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.
Se Pu. 2019 Aug 8;37(8):911-917. doi: 10.3724/SP.J.1123.2019.04028.
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 -zearalanol, -zearalanol and a dehydration product of zearalanol with relative response factors of 0.5352, 0.8594 and 0.6973, 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.
建立了一种液相色谱法用于测定玉米赤霉烯酮（ZAN）原料药。采用超高效液相色谱 - 二极管阵列检测器（UPLC - DAD）和超高效液相色谱 - 高分辨率质谱（UPLC - HRMS）对ZAN及其痕量杂质进行定性分析，并计算各杂质的响应因子。ZAN原料药中的三种主要有机杂质被鉴定为α-玉米赤霉醇、β-玉米赤霉醇和玉米赤霉醇的脱水产物，其相对响应因子分别为0.5352、0.8594和0.6973。采用校正因子归一化法测定ZAN原料药的主成分。玉米赤霉烯酮的纯度测定为99.6%，标准偏差为0.01%。该方法可为ZAN标准物质的研制提供技术支持。
