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(95ag) Understanding Phase Transition of Acetaminophen in the Bulk and Surface of Acetaminophen

Authors: 
Abouhakim, H., University of Leeds
Hassanpour, A., University of Leeds
Muller, F. L., University of Leeds
Schroeder, S., University of Leeds
Quayle, M., University of Leeds
Pharmaceutical solids processing often lead to the generation of new phases in the bulk and on the surface of the processed drugs. Phase transformation of the API can potentially change the physiochemical properties and influence the drug performances including solubility, dissolution and stability. To detect these changes, analytical tools such as XRD are usually employed. However, these techniques remain suitable for bulk analysis. Whereas, phase transition on the surface remains hard to detect due to the lack of literature, researches in this area and the absence of surface analytical techniques. The aim of this work is to investigate different phases (pure crystalline, partially crystalline partially amorphous and amorphous) of Acetaminophen drug by combining bulk and surface analytical techniques. For bulk analysis, FTIR and XRD have been employed. The former shows no significant differences between Acetaminophen various phases. Whereas the latter confirmed the presence of different phases indicated by a remarkable variation in the absorbance intensity the peak width. Where, high and sharp peaks obtained for the pure crystalline Acetaminophen, fewer peaks observed for semi crystalline Acetaminophen and a single broad peak observed for the amorphous Acetaminophen. For the surface analysis, Nitrogen K near-edge X-ray absorption fine structure (NEXAFS) spectra of a series of NEXAFS indicates that the precise determination of IPs and σ* shape resonance energies is sensitive enough to distinguish between the different phases of Acetaminophen. DFT calculations provides information on the molecular orbitals involved during electronic excitation occurred as a result of NEXAFS experiment.