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

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。

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

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 0.5352, 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.