高效液相色谱–示差折光法间接测定高糊化度–焙烤食品中低聚木糖含量  

Determination content of xylo-oligosaccharides in high gelatinization-baked foods by high performance liquid chromatography with refractive indexdetector

作　　者：武亭亭 陈娟娟 刘佳 何国亮 赵晨红 赵士聪 陈修红 WU Ting-Ting;CHEN Juan-Juan;LIU Jia;HE Guo-Liang;ZHAO Chen-Hong;ZHAO Shi-Cong;CHEN Xiu-Hong(National Non-Staple Food Quality Inspection and Testing Center,International Trade Food Science Research Institute Co.,Ltd.,Beijing 102209,China;Beijing Key Laboratory of Nutrition Health and Food Safety,Nutrition&Health Research Institute,COFCO Corporation,Beijing 102209,China)

机构地区：[1]国家副食品质量检验检测中心,国贸食品科学研究院有限公司,北京102209 [2]营养健康与食品安全北京市重点实验室,中粮营养健康研究院有限公司,北京102209

出　　处：《实验室检测》2024年第10期9-14,共6页Laboratory Testing

摘　　要：目的建立高效液相色谱–示差折光法间接测定高糊化度–焙烤食品中低聚木糖含量的分析方法。方法样品经石油醚脱脂后20%乙醇水溶液提取,68%乙醇沉淀糊精、淀粉等大分子糖类,提取液中糖被稀硫酸水解为单糖,水解前后的样品溶液经酰胺基柱分离,示差折光检测器检测,外标法定量。水解前后木糖含量差值乘以低聚木糖与木糖的平均转化系数即得样品中低聚木糖含量。结果木糖质量浓度为0.25~5.00 mg/mL时,其峰面积与浓度之间线性关系良好(r=0.9998)。高糊化度–焙烤食品中的加标回收率在92.0%~95.8%之间,相对标准偏差(relative standard deviation,RSD)在1.8%~4.0%之间。低聚木糖检出限为0.03 g/100 g,定量限为0.1 g/100 g。结论本方法采用低浓度乙醇提取样品,避免了样品糊化对低聚木糖包埋降低提取效率及测定结果偏低的影响。方法操作可行,专一性强,能够准确、快速地测定高糊化度–焙烤食品中低聚木糖的含量。Objective To established an analytical method for indirect determination of xylo-oligosaccharides in high gelatinization-baked foods by high performance liquid chromatography with refractive index detector.Methods After degreased with petroleum ether,the samples were extracted with 20%ethanol solution,and macromolecular sugars such as dextrin and starch were precipitated with 68%ethanol solution.The sugars in the extraction solution were hydrolyzed into monosaccharides by diluted sulfuric acid,the solution before and after hydrolysis was separated by amide column,detected by refractive index detector,and quantified by external standard method.The product between the difference of xylose before and after hydrolysis and the average conversion coefficient of xylo-oligosaccharides and xylose was the xylooligosaccharides.Results When the xylose was 0.25~5.00 mg/mL,there was a good linear relationship between peak area and concentration(r=0.9998).The recovery rates ranged from 92.0%to 95.8%,the relative standard deviations(RSDs)were 1.8%~4.0%in high gelatinization-baked foods.The limit of detection and limit of quantization of xylo-oligosaccharides were 0.03 g/100 g,0.1 g/100 g respectively.Conclusion The extraction method of low concentration ethanol solution is feasible and specific.The method avoided the impact of high gelatinization on the low extraction efficiency and measurement results.It can determine xylo-oligosaccharides in high gelatinization-baked foods accurately and quickly.

关 键 词：高效液相色谱法 低聚木糖 高糊化度 焙烤食品 水解 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.72[轻工技术与工程—食品科学与工程]