玉米赤霉酮纯度标准物质杂质定性鉴定与主成分定量分析  

Qualitative identification of impurities and principal component quantitative analysis of zearalanone on purity certified reference material

作　　者：冯梦雨 刘栓 高燕 周澍堃 国振[1] 李秀琴[1] 张庆合[1] FENG Mengyu;LIU Shuan;GAO Yan;ZHOU Shukun;GUO Zhen;LI Xiuqin;ZHANG Qinghe(National Institute of Metrology,Beijing 100029,China;Beijing University of Chemical Technology,Beijing 100029,China)

机构地区：[1]中国计量科学研究院,北京100029 [2]北京化工大学,北京100029

出　　处：《色谱》2019年第8期911-917,共7页Chinese Journal of Chromatography

基　　金：国家重点研发计划“战略性国际科技创新合作重点专项”(2016YFE0206500)~~

摘　　要：建立了高纯玉米赤霉酮中痕量杂质的液相色谱分离分析方法,进行了标准物质纯度的定量分析。采用超高效液相色谱-二极管阵列检测法(UPLC-DAD)和UPLC-四极杆/静电场轨道阱高分辨质谱技术(UPLC-HRMS)鉴定了玉米赤霉酮原料中3种主要有机杂质(β-玉米赤霉醇、α-玉米赤霉醇和脱水玉米赤霉醇);计算了3种杂质的相对响应因子(0.535 2 、 0.859 4 和 0.697 3 )。基于UPLC-DAD,采用校准因子归一化方法对玉米赤霉酮原料中主成分进行测定,标准物质纯度为99.6%,测量标准偏差为0.01%。该方法可为玉米赤霉酮标准物质的研制提供技术支撑。A liquid chromatography method was established for the determination of zearalanone (ZAN) raw material.The qualitative analysis of ZAN and its trace impurities was performed by ultra performance liquid chromatography-diode array detector (UPLC-DAD) and ultra performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS),and the response factors of each impurity were calculated.The three main organic impurities in the ZAN raw material were identified as β-zearalanol,α-zearalanol and a dehydration product of zearalanol with relative response factors of 0.535 2,0.859 4 and 0.697 3,respectively.The main component of the ZAN raw material was determined by the calibration factor normalization method.The purity of zearalanone was determined to be 99.6% with a standard deviation of 0.01%.This method can provide a technical support for the development of ZAN standard materials.

关 键 词：超高效液相色谱-二极管阵列检测 高分辨质谱 定性鉴定 标准物质 玉米赤霉酮 

分 类 号：O658[理学—分析化学]