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首页> 外文期刊>Journal of biomedical materials research. Part B, Applied biomaterials. >Evaluation of an improved acid hydrolysis-HPLC assay for the acetyl content in chitin and chitosan.
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Evaluation of an improved acid hydrolysis-HPLC assay for the acetyl content in chitin and chitosan.

机译:评估一种改进的酸水解-HPLC测定甲壳质和壳聚糖中乙酰基含量的方法。

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摘要

Functional properties of the amino polysaccharides, chitin and chitosan, vary significantly with their acetyl content. The acid hydrolysis-HPLC method offers good accuracy and precision to assay the acetyl content regardless of the solubility of the sample. In this research, the hydrolysis parameters were changed, and the analytical method was counterchecked with other methods. Complete hydrolysis was achieved by mixing chitosan with 1.4 mM oxalic acid and 12 M sulfuric acid followed by treatment at 110 degrees C for 40 min. A sealed glass ampule was used instead of a vacuum hydrolysis tube. The acetic acid released during acid hydrolysis was measured quantitatively by HPLC. A high correlation (r(2) = 0.98) was obtained between the modified HPLC assay and the solid-state (13)C CP/MAS NMR method for the samples of various crustacean sources with a wide range of acetyl contents. The modified HPLC method was also highly correlated (r(2) = 0.99) with the first derivative UV method for soluble chitosan.
机译:氨基多糖,几丁质和壳聚糖的功能特性随乙酰基含量的不同而有很大差异。无论样品的溶解度如何,酸水解-HPLC方法都能提供良好的准确性和精密度来测定乙酰基含量。在这项研究中,改变了水解参数,并与其他方法反驳了分析方法。通过将壳聚糖与1.4 mM草酸和12 M硫酸混合,然后在110摄氏度下处理40分钟,可以实现完全水解。使用密封的玻璃安瓿瓶代替真空水解管。通过HPLC定量地测量在酸水解期间释放的乙酸。改进的HPLC分析方法与固态(13)C CP / MAS NMR方法对各种甲壳类来源且乙酰基含量范围广泛的样品之间的相关性高(r(2)= 0.98)。改进的HPLC方法与可溶性壳聚糖的一阶导数UV方法也高度相关(r(2)= 0.99)。

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