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
武亭亭 1陈娟娟 1刘佳 1何国亮 1赵晨红 1赵士聪 1陈修红1
作者信息
- 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;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
- 折叠
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.
Abstract
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 xylo-oligosaccharides.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Key words
high performance liquid chromatography/xylo-oligosaccharides/high gelatinization/baked foods/hydrolysis引用本文复制引用
出版年
2024
NETL
NSTL
万方数据