甲卡西酮纯度标准物质的研制  

The Development of Methcathinone Certified Reference Materials

作　　者：韦棋 苏福海[1] WEI Qi;SU Fuhai(National Institute of Metrology of China,Beijing,100029)

机构地区：[1]中国计量科学研究院,北京100029

出　　处：《计量科学与技术》2020年第11期10-16,共7页Metrology Science and Technology

基　　金：国家重点研发计划(2018YFC0807301-4)。

摘　　要：针对目前违禁药物成分量检测的需求,研制了甲卡西酮国家级标准物质。通过对经筛选的原料纯品进行液相色谱-质谱(LC-MS)、核磁以及离子色谱定性分析,利用质量平衡法对甲卡西酮原料进行纯度定值。在基于色谱的质量平衡法的基础上优化了检测条件,以液相色谱和气相色谱确定了主成分的含量。综合考虑测定水分、挥发性有机物和ICP-MS对无机元素杂质的测定,得到甲卡西酮纯度定值为99.78%,并进行了均匀性和稳定性实验以及不确定度评定。此方法研制的甲卡西酮纯度标准物质目前已被批准为国家一级标准物质并应用于实际的检测中。To meet the requirement of drug abuse detection,the Certified Reference Materials(CRMs)was developed.The purity of Methcathinone was determined by mass balance method using the liquid chromatography-mass spectrometry(LC-MS),1H Nuclear Magnetic Resonance(1H NMR),and Ion chromatography(IC)for qualitative analysis of crude materials.Based on the aforementioned method,the detection conditions were optimized,and the purity of Methcathinone was determined by high-performance liquid chromatography(HPLC)and gas chromatography(GC).Considering the determination of moisture,volatile organic compounds,and inorganic element impurities,the main component purity of Methcathinone was determined at 99.78%by ICP-MS,and the uniformity and stability experiments,as well as the uncertainty evaluation were carried out.The newly developed CRM has been approved as a national CRM and used in actual testing.

关 键 词：甲卡西酮 标准物质 色谱法 质量平衡法 不确定度评定 

分 类 号：TQ421.31[化学工程] O657[理学—分析化学] D918.9[理学—化学]