Le Bail P, Rondeau C, Buléon A
Unité de Physicochimie des Macromolécules, Institut National de la Recherche Agronomique, BP 71627, 44316 Nantes, Cedex 03, France.
Int J Biol Macromol. 2005 Mar;35(1-2):1-7. doi: 10.1016/j.ijbiomac.2004.09.001. Epub 2004 Dec 8.
Crystalline amylose complexes were prepared with decanal, 1-butanol, menthone and alpha-naphtol. Their crystalline structure and the related helical conformation, determined by wide angle X-ray diffraction (WAXD) and 13C CPMAS solid state NMR, were assigned to V6I, V6II, V6III and V8 types, respectively. It was possible to propose some hypotheses on the possible nature of interactions and especially intra-/inter-helical inclusion. Some shifts in the NMR C1 carbon signals were attributed to the presence of ligand in specific sites inside the structure for a same type of V6 helical conformation. Moreover, the crystallinity and polymorphic changes induced by desorption/rehydration were studied. A general increase of the carbon resonances sharpness upon rehydration has been observed, but also a V6II-V6I transition when decreasing the water content. Differential scanning calorimetry (DSC) experiments were also performed to approach the thermostability of the four types of complex and also the way they form again after melting/cooling sequences.
用癸醛、1-丁醇、薄荷酮和α-萘酚制备了结晶直链淀粉复合物。通过广角X射线衍射（WAXD）和13C CPMAS固体核磁共振确定了它们的晶体结构和相关的螺旋构象，分别归为V6I、V6II、V6III和V8类型。可以对相互作用的可能性质，特别是螺旋内/螺旋间包合的可能性质提出一些假设。对于相同类型的V6螺旋构象，核磁共振C1碳信号的一些位移归因于结构内特定位置存在配体。此外，还研究了解吸/再水化引起的结晶度和多晶型变化。观察到再水化后碳共振锐度普遍增加，同时水分含量降低时会发生V6II-V6I转变。还进行了差示扫描量热法（DSC）实验，以研究这四种复合物的热稳定性以及它们在熔化/冷却序列后再次形成的方式。
