分析化学2025，Vol.53Issue(12)：2032-2042,11.DOI:10.19756/j.issn.0253-3820.251231
蔗果四糖三水合物精细结构表征与纯度标准物质研制
Fine Structural Characterization of Nystose Trihydrate and Development of Its Certified Reference Material
摘要
Abstract
To meet the metrological traceability requirements for fructooligosaccharide(FOS)detection in the fields such as food,a purity certified reference material of nystose trihydrate was developed.Comprehensive qualitative analysis of the pure raw material was performed using nuclear magnetic resonance(NMR)spectroscopy,mass spectrometry(MS),and X-ray diffraction(XRD).In the NMR analysis,in addition to¹H NMR and¹³C NMR spectra,¹H-¹H correlation spectroscopy(COSY),heteronuclear single-quantum coherence(HSQC),and heteronuclear multiple-bond correlation(HMBC)were also employed to identify glycosyl units,stereochemical configurations,and glycosidic bond linkage sites.Purity determination was conducted using both the mass balance method and quantitative nuclear magnetic resonance(qNMR)method.For the mass balance method,high-performance liquid chromatography-charged aerosol detector(HPLC-CAD)was used to quantify structurally related impurities;Karl Fischer coulometry with oven injection was applied to determine moisture content;headspace gas chromatography-flame ionization detector(HS-GC-FID)was utilized to measure residual volatile organic solvents;and inductively coupled plasma-mass spectrometry(ICP-MS)was employed to quantify non-volatile impurities.For the qNMR method,deuterium oxide(D2O)was used as the solvent,with potassium hydrogen phthalate as the internal standard.The homogeneity and stability of the reference material were evaluated using HPLC-CAD.Uncertainty assessment was systematically conducted,including uncertainties introduced by weighing,purity determination,homogeneity,and stability.Finally,the certified purity value of nystose trihydrate was 99.2%with a relative expanded uncertainty of 0.3%(k=2).The developed certified reference material in this work could provide a basis for traceability in relevant FOS detection.关键词
蔗果四糖三水合物/低聚果糖/标准物质/高效液相色谱-电雾式检测器/核磁共振波谱Key words
Nystose trihydrate/Fructooligosaccharide/Certified reference material/High-performance liquid chromatography-charged aerosol detector/Nuclear magnetic resonance spectroscopy引用本文复制引用
齐琦,董睿之,柳玉蓉,周霞,李倩,李秀琴,张庆合..蔗果四糖三水合物精细结构表征与纯度标准物质研制[J].分析化学,2025,53(12):2032-2042,11.基金项目
国家重点研发计划项目(No.2022YFF0710401)、国家市场监督管理总局科技计划项目(No.2023MK179)和中国计量科学研究院中央级公益性科研院所基本科研业务费专项资金项目(No.AKYZD2306-1)资助. Supported by the National Key Research and Development Program of China(No.2022YFF0710401),the Science and Technology Program of State Administration for Market Regulation(No.2023MK179)and the Fundamental Research Funds for the Central Public-Interest Scientific Institution(No.AKYZD2306-1). （No.2022YFF0710401）
