气相色谱法测定羟丙基壳聚糖的摩尔取代度  

Determination of Molar Substitution Degree of Hydroxypropyl Chitosan by Gas Chromotography

作　　者：王滕斌 郭友利 张永勤[1] WANG Tengbin;GUO Youli;ZHANG Yongqin(College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China;Yantai Tianlu Food Co.,Ltd.,Yantai 264000,China)

机构地区：[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

出　　处：《青岛科技大学学报（自然科学版）》2024年第4期23-27,48,共6页Journal of Qingdao University of Science and Technology:Natural Science Edition

基　　金：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).

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^(1)H 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^(1)H NMR法的结果呈线性关系,其校正系数为1.85;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。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^(1)H 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^(1)H NMR method,and its correction coefficient is 1.85.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.

关 键 词：气相色谱法 测定 羟丙基 摩尔取代度 

分 类 号：TQ207.2[化学工程—有机化工]