利 通1,2，陳 茜1,2，貝榮廷1,2，何焜鵬1,2，凌育昕1,2，林 丹1,2，鄭澤洋1,2
（1 廣東省食品工業研究所有限公司，廣東 廣州 511442；
2 廣東省食品質量監督檢驗站，廣東 廣州 511442）
摘 要：本文研究了一種離子色譜法快速、準確測定食品殼寡糖含量的方法，研究不同柱溫、流動相及洗脫程序、提 取條件的優化（凈化柱的選擇、柱回收考察、酸水解溶液濃度的選擇、酸水解時長的選擇）等對殼寡糖測定的影響，最 終確定試樣在100℃水浴下，用8mol/L 鹽酸溶液水解8h，水解液經強陽離子交換固相萃取后，采用糖分析（4.0mm× 250mm，10µm，保護柱 4.0mm×50mm）色譜柱分離，水和 200mmol/L 氫氧化鈉溶液作為流動相梯度洗脫，離子色譜 法測定殼寡糖的含量。方法驗證表明，樣品在0.05μg/mL～10μg/mL質量濃度范圍之間具有良好的線性關系（R2> 0.9998），樣品回收率范圍在 93.35%～102.93%，方法精密度相對標準偏差 RSD%（n=3）在 0.12%～1.74%，表明該檢測 方法簡便、準確、可靠，線性關系、精密度、重復性、穩定性、加樣回收率均較好，可用于食品中殼寡糖的定量分析。
關鍵詞：食品；殼寡糖；氨基葡萄糖；離子色譜法
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
中圖分類號：TS207 文獻標志碼：A 文章編號：1007-7871（2025）06-0011-07
2025，Vol.28，No.6