利 通1,2，陈 茜1,2，贝荣廷1,2，何焜鹏1,2，凌育昕1,2，林 丹1,2，郑泽洋1,2
（1 广东省食品工业研究所有限公司，广东 广州 511442；
2 广东省食品质量监督检验站，广东 广州 511442）
摘 要：本文研究了一种离子色谱法快速、准确测定食品壳寡糖含量的方法，研究不同柱温、流动相及洗脱程序、提 取条件的优化（净化柱的选择、柱回收考察、酸水解溶液浓度的选择、酸水解时长的选择）等对壳寡糖测定的影响，最 终确定试样在100℃水浴下，用8mol/L 盐酸溶液水解8h，水解液经强阳离子交换固相萃取后，采用糖分析（4.0mm× 250mm，10µm，保护柱 4.0mm×50mm）色谱柱分离，水和 200mmol/L 氢氧化钠溶液作为流动相梯度洗脱，离子色谱 法测定壳寡糖的含量。方法验证表明，样品在0.05μg/mL～10μg/mL质量浓度范围之间具有良好的线性关系（R2> 0.9998），样品回收率范围在 93.35%～102.93%，方法精密度相对标准偏差 RSD%（n=3）在 0.12%～1.74%，表明该检测 方法简便、准确、可靠，线性关系、精密度、重复性、稳定性、加样回收率均较好，可用于食品中壳寡糖的定量分析。
关键词：食品；壳寡糖；氨基葡萄糖；离子色谱法
Determination of Chitosan Oligosaccharides in Food by Ion Chromatography
LI Tong1,2，CHEN Qian1,2，BEI Rong-ting1,2，HE Kun-peng1,2，LING Yu-xin1,2，LIN Dan1,2，ZHENG Ze-yang1,2
（1 Guangdong Food Industry Research Institute Co.，Ltd.，Guangzhou 511442，China；
2 Guangdong Food Quality Supervision and Inspection Station，Guangzhou 511442，China）
Abstract: This paper studies a rapid and accurate method using ion chromatography to determine the content of Chitosan Oligosaccharides in food. It investigates the effects of optimizing different column temperatures，mobile phases，elution programs，and extraction conditions（such as the selection of purification columns，column recovery evaluation，choice of acid hydrolysis solution concentration，and duration of acid hydrolysis）on the determination of Chitosan Oligosaccharides. The final method established involves hydrolyzing the sample in 8mol/L hydrochloric acid solution at 100℃ for 8 hours in a water bath. The hydrolysate is subjected to strong cation exchange solid-phase extraction，followed by separation using a carbohydrate analysis column（4.0mm×250mm，10µm，with a guard column 4.0mm×50mm）. Water and 200mmol/L sodium hydroxide solution are used as the mobile phase with gradient elution. The content of Chitosan Oligosaccharides is then determined by ion chromatography. Method validation shows that the samples exhibit a good linear relationship within a concentration range of 0.05μg/mL to 10μg/mL（R²> 0.9998）. The sample recovery rate ranges from 93.35% to 102.93%，and the method precision relative standard deviation RSD%（n=3）ranges from 0.12% to 1.74%，indicating that this detection method is simple，accurate，and reliable. The linearity，precision，repeatability，stability，and spiked recovery are all satisfactory，making it suitable for the quantitative analysis of Chitosan Oligosaccharides in food.
Key words: food；chitosan oligosaccharide；glucosamine；ion chromatography
中图分类号：TS207 文献标志码：A 文章编号：1007-7871（2025）06-0011-07
2025，Vol.28，No.6