Characterization and quantitation of clarithromycin polymorphs by powder X-ray diffractometry and solid-state NMR spectroscopy.
Characterization of clarithromycin polymorph was performed by solid-state cross polarization and magic angle spinning (CP/MAS) 13C-NMR spectroscopy. Two polymorphs, form II and form I, of clarithromycins indicated characteristic resonances of C1 carbonyl carbon at 176.2 and 175.2 ppm, respectively. Since each peak of C1 carbon was well separated in the spectrum of the two polymorphs, we performed quantitative analysis of the polymorphic fraction from the peak area of these peaks. The peak area of form I was found to linearly increase with an increase of its content, with a correlation coefficient of above 0.99. Solid-state NMR was found to be a useful technique to determine the characteristics of the polymorphic forms.
Graduate School of Pharmaceutical Sciences, Chiba University, Chiba, Japan. ytozuka@p.chiba-u.ac.jp
Yuichi
Y
Tozuka
Atsutoshi
A
Ito
Hiroko
H
Seki
Toshio
T
Oguchi
Keiji
K
Yamamoto
D017291:Clarithromycin / Q000032:analysis* / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods; D033362:Powder Diffraction / Q000379:methods*; D014961:X-Ray Diffraction / Q000379:methods
D017291:Clarithromycin