高效液相色谱串联质谱法测定酸奶中木糖和5种低聚木糖含量  

Determination of Xylose and 5 Xylo-oligosaccharides in Yogurt by HPLC-MS/MS

作　　者：甄振鹏 高裕锋 李硕聪 庞扬海 黄敏兴 余构彬 郭剑雄 ZHEN Zhen-peng;GAO Yu-feng;LI Shuo-cong;PANG Yang-hai;HUANG Min-xing;YU Gou-bin;GUO Jian-xiong(Guandong Provincial Bioengineering Institute(Guangzhou Sugarcane Industry Research Institute),China Sugar Inspection Center,Research Center for Sugarcance Industry Engineering Technology of Light Industry,China,Guangzhou 510316,Guandong,China)

机构地区：[1]广东省生物工程研究所(广州甘蔗糖业研究所),国家糖业质量监督检验中心,中国轻工业甘蔗制糖工程技术研究中心,广东广州510316

出　　处：《食品研究与开发》2020年第19期157-161,共5页Food Research and Development

基　　金：广东省科技计划项目(2016A040403066);广州市科技计划项目(201806010093)。

摘　　要：采用高效液相色谱串联质谱法(high performance liquid chromatography tandem mass spectrometry,HPLC-MS/MS)检测技术测定酸奶中木糖和低聚木糖(木二糖~木六糖)的含量。酸奶样品经乙醇:水(9:1,体积比)提取,采用Altus UPLC BEH Amide(1.7μm,2.1 mm×100 mm)柱,以乙腈-0.10%氨水溶液为流动相分离目标物。电喷雾质谱负离子模式(electron spray ionization negative,ESI-)下,多反应监测(multiple reaction monitoring,MRM)检测,外标法定量。该方法在0.1 mg/L^5.0 mg/L线性关系良好,相关系数(R>0.999 5),方法检出限在0.12 mg/kg^0.54 mg/kg之间。3个加标水平下进行回收率试验,回收率范围为76.5%~88.4%,相对标准偏差为5.1%~9.8%(n=6)。该方法样品前处理简易、方便,精密度、准确度和灵敏度均满足酸奶中木糖与低聚木糖的检测要求。A method for the determination of xylose and xylo-oligosaccharides in yogurt was established based on the high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The samples were extracted by ethanol:water(9∶1,volume ratio),then separated in an Altus UPLC BEH Amide column(1.7μm,2.1 mm×100 mm)with binary mobile phase of 0.10%ammonia and acetonitrile.The HPLC-MS/MS with electron spray ionization negative(ESI-)mode was operated and with multiple-reaction monitoring(MRM)mode,the contents of xylo-oligosaccharides were obtained by the external standard method for quantitative analysis.Linearity was observed in the range of 0.1 mg/L to 5.0 mg/L with correlation coefficient higher than 0.9995,and limits of detection(LODs)was between 0.12 mg/kg and 0.54 mg/kg.The recoveries of xylo-oligosaccharides at three levels were ranged from 76.5%to 88.4%with the relative standard deviations(RSDs)of 5.1%to 9.8%(n=6)in yogurt.The method was simple,easily and characterized with acceptable sensitivity and accuracy to meet the requirements for the determination of xylose and xylo-oligosaccharides in yogurt.

关 键 词：木糖 低聚木糖 酸奶 功能性低聚糖 高效液相色谱串联质谱 

分 类 号：TS252.54[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]