006863:Hydrogen-Ion Concentration; D007700:Kinetics; D057230:Limit of Detection; D011759:Pyrrolidines / Q000032:analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012996:Solutions; D053719:Tandem Mass Spectrometry; D013696:Temperature; D013816:Thermodynamics
chemical_list: D002511:Cephalosporins; D011759:Pyrrolidines; D012996:Solutions; C054965:N-methylpyrrolidine; D000077723:Cefepime
keywords: cefepime hydrochloride; degradation process; densitometric detection; thin-layer chromatography