离子色谱法检测食品中壳寡糖含量的研究

Determination of chitosan oligosaccharide in foods by ion chromatography

目的建立一种食品中壳寡糖含量的离子色谱检测方法。方法样品经盐酸溶液水解后,氢氧化钠溶液中和至中性,过反相固相萃取柱净化。采用水(A)、200 mmol/L氢氧化钠(B)和150 mmol/L氢氧化钠-500 mmol/L乙酸钠(C)作为流动相进行梯度洗脱,脉冲安培检测器定量测定。结果确定壳寡糖水解最佳条件为水解温度为110℃,盐酸溶液浓度为8mol/L,水解时间为4h,回收率在87.72%~103.37%,平均回收率为95.58%,相对标准偏差为5.80%,方法定量限为0.1 g/100g。结论该方法快速、准确、灵敏,适用于食品中壳寡糖含量的测定。

Objective To establish a method for determination of chitosan oligosaccharide in foods by ion chromatography. Methods Samples were hydrolyzed with muriatic acid and neutralized with sodium hydroxide solution, then purified with reversed phase solid phase extraction column. The water(A), 200 mmol/L sodium hydroxide solution(B) and 150 mmol/L sodium hydroxide solution-500 mmol/L sodium acetate solution(C) were used as mobile phases for gradient elution, and pulsed amperometric detector was used for quantitative determination.Results The best conditions of hydrolyzing chitosan oligosaccharide were as follows: hydrolysis temperature was110 ℃, muriatic acid was 8 mol/L, and hydrolysis time was 4 h. The recoveries were ranged from 87.72% to103.37%, the average recovery was 95.58%. The relative standard deviation(RSD) was 5.80%, and the limit of quantitation(LOQ) was 0.1 g/100 g. Conclusion This method is fast, accurate and sensitive, which is suitable for the determination of chitosan oligosaccharide in food samples.