Jendrzejewska Izabela
Institute of Chemistry, Faculty of Science and Technology, University of Silesia, Katowice, Poland.
Front Chem. 2020 Sep 30;8:672. doi: 10.3389/fchem.2020.00672. eCollection 2020.
It is estimated that ~50% of medications and dietary supplements offered in the Internet are counterfeit. X-ray diffraction is one of the techniques which may be successfully applied to identify various chemical compounds in polycrystalline mixtures such as dietary supplements, but also medications, narcotics or designer drugs. X-ray diffraction enables the understanding of compositions of such mixtures. For the tests, 22 dietary supplements which should contain magnesium and calcium compounds, available in pharmacies, groceries, Internet shops, as well as in shops for sportspersons, were selected. Identification of crystalline substances present in the tested sample consists in determination of inter-planar distances of investigated substances and determination of intensity of the obtained diffraction lines, and then in comparing them with values contained in diffraction databases. In this study, the ICDD-PDF2 database was used. The most important criterion in qualitative analysis, confirming the presence of a given phase, is the conformity of positions of diffraction lines in the recorded diffraction image with those in the reference image. Reflection shifts for the individual θ angles compared with the data from the database should not exceed 0.2°. In most cases, X-ray analysis of the investigated dietary supplements proved the presence of magnesium and calcium compounds declared by the manufacturer, as well as allowing the identification of auxiliary substances present in the tested products. In the case of two magnesium-containing dietary supplements, the magnesium compounds declared by the manufacturer were not found. Our studies confirmed the effectiveness of X-ray structural analysis and proved the possibility of distinguishing counterfeit preparations from authentic products, as well as to use this method for the quality control of such pharmaceutical preparations.
据估计,互联网上提供的药物和膳食补充剂中约有50%是假冒的。X射线衍射是一种可以成功应用于识别多晶混合物(如膳食补充剂,但也包括药物、麻醉品或设计药物)中各种化合物的技术。X射线衍射能够了解此类混合物的成分。为了进行测试,我们选择了22种应含有镁和钙化合物的膳食补充剂,这些产品在药店、杂货店、网上商店以及运动用品商店均有销售。对测试样品中存在的晶体物质进行鉴定,包括测定被研究物质的晶面间距以及所获得衍射线条的强度,然后将它们与衍射数据库中包含的值进行比较。在本研究中,使用了ICDD - PDF2数据库。定性分析中确认给定物相存在的最重要标准是记录的衍射图像中衍射线条的位置与参考图像中的位置相符。与数据库数据相比,各个θ角的反射位移不应超过0.2°。在大多数情况下,对所研究的膳食补充剂进行的X射线分析证明了制造商宣称的镁和钙化合物的存在,同时也能够鉴定出测试产品中存在的辅助物质。在两种含镁膳食补充剂的情况下,未发现制造商宣称的镁化合物。我们的研究证实了X射线结构分析的有效性,并证明了区分假冒制剂与正品的可能性,以及将该方法用于此类药物制剂质量控制的可能性。