Polymorphism in Sulfanilamide: 14N Nuclear Quadrupole Resonance Study

J Pharm Sci. 2019 Sep;108(9):2865-2870. doi: 10.1016/j.xphs.2019.05.015. Epub 2019 May 22.

Abstract

To demonstrate the selectivity of 14N nuclear quadrupole resonance (14N NQR) spectroscopy in chemistry and pharmacy, a study of sulfanilamide polymorphism was undertaken. We studied 3 known polymorphs of sulfanilamide by 14N NQR. We found at room temperature 2 sets of 3 14N NQR transition frequencies, corresponding to 2 different nitrogen sites in the crystal structure for each of 3 polymorphs. We measured the temperature dependence of all quadrupole frequencies ν+, ν-. In each set, only 1 of the 3 14N NQR frequencies is enough to characterize the polymorph. Spin-lattice relaxation time (T1) measurement is supplemental information. We also measured the transition temperature between polymorphs and estimated the ratio of polymorphs after thermal treatment of sample.

Keywords: NQR; drug polymorphism; sulfanilamide; temperature dependence of NQR frequencies.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chemistry, Pharmaceutical
  • Crystallization
  • Magnetic Resonance Spectroscopy
  • Nitrogen / chemistry
  • Sulfanilamide / chemistry*
  • Temperature

Substances

  • Sulfanilamide
  • Nitrogen