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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
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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.
作者 王滕斌 郭友利 张永勤 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)
出处 《青岛科技大学学报(自然科学版)》 CAS 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).
关键词 气相色谱法 测定 羟丙基 摩尔取代度 gas chromotography determination hydroxypropyl degree of molar substitution
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