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目的:分析白矾、枯矾及其伪品的X射线衍射(X-ray diffraction,XRD),拉曼和近红外(Near Infrared,NIR)光谱特征与差异,建立快速鉴别白矾、枯矾和常见伪品的新方法。方法:从不同药材市场购得白矾9批,枯矾5批,自制枯矾2批。采集以上样品的XRD,NIR和拉曼光谱,归纳其光谱特征,分析光谱明显差异。结果:明矾和其伪品铵明矾的XRD,NIR及拉曼光谱具有明显差异。在XRD图谱中,铵明矾在2θ=14.56°处有1小峰,正品白矾没有此峰;在NIR光谱中,铵明矾在4 650 cm~(-1)处有1特征峰,而正品白矾无此峰;在拉曼光谱中,正品白矾在990 cm~(-1)处的最强峰发生分裂,974 cm~(-1)处产生1中等强度尖峰,而铵明矾无974 cm~(-1)峰,以上差异可用于二者快速鉴别。此外,正品枯矾XRD图谱具有9个明显特征峰(2θ=11.18°,21.88°,24.58°,31.42°,33.76°,38.25°,39.94°,50.24°,50.99°),NIR光谱在7 000 cm~(-1)和5 150 cm~(-1)处有2个较为平缓的吸收峰,可作为鉴别枯矾真伪的特征峰。结论:XRD,NIR和拉曼光谱特征可共同用于白矾、枯矾及其伪品的准确鉴别;NIR结合拉曼光谱技术能够为白矾及其炮制品的质控和快检提供快速准确的新方法。
OBJECTIVE: To analyze the characteristics and differences of X-ray diffraction (XRD), Raman and near infrared (NIR) spectrum of alum, alum and their counterfeit products and to establish a rapid identification of alum, alum and common pseudo New method of product. Methods: 9 batches of alum, 5 batches of alum, and 2 batches of self-made alum were purchased from different medicinal markets. The above samples were collected by XRD, NIR and Raman spectra, summarized the spectral characteristics, analysis of significant differences in spectra. Results: XRD, NIR and Raman spectra of alum and its counterfeit ammonium alum were significantly different. In the XRD pattern, ammonium alum has a small peak at 2θ = 14.56 °, which is absent from the genuine alum. In the NIR spectrum, the ammonium alum has a characteristic peak at 4 650 cm -1, whereas the authentic alum has no such peak In the Raman spectrum, the strongest peak of the genuine alum at 990 cm -1 was split, with a moderate intensity peak at 974 cm -1, while the ammonium alum had no peak at 974 cm -1 ) Peak, the above differences can be used for rapid identification of the two. In addition, the XRD patterns of the genuine product showed nine characteristic peaks (2θ = 11.18 °, 21.88 °, 24.58 °, 31.42 °, 33.76 °, 38.25 °, 39.94 °, 50.24 °, 50.99 °) There were two more gentle absorption peaks at ~ (-1) and 5 150 cm ~ (-1). Conclusion: The XRD, NIR and Raman spectra can be used for the accurate identification of alum, Alum and their counterfeit products. NIR combined with Raman spectroscopy can provide a fast and accurate new method for quality control and quick check of alum and its processed products method.