E0021

Solid State Characterization by HR-XRPD and NMR sSpectroscopy of Enantiomeric Drug R(-)-Albuterol Sulfate. S.L. Cuffini¹, M. Palacio¹, C. Ferrayoli¹, S. Palacios¹, S. Pagola², J. Schneider³ and P.W. Stephens², ¹CEPROCOR-Agencia Córdoba Ciencia, Argentine, ²Dept. of Physics and Astronomy, SUNY Stony Brook, NY 11974 USA, ³IFSC, Univ. de São Paulo, São Carlos, S.P., Brasil.

Racemic albuterol (salbutamol) is composed of an equimolar mixture of stereoisomers used for asthma therapy (1). R-albuterol should have advantages over racemic albuterol in this therapy and it is important to obtain the drug in pure form. The aim of this work is to show the solid state characterization of the crystallization process from racemic compound up to one enantiomer (R) and determination of the crystal structure of R-albuterol by High resolution X-ray powder diffraction (HR-XRPD) using Synchrotron Radiation and NMR spectroscopy. HR-XRPD data were collected at room temperature at the SUNY X3B1 beamline, N.S.L.S. (BNL). The structure solution of R-Albuterol was obtained by molecular location using the program PSSP (Powder Structure Solution Program) (2). High-resolution solid-state ¹³C NMR measurements were carried out in a Varian Unity INOVA spectrometer at 9.4T. Crystallographic data of (R)-Albuterol obtained by HR-XRPD are, a = 28.0872(18) b = 6.1464(4) c = 16.5095(11), α = 90, β = 95.558(4), γ = 90, with monoclinic system and space group C2, presenting two non-equivalent molecule per cell. The ¹³C NMR lines were assigned using literature information (3) and comparing the CP and non-protonated spectra. Lines from C1, C3/C5, C10 and methyl groups are clearly split, indicating the presence two non-equivalent molecules. The combination of solid-state NMR spectroscopy and HR-XRPD provide a complete solid characterization of this type of drugs.