Investigation of forced and total degradation products of amlodipine besylate by liquid chromatography and liquid chromatography-mass spectrometry

• Published in: Chemical Industry and Chemical Engineering Quarterly 2014-01, Vol.20 (2), p.295-304
• Main Authors: Stoiljkovic, Zora, Jadranin, Milka, Djuric, Svetlana, Petrovic, Slobodan, Ivic, Avramov, Mijin, Dusan
• Format: Article
• Language: English
• Subjects: amlodipine besylate; forced degradation; liquid chromatography-mass spectrometry; reversed phase liquid chromatography
• ISSN: 1451-9372; 2217-7434
• DOI: 10.2298/CICEQ121226011S

An isocratic, reversed-phase liquid chromatographic method was applied for the investigation of the degradation products of amlodipine besylate under the stressed conditions in solution. Amlodipine besylate stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation and photodegradation as well as to the electrochemical degradation by cyclic voltammetry in 0.05 mol/L NaHCO3 on gold electrode. The total degradation of amlodipine besylate was achieved in 5 mol/L NaOH at 80?C for 6 h and the compound with molecular formula C15H16NOCl was identified as a main degradation product. Under acidic (5 mol/L HCl at 80?C for 6 h) stress conditions 75.2% of amlodipine besylate degradation was recorded. Oxidative degradation in the solution of 3% H2O2-methanol 80:20 at 80?C for 6 h showed that amlodipine besylate degraded to 80.1%. After 14 days of expose in photostability chamber amlodipine besylate solution showed degradation of 32.2%. In electrochemical degradation after 9 hours of cyclization the beginning of amlodipine oxidation was shifted for 200 mV to more negative potentials, with the degradation of 66.5%. Mass spectrometry analysis confirmed the presence of dehydro amlodipine derivate with molecular formula C20H23N2O5Cl in oxidative and acidic conditions while in electrochemical degradation was detected in traces.