Leibniz-Institut für Polymerforschung Dresden, Physikalische Chemie und Physik der Polymere, Hohe Straße 6, D-01069 Dresden, Germany.
Int J Biol Macromol. 2021 Feb 28;171:242-261. doi: 10.1016/j.ijbiomac.2021.01.010. Epub 2021 Jan 6.
In recent years, chitosan has attracted considerable interest in many fields due to its sufficient charge density under biological, non-hazardous conditions. Since chitosan originates from natural resources and has two different monomer units, its characterization must be carried out in a goal-oriented and precise manner. This work focuses on the characterization of chitosans most important parameters - solubility, crystallinity, degree of deacetylation (DD) and molecular weight - in a simple and convenient way. The DD was determined using Nuclear Magnetic Resonance spectroscopy (NMR), Particle Charge Detection (PCD), Fourier Transform Infrared spectroscopy (FTIR), CHN elemental analysis (CHN-EA) and conductometric/potentiometric titration with special attention to its physical state as solid or liquid. Investigation of DD by FTIR was successfully determined by calculating peak heights, peak areas and peak deconvolution from a linear combination of Gaussian and Lorentzian functions. Asymmetrical flow field flow fractionation with light scattering detection (AF4-LS) was applied in order to calculate molar masses and radii. In addition, pH-potentiometric titrations demonstrated a reproducible displacement of the point of zero charge (PZC) in form of a hysteresis depending on the titration direction. The DD affects the crystallinity, which was determined by deconvolution of the crystalline and amorphous domains.
近年来,壳聚糖因其在生物、非危害条件下具有足够的电荷密度而在许多领域引起了相当大的兴趣。由于壳聚糖源自天然资源且具有两个不同的单体单元,因此必须有针对性且精确地对其进行表征。这项工作重点关注壳聚糖最重要的参数——溶解度、结晶度、脱乙酰度 (DD) 和分子量——的简单方便的表征方法。使用核磁共振波谱 (NMR)、颗粒电荷检测 (PCD)、傅里叶变换红外光谱 (FTIR)、元素分析 (CHN-EA) 等方法确定 DD,特别注意其物理状态是固体还是液体。通过计算峰高、峰面积和由高斯和洛伦兹函数线性组合的峰解卷积,成功地通过 FTIR 对 DD 进行了研究。为了计算摩尔质量和半径,应用了不对称流场流分离与光散射检测 (AF4-LS)。此外,pH 电位滴定法显示出取决于滴定方向的零电荷点 (PZC) 滞后的可重复位移。DD 会影响结晶度,这是通过对结晶和非晶区的解卷积来确定的。