- HPLC method for simultaneous analysis of ticagrelor and its organic impurities and identification of two major photodegradation products
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A simple, fast and sensitive analytical method by high-performance liquid chromatography (HPLC) was developed and validated for the simultaneous determination of ticagrelor and two synthesis impurities. The HPLC method was established using an Agilent 1200 Series equipment coupled to photodiode array detector (PDA) at 270?nm with a Zorbax Plus C8 column (150?×?4.6?mm, 5.0?μm), injection volume of 20?μL, and a constant temperature of 25?°C. The mobile phase consisted of acetonitrile: ammonium acetate 50?mM (57:43, v/v) and pH adjusted to 8.2 with ammonium hydroxide 6?M, at a flow rate of 0.7?mL/min. No interference peaks from excipients and diluent system indicated the specificity of the method. The calibration curves showed determination coefficients (r2)?>?0.99, calculated by linear regression. The limit of quantitation (LOQ) for impurities 1 and 2 were 2.0 and 0.2?μg/mL, respectively. Intra and interday relative standard deviations (RSDs) were ?2% for ticagrelor and ?6% for the impurities, proving the precision of the method. Besides, two mayor degradation products formed when sample solutions of ticagrelor were exposed to UVC radiation were elucidated and the mechanisms involved in the photolytic degradation of ticagrelor were proposed.
- Bueno, Lívia Maronesi,Manoel, Joanna Wittckind,Giordani, Camila Ferrazza Alves,Mendez, Andreas Sebastian Loureiro,Volpato, Nadia Maria,Schapoval, Elfrides Eva Scherman,Steppe, Martin,Garcia, Cássia Virginia
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- Synthesis of ticagrelor analogues belonging to 1,2,3-triazolo[4,5-d]pyrimidines and study of their antiplatelet and antibacterial activity
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Based on the recent observation that the antiplatelet agent ticagrelor and one of its metabolite exert bactericidal activity against gram-positive bacteria, a series of 1,2,3-triazolo[4,5-d]pyrimidines structurally related to ticagrelor were synthesized and examined as putative antiplatelet and antibacterial agents. The aim was to assess the possibility of dissociating the two biological properties and to find novel 1,2,3-triazolo[4,5-d]pyrimidines expressing antiplatelet activity and devoid of in vitro antibacterial activity. The new compounds synthesized were known metabolites of ticagrelor as well as structurally simplified analogues. Some of them were found to express antiplatelet activity and to lose the antibacterial activity, supporting the view that the two activities were not necessarily linked.
- Goffin, Eric,Jacques, Nicolas,Lancellotti, Patrizio,Musumeci, Lucia,Nchimi, Alain,Pirotte, Bernard,Oury, Cécile
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