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202404003.pdf
文章编号： 1672-6987（2024）04-0023-05； DOI： 10.16351/j.1672-6987.2024.04.003
王滕斌1， 郭友利2， 张永勤1*(1. 青岛科技大学 化工学院， 山东 青岛 266042；2. 烟台天鹭食品有限公司， 山东 烟台 264000)
摘要： 建立并优化了测定羟丙基壳聚糖(HPCS)摩尔取代度(MS)的气相色谱法(GC法)，并与1H NMR法进行比较。结果表明，用特氟龙内衬-铝盖的反应瓶进行样品前处理较合理，自动进样可提高精密度，标准曲线测定法优于美国药典中的单点法；所测MS值与1H NMR法的结果呈线性关系，其校正系数为185；当HPCS的原料壳聚糖的乙酰化度（DA）小于5%时，对MS的测定的影响较小，其相对误差<1%。因此，可成为HPCS生产企业的常规检测方法，用于大批量测试。
关键词： 气相色谱法； 测定； 羟丙基； 摩尔取代度
中图分类号： TQ 207+.2文献标志码： A
引用格式： 王滕斌， 郭友利， 张永勤. 气相色谱法测定羟丙基壳聚糖的摩尔取代度［J］. 青岛科技大学学报(自然科学版), 2024, 45（4）： 23-27.
WANG Tengbin， GUO Youli， ZHANG Yongqin. Determination of molar substitution degree of hydroxypropyl chitosan by gas chromotography［J］. Journal of Qingdao University of Science and Technology（Natural Science Edition), 2024, 45（4）： 23-27.
Determination of Molar Substitution Degree of Hydroxypropyl
Chitosan by Gas Chromotography
WANG Tengbin1, GUO Youli2, ZHANG Yongqin1
(1, College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;
2. Yantai Tianlu Food Co., Ltd., Yantai 264000, China)
Abstract: In this paper, a gas chromatography method(GC method) for the determination of molar substitution degree (MS) of hydroxypropyl chitosan (HPCS) was established and optimized, and compared with 1H NMR method. The results show that it is reasonable to use reaction vials with teflon-lined and aluminum-cap for sample pretreatment, automatic sampling improves precision. The standard curve method is superior to the single-point method in the US Pharmacopoeia. The measured MS values have a linear relationship with those from 1H NMR method, and its correction coefficient is 185. When the acetylation degree (DA) of the raw material chitosan is less than 5%, little effect on the MS measurement, and the relative error is less than 1%. Therefore, this method can be used as a routine test in HPCS manufacturers for large-scale of measurement.
Key words: gas chromotography; determination; hydroxypropyl; degree of molar substitution
收稿日期： 2024-04-15
基金项目： 山东省重点研发计划项目（2019GSF107081）；青岛市科技民生计划项目（17-6-3-28-gx）.
作者简介： 王滕斌(1997—), 男, 硕士研究生.*通信联系人.
