Faculty of Pharmaceutical Sciences, Toho University.
Chem Pharm Bull (Tokyo). 2022;70(2):182-186. doi: 10.1248/cpb.c21-00912.
Bromine K-edge X-ray absorption near-edge structure (XANES) spectroscopy analyses were used to evaluate the crystals of the active pharmaceutical ingredients, eletriptan hydrobromide, dextromethorphan hydrobromide and scopolamine hydrobromide salts and the solid dispersion of eletriptan hydrobromide. The crystals and the solid dispersion of the active pharmaceutical ingredient (API) salts could be discriminated based on the shape of the XANES spectra. The differences in the shape of XANES spectra was ascribable to the differences in the interatomic interactions of the bromine ions based on the crystal structures. Ratio of the eletriptan hydrobromide α-form crystal in mixed powders of α-form and monohydrate crystals could be quantified by the linear-combination fitting using their XANES spectra. These results indicated that the XANES spectroscopy are a potent method for evaluating the APIs of pharmaceutical formulations even at the higher energy region around the bromine K-edge of 13470 eV.
溴 K 边 X 射线吸收近边结构（XANES）光谱分析用于评估活性药物成分的晶体，如依托立坦氢溴酸盐、右美沙芬氢溴酸盐和莨菪碱氢溴酸盐盐以及依托立坦氢溴酸盐的固体分散体。基于 XANES 光谱的形状，可以区分活性药物成分（API）盐的晶体和固体分散体。XANES 光谱形状的差异归因于基于晶体结构的溴离子原子间相互作用的差异。通过使用 XANES 光谱对α 形式和一水合物晶体的混合物粉末进行线性组合拟合，可以定量确定混合粉末中依托立坦氢溴酸盐 α 形式晶体的比例。这些结果表明，即使在溴 K 边 13470eV 附近的较高能量区域，XANES 光谱也是评估药物制剂 API 的有效方法。
