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Insulin polymorphism induced by two polyphenols: new crystal forms and advances in macromolecular powder diffraction
Acta Crystallographica Section D ( IF 2.6 ) Pub Date : 2020-11-02 , DOI: 10.1107/s205979832001195x Dimitris Panagiotis Triandafillidis 1 , Nikolaos Parthenios 1 , Maria Spiliopoulou 1 , Alexandros Valmas 1 , Christos Kosinas 1 , Fabia Gozzo 2 , Mathilde Reinle-Schmitt 2 , Detlef Beckers 3 , Thomas Degen 3 , Mihaela Pop 4 , Andrew N Fitch 5 , Jan Wollenhaupt 6 , Manfred S Weiss 7 , Fotini Karavassili 1 , Irene Margiolaki 1
Acta Crystallographica Section D ( IF 2.6 ) Pub Date : 2020-11-02 , DOI: 10.1107/s205979832001195x Dimitris Panagiotis Triandafillidis 1 , Nikolaos Parthenios 1 , Maria Spiliopoulou 1 , Alexandros Valmas 1 , Christos Kosinas 1 , Fabia Gozzo 2 , Mathilde Reinle-Schmitt 2 , Detlef Beckers 3 , Thomas Degen 3 , Mihaela Pop 4 , Andrew N Fitch 5 , Jan Wollenhaupt 6 , Manfred S Weiss 7 , Fotini Karavassili 1 , Irene Margiolaki 1
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This study focuses on the polymorphism of human insulin (HI) upon the binding of the phenolic derivatives p‐coumaric acid or trans‐resveratrol over a wide pH range. The determination of the structural behaviour of HI via X‐ray powder diffraction (XRPD) and single‐crystal X‐ray diffraction (SCXRD) is reported. Four distinct polymorphs were identified, two of which have not been reported previously. The intermediate phase transitions are discussed. One of the novel monoclinic polymorphs displays the highest molecular packing among insulin polymorphs of the same space group to date; its structure was elucidated by SCXRD. XRPD data collection was performed using a variety of instrumental setups and a systematic comparison of the acquired data is presented. A laboratory diffractometer was used for screening prior to high‐resolution XRPD data collection on the ID22 beamline at the European Synchrotron Radiation Facility. Additional measurements for the most representative samples were performed on the X04SA beamline at the Swiss Light Source (SLS) using the MYTHEN II detector, which allowed the detection of minor previously untraceable impurities and dramatically improved the d‐spacing resolution even for poorly diffracting samples.
中文翻译：
两种多酚诱导的胰岛素多态性：新的晶体形式和高分子粉末衍射的进展
这项研究着重于人胰岛素（HI）在酚类衍生物对香豆酸或反式香豆素结合后的多态性白藜芦醇在很宽的pH范围内。报告了通过X射线粉末衍射（XRPD）和单晶X射线衍射（SCXRD）确定的HI的结构行为。确定了四个不同的多晶型物，其中两个以前未曾报道过。讨论了中间相变。迄今为止，一种新型的单斜晶型多晶型物在同一空间群的胰岛素多晶型物中表现出最高的分子堆积；SCXRD阐明了它的结构。XRPD数据收集是使用多种仪器设置进行的，并且对获得的数据进行了系统的比较。在欧洲同步辐射装置的ID22光束线上高分辨率XRPD数据采集之前，使用实验室衍射仪进行筛选。d间距分辨率，即使是衍射差的样品也是如此。
更新日期：2020-11-02
中文翻译：
两种多酚诱导的胰岛素多态性：新的晶体形式和高分子粉末衍射的进展
这项研究着重于人胰岛素（HI）在酚类衍生物对香豆酸或反式香豆素结合后的多态性白藜芦醇在很宽的pH范围内。报告了通过X射线粉末衍射（XRPD）和单晶X射线衍射（SCXRD）确定的HI的结构行为。确定了四个不同的多晶型物，其中两个以前未曾报道过。讨论了中间相变。迄今为止，一种新型的单斜晶型多晶型物在同一空间群的胰岛素多晶型物中表现出最高的分子堆积；SCXRD阐明了它的结构。XRPD数据收集是使用多种仪器设置进行的，并且对获得的数据进行了系统的比较。在欧洲同步辐射装置的ID22光束线上高分辨率XRPD数据采集之前，使用实验室衍射仪进行筛选。d间距分辨率，即使是衍射差的样品也是如此。
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