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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
【摘要】 建立并优化了测定羟丙基壳聚糖(HPCS)摩尔取代度(M_S)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M_S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M_S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(M_S) 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 M_S 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 M_S 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;
- 【文献出处】 青岛科技大学学报(自然科学版) ,Journal of Qingdao University of Science and Technology(Natural Science Edition) , 编辑部邮箱 ,2024年04期
- 【分类号】O636.1;O657.71
- 【下载频次】26