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Degradation of the active pharmaceutical ingredient canagliflozin using electrochemical oxidation
Bolíková, Markéta ; Křížek, Tomáš (advisor) ; Kozlík, Petr (referee)
This bachelor thesis is aimed at degradation of the active pharmaceutical ingredient canagliflozin by the electrochemical oxidation. The aim is to explore the influence of given measurement conditions on the course and the results of the electrochemical oxidation and to find out, under which conditions the largest percentage of the degradation products is formed. These conditions are, for example, the concentrations and pH values of the buffers which are used to dissolve the samples of canagliflozin, the flow rate of the electrochemically stressed substance solution through the flow cell or the thickness of the gasket inserted in front of the working electrode. Canagliflozin is an orally administered blood glucose lowering antidiabetic and is used to treat diabetes mellitus 2. type. It is one of the inhibitors of the sodium-glucose transporter type 2. For the separation of the degradation products of this pharmaceutically active substance, a high performance liquid chromatography (HPLC) method with a UV/VIS diode array detector using an Agilent Poroshell 120 SB-Aq chromatographic column (2.1 × 100 mm; 2.7 µm) was chosen. The mobile phase contained an aqueous component, which was 10 mM formate buffer with pH 3.5 and the organic component, which was acetonitrile. The electrochemical oxidation of...
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Forced degradation study of canagliflozin with the use of HPLC
Máchalová, Jitka ; Křížek, Tomáš (advisor) ; Sobotníková, Jana (referee)
In this work a method for determination of canagliflozin and its degradation products by HPLC with UV and MS detector was developed. The developed method was used to study the forced degradation of canagliflozin and to investigate the major degradation products resulting from exposure of canagliflozin to oxidative stress. Canagliflozin is a phenolic glycoside derivative and a glucose-sodium transporter 2 inhibitor that stimulates urinary glucose excretion by suppressing glucose reabsorption from the proximal tubule in the kidneys. Canagliflozin is used to control blood glucose levels in patients with type 2 diabetes. In an optimized method, an Agilent Poroshell 120 SB-Aq (2.1 × 100 mm, 2.7 µm) column was used and a mixture of buffer (10mM HCOOH adjusted with ammonium hydroxide to pH 3.5) and acetonitrile as a mobile phase. The method validation included testing of accuracy, repeatability, the limit of detection and quantification, linearity and linear dynamic range, the robustness of the method, and testing of sample stability. The limit of detection of the method was 8.9·10-5 mg ml-1 (2.0·10-7 mol l-1 ) and the limit of quantification was 3.0·10-4 mg ml-1 (6.8·10-7 mol l-1 ). At a concentration of 0.3 mg ml-1 , the repeatability (n = 7) was 0.17 % and 0.75 % for the retention time and the peak...
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