Determination of chitosan with a modified acid hydrolysis and HPLC method
Determination of chitosan with a modified acid hydrolysis and HPLC method
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改进的酸水解高效液相色谱法测定壳聚糖
DOI：
10.1016/j.carres.2012.11.005
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发表时间：
2013-01-25
影响因子：
3.1
通讯作者：
Xia, Wenshui
中科院分区：
文献类型：
--
作者：
Li, Bo;Zhang, Jiali;Xia, Wenshui
葡糖胺（GlcN）的酸水解和随后的定量广泛用于壳聚糖定量。壳聚糖水解过程中GlcN的降解是导致回收率下降的主要原因，这使得该方法不适用于壳聚糖的定量。10 mg壳聚糖用10 mL HCl-H3 PO 4（摩尔比75：25）的混合酸溶液水解，回收率最高，显著高于盐酸水解。进一步研究表明，最佳水解条件为：HCl-H3 PO 4（4.5：1.5M），水解时间24 h，水解温度110 ℃。在HPLC定量之前，用9-芴基甲氧羰基氯（FMOC-Cl）中和并衍生水解产物。FMOC-Cl：GlcN的最佳比例为53：1，过量的FMOC-Cl由溶液的高离子强度诱导。该定量方法经过验证，具有良好的线性、准确度和精密度，适用于壳聚糖的测定。(C)2012爱思唯尔有限公司保留所有权利。
Acid hydrolysis and subsequent quantification of glucosamine (GlcN) are widely used for chitosan quantification. Degradation of GlcN during chitosan hydrolysis was the main reason for the decrease of recovery, which made the method improper for the quantification of chitosan. Ten milligram of chitosan hydrolyzed with 10 mL mixed acid solution of HCl-H3PO4 (75:25 in molar ratio) showed the highest recovery, significantly higher than HCl hydrolysis. Further study revealed that the optimum conditions involved the hydrolysis with HCl-H3PO4 (4.5:1.5 M) for 24 h at 110 degrees C. The hydrolysate was neutralized and derived with 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl) before HPLC quantification. The optimum ratio of FMOC-Cl:GlcN was 53:1, with excess FMOC-Cl induced by the high ionic strength of the solution. This quantification procedure was then validated and proved to be specific, with good linearity, accuracy, and precision, making it well-suited for the determination of chitosan. (C) 2012 Elsevier Ltd. All rights reserved.