美雄酮甲醇溶液标准物质的定值及不确定度评定

The Certification and Uncertainty Evaluation of Methandienone Methanol Solution

针对目前食品中兴奋剂类药物检测的需求,研制了美雄酮甲醇溶液国家级标准物质。通过对经筛选的市售原料纯品进行液相色谱-质谱和红外光谱定性分析后,研究利用高效液相色谱法(HPLC)和差示扫描量热法(DSC)对美雄酮蛋白同化类固醇类兴奋剂原料进行纯度定值。利用HPLC在245nm监测,以水(含0.1%HAc)+乙腈=50+50(体积比)作为流动相进行等度洗脱,以Inertsil ODS-SP(250mm×4.6mm,5μm)进行分离,测定了液相条件下的美雄酮固体的纯度。综合考虑DSC对美雄酮纯度测定的结果,得到美雄酮纯度定值为99.6%。同时,分别利用热重分析法和电感耦合等离子体质谱法测定水分和无机元素杂质的含量。美雄酮溶液标准物质经重量-重量法配制后,进行均匀性和稳定性实验,浓度赋值后进行了不确定度评定。研制的美雄酮溶液标准物质目前已被批准为国家二级标准物质并应用于实际的检测中。

To meet the requirement of doping detection in food,methandienone solution certified reference material（CRM） was developed.After the qualitative analysis on commercial material by LC-MS and IR,the purity of methandienone was certified by HPLC and DSC.The purity of methandienone was 99.6% determined by HPLC at 245nm with mobile phase of water（containing 0.1% HAc） and acetonitrile（50 /50,V /V） and Inertsil ODS-SP（250mm × 4.6mm,5μm）.At the same time,water content and inorganic impurity were determined by TGA and ICP-MS.Methandienone solution CRM was prepared by gravity method.After the homogeneity and stability testing,the concentration of methandienone solution CRM was certified and the uncertainty was evaluated.The CRM has been approved as national CRM and applied in the doping detection.