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
王滕斌 1郭友利 2张永勤1
作者信息
- 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
- 折叠
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.
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 op-timized,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 sam-pling 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 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Key words
gas chromotography/determination/hydroxypropyl/degree of molar substitu-tion引用本文复制引用
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)
出版年
2024
NETL
NSTL
万方数据