Vibrational spectroscopic characterisation of salmeterol xinafoate polymorphs and a preliminary investigation of their transformation using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry.
Knowledge and control of the polymorphic phases of chemical compounds are important aspects of drug development in the pharmaceutical industry. Salmeterol xinafoate, a long acting beta-adrenergic receptor agonist, exists in two polymorphic Forms, I and II. Raman and near infrared spectra were obtained of these polymorphs at selected wavelengths in the range of 488-1064 nm; significant differences in the Raman and near-infrared spectra were apparent and key spectral marker bands have been identified for the vibrational spectroscopic characterisation of the individual polymorphs which were also characterised with X ray diffractometry. The solid-state transition of salmeterol xinafoate polymorphs was studied using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry isothermally between transitions. This method assisted in the unambiguous characterisation of the two polymorphic forms by providing a simultaneous probe of both the thermal and vibrational data. The study demonstrates the value of a rapid in situ analysis of a drug polymorph which can be of potential value for at-line in-process control.
Chemical & Forensic Sciences, University Analytical Centre, School of Life Sciences, University of Bradford, Richmond Road, Bradford BD7 1DP, UK.
Hassan Refat H
HR
Ali
Howell G M
HG
Edwards
Michael D
MD
Hargreaves
Tasnim
T
Munshi
Ian J
IJ
Scowen
Richard J
RJ
Telford
D000420:Albuterol / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D002152:Calorimetry, Differential Scanning / Q000379:methods*; D015394:Molecular Structure; D000068299:Salmeterol Xinafoate; D013055:Spectrophotometry, Infrared; D013059:Spectrum Analysis, Raman / Q000379:methods*; D013696:Temperature; D014732:Vibration; D014961:X-Ray Diffraction
D000068299:Salmeterol Xinafoate; D000420:Albuterol