Sato H, Mizutani S, Tsuge S, Ohtani H, Aoi K, Takasu A, Okada M, Kobayashi S, Kiyosada T, Shoda S
Department of Applied Chemistry, Graduate School of Engineering, Nagoya University, Nagoya 464-01, Japan.
Anal Chem. 1998 Jan 1;70(1):7-12. doi: 10.1021/ac9706685.
A new method to determine directly and rapidly the degree of acetylation of chitin/chitosan was developed based on reactive pyrolysis-gas chromatography in the presence of an oxalic acid aqueous solution. The degree of acetylation was precisely evaluated on the basis of peak intensities of the characteristic products such as acetonitrile, acetic acid, and acetamide originating from the N-acetyl group of N-acetyl-d-glucosamine units of chitin/chitosan. The observed values were in good agreement with those obtained by (1)H NMR and the other methods. Moreover, the proposed technique was applicable to any kinds of chitin/chitosan samples over the whole range of acetylation including insoluble chitin/chitosan and perfectly acetylated artificial chitin having higher crystallinity to which (1)H NMR had been inapplicable.
基于在草酸水溶液存在下的反应热解-气相色谱法，开发了一种直接快速测定几丁质/壳聚糖乙酰化程度的新方法。根据源自几丁质/壳聚糖中N-乙酰-d-葡萄糖胺单元N-乙酰基的乙腈、乙酸和乙酰胺等特征产物的峰强度，精确评估乙酰化程度。观测值与通过1H NMR和其他方法获得的值高度一致。此外，所提出的技术适用于整个乙酰化范围内的任何种类的几丁质/壳聚糖样品，包括不溶性几丁质/壳聚糖和结晶度较高的完全乙酰化人工几丁质，而1H NMR对这些样品不适用。
