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通过傅里叶变换红外光谱法(FTIR)、核磁共振氢谱(H NMR)和紫外分光光度法测量壳聚糖薄膜的脱乙酰度。

Measurement of the degree of deacetylation in chitosan films by FTIR, H NMR and UV spectrophotometry.

作者信息

Sánchez-Machado Dalia I, López-Cervantes Jaime, Escárcega-Galaz Ana A, Campas-Baypoli Olga N, Martínez-Ibarra Diana M, Rascón-León Salvador

机构信息

Instituto Tecnológico de Sonora, Ciudad Obregón, Sonora MX-85000, México.

出版信息

MethodsX. 2024 Jan 23;12:102583. doi: 10.1016/j.mex.2024.102583. eCollection 2024 Jun.

Abstract

The chitosan films were prepared from shrimp, squid, and crab to corroborate that regardless of the source of the chitosan, it was possible to measure the degree of deacetylation. In this work, the degree of deacetylation of chitosan was evaluated via UV, FTIR and H NMR spectrophotometry methodologies. Values in a range of 74 to 99% degree of deacetylation (DD) were obtained and varied depending on the method used and the source of chitosan. The spectrophotometric method is one of the most commonly used for this determination; however, it has the limitation that D-glucosamine and N-acetylglucosamine share similar wavelengths. All three methods were simple and provided rapid analysis; however, NMR, in particular, was expensive due to its equipment specifications. For this reason, its important to select the simplest method than can be routinely used.•The simplest used technique to determine the degree of deacetylation is infrared spectroscopy.•The degree of acetylation of chitosan is related to its physicochemical properties; its determination is an important parameter due to its association with chitosan applications in different industrial areas.•The H NMR method is very precise and requires expensive equipment and trained personal. Thus, it cannot be used routinely to determine the degree of deacetylation.

摘要

壳聚糖薄膜由虾、鱿鱼和螃蟹制备而成,以证实无论壳聚糖的来源如何,都可以测量其脱乙酰度。在这项工作中,通过紫外、傅里叶变换红外光谱(FTIR)和氢核磁共振(H NMR)分光光度法对壳聚糖的脱乙酰度进行了评估。获得了脱乙酰度(DD)在74%至99%范围内的值,且该值因所使用的方法和壳聚糖的来源而异。分光光度法是最常用于此测定的方法之一;然而,它存在一个局限性,即D - 葡萄糖胺和N - 乙酰葡萄糖胺具有相似的波长。所有这三种方法都很简单且能提供快速分析;然而,特别是核磁共振(NMR),由于其设备规格原因成本较高。因此,选择能够常规使用的最简单方法很重要。

•用于测定脱乙酰度的最简单技术是红外光谱法。

•壳聚糖的乙酰化程度与其物理化学性质相关;由于其与壳聚糖在不同工业领域的应用相关联,其测定是一个重要参数。

•氢核磁共振(H NMR)方法非常精确,但需要昂贵的设备和专业人员。因此,它不能常规用于测定脱乙酰度。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9a1a/10837090/9facd1ca5f4f/ga1.jpg

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