A Proton Nuclear Magnetic Resonance Method for Quantitative Analysis of Ticagrelor

Abstract

A novel proton nuclear magnetic resonance (1H NMR) method for determining the absolute content of ticagrelor was proposed. The ideal spectra were obtained on a Bruker Avance-300 spectrometer with deuterated methanol (CD3OD) as the solvent and sulfadoxin as the internal standard. The ticagrelor signals at δH 7.14 (2H, m) and δH 7.04 (1H, s), as well as those of sulfadoxin at δH 8.04 (1H, s), δH 7.73 (2H, d) and δH 6.54 (2H, d), were selected for quantitative analysis. The detection conditions were as following:probe temperature 308 K, spectrum width 3 511.5 Hz, center frequency 1 470.6 Hz, pulse angle θ=30°, delay time (d1) 10 s, number of scans 16 and line broadening 0.3 Hz. The signals from ticagrelor and internal standard sulfadoxin showed good separation, precision, reproducibility, and wide linearity ranges with Y=1.053X-0.081 (r=0.996, n=5). The content of ticagrelor was estimated to be 99.4% (RSD=0.20%). This method was proven simple, accurate and rapid.

Keywords

• proton nuclear magnetic resonance (1h nmr)
• ticagrelor
• content determination