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无定形橙皮素在玻璃化转变温度以上的分子弛豫行为和等温结晶

Molecular relaxation behavior and isothermal crystallization above glass transition temperature of amorphous hesperetin.

作者信息

Shete Ganesh, Khomane Kailas S, Bansal Arvind Kumar

机构信息

Department of Pharmaceutics, National Institute of Pharmaceutical Education and Research (NIPER), S.A.S. Nagar, Punjab, 160062, India.

出版信息

J Pharm Sci. 2014 Jan;103(1):167-78. doi: 10.1002/jps.23766. Epub 2013 Nov 1.

Abstract

The purpose of this paper was to investigate the relaxation behavior of amorphous hesperetin (HRN), using dielectric spectroscopy, and assessment of its crystallization kinetics above glass transition temperature (Tg ). Amorphous HRN exhibited both local (β-) and global (α-) relaxations. β-Relaxation was observed below Tg , whereas α-relaxation prominently emerged above Tg . β-Relaxation was found to be of Johari-Goldstein type and was correlated with α-process by coupling model. Secondly, isothermal crystallization experiments were performed at 363 K (Tg + 16.5 K), 373 K (Tg + 26.5 K), and 383 K (Tg + 36.5 K). The kinetics of crystallization, obtained from the normalized dielectric strength, was modeled using the Avrami model. Havriliak-Negami (HN) shape parameters, αHN and αHN .βHN , were analyzed during the course of crystallization to understand the dynamics of amorphous phase during the emergence of crystallites. HN shape parameters indicated that long range (α-like) were motions affected to a greater extent than short range (β-like) motions during isothermal crystallization studies at all temperature conditions. The variable behavior of α-like motions at different isothermal crystallization temperatures was attributed to evolving crystallites with time and increase in electrical conductivity with temperature.

摘要

本文旨在利用介电谱研究无定形橙皮素(HRN)的弛豫行为,并评估其在玻璃化转变温度(Tg)以上的结晶动力学。无定形HRN表现出局部(β-)和整体(α-)弛豫。β-弛豫在Tg以下观察到,而α-弛豫在Tg以上显著出现。发现β-弛豫属于Johari-Goldstein类型,并通过耦合模型与α-过程相关。其次,在363 K(Tg + 16.5 K)、373 K(Tg + 26.5 K)和383 K(Tg + 36.5 K)下进行等温结晶实验。从归一化介电强度获得的结晶动力学,使用Avrami模型进行建模。在结晶过程中分析Havriliak-Negami(HN)形状参数αHN和αHN.βHN,以了解微晶出现过程中非晶相的动力学。HN形状参数表明,在所有温度条件下的等温结晶研究中,长程(α样)运动比短程(β样)运动受到的影响更大。不同等温结晶温度下α样运动的可变行为归因于微晶随时间的演变以及电导率随温度的增加。

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