离子色谱分离保留因子计算定性分析低聚壳寡糖的研究

发布时间：2018-04-27 08:25

本文选题：低聚壳寡糖 + 壳聚糖　；参考：《药物分析杂志》2017年01期

【摘要】：目的:建立阴离子交换色谱分离,并用保留因子计算法定性分析低聚壳寡糖。方法:首先利用高效阴离子交换色谱-积分脉冲安培检测法(HPAEC-IPAD)对5种壳寡糖(聚合度DP=2~6)标准样品进行分离;分离条件:采用DIONEX CarboPac·PA10(4.0 mm×50 mm)保护柱和DIONEX CarboPac·PA10(4.0 mm×250mm)分析柱,淋洗液采用氢氧化钠溶液,积分脉冲安培法检测。然后用建立的分离方法对壳寡糖样品进行分离并定性。再根据所得样品色谱峰的保留时间分别计算保留因子,建立壳寡糖聚合度(DP)与其保留因子(k')的相关关系,根据建立的相关关系对未知的壳寡糖进行定性,并用质谱方法对未知壳寡糖样品进行验证。结果:壳寡糖聚合度的对数值与其保留因子的对数值具有线性关系,回归系数R~2≥0.998 7,利用建立的线性回归方程对样品中的4种未知壳寡糖样品的定性结果为壳七糖、壳八糖、壳九糖和壳十糖,误差≤5.66%。质谱方法对未知壳寡糖样品进行了验证,验证结果为样品中存在壳二糖、壳三糖、壳四糖、壳五糖、壳六糖、壳七糖和壳八糖。结论:对于壳寡糖样品用离子色谱分离,保留因子计算来定性壳寡糖聚合度的方法是可行的。
[Abstract]:Objective: to establish anionic exchange chromatography and to calculate the legal analysis of oligochitosan oligosaccharides with retention factors. Methods: first, 5 kinds of chitosan oligosaccharides (DP=2~6) standard samples were separated by high performance anion exchange chromatography - integrated pulse amperometric detection (HPAEC-IPAD), and the separation conditions were: using DIONEX CarboPac. PA10 (4 mm x 50 mm). The column and DIONEX CarboPac PA10 (4 mm x 250mm) column were analyzed with sodium hydroxide solution and integrated pulse ampere method. Then the chitosan oligosaccharide samples were separated and qualitatively separated by the established separation method. The retention factors were calculated according to the retention time of the chromatographic peaks, and the degree of polymerization of chitosan oligosaccharides (DP) and their retention were established. The correlation relation of factor (k'), the unknown shell oligosaccharides are qualitatively determined according to the relationship established, and the samples of the unknown shell oligosaccharides are verified by mass spectrometry. Results: the value of the degree of polymerization of the oligosaccharide oligosaccharides has a linear relationship with the value of the retention factor, the regression coefficient R~2 is more than 0.9987, and the linear regression equation established to the sample is used for the sample. The qualitative results of 4 uncharted oligosaccharides were shell seven sugar, shell eight sugar, shell nine sugar and shell ten sugar. The samples of unknown shell oligosaccharides were verified by error less than 5.66%. mass spectrometry. The results showed that there were shell two sugar, shell three sugar, shell four sugar, shell five sugar, shell six sugar, shell seven sugar and shell eight sugar. It is feasible to determine the degree of polymerization of chitosan oligosaccharides by spectral separation and retention factor calculation.

【作者单位】：浙江树人大学生物与环境工程学院;
【基金】：浙江省自然科学重点基金(编号:Z14B070001) 浙江省分析测试基金(编号:2015C37039)
【分类号】：R917

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