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作 者:卢蕾[1,2] 李秀琴[2] 邵春发[2] 李英杰[1] 张庆合[2]
机构地区:[1]齐齐哈尔大学,齐齐哈尔161006 [2]中国计量科学研究院,北京100013
出 处:《化学分析计量》2011年第2期4-8,共5页Chemical Analysis And Meterage
基 金:国家自然科学基金项目(20775075);国家科技基础性工作专项项目(2008FY130200)
摘 要:研制了呋喃它酮的代谢产物5-甲基吗啡-3-氨基-2-唑烷基酮(AMOZ)的标准物质。采用红外光谱和液相色谱-质谱法对AMOZ进行了定性鉴定,建立并优化了用于AMOZ主成分定值的高效液相色谱-二极管阵列检测器法(HPLC-DAD)、气相色谱-氢火焰离子化检测器法(GC-FID)和差示扫描量热法(DSC)。将卡尔费休法和热重分析法分别用于水分和无机杂质的分析。均匀性和稳定性检验结果表明,研制的AMOZ标准物质均匀性良好,稳定时间为7个月。当AMOZ纯度值为99.28%时,扩展不确定度为0.50%(k=2)。3-amino-5-marpholinomethyl-2-oxazolidinoneone reference material was prepared. IR spectrum and LC - MS method were used to identify the structure of the material. High performance liquid chromatography - diode array detector ( HPLC - DAD), gas chromatography - hydrogen flame ionization detector ( GC - FID) and differential scanning calorimeter (DSC) method were established and the principal component values were determined by these methods. Karl fischer method and thermo gravimetric analyzer were used to determine moisture and inorganic impurities. Test results showed that3-amino-5-marpholinomethyl-2-oxazolidinone reference material was homogeneous. It was found to be stable at least 7 months. The certified purity value of 3-amino-5-marpholinomethyl-2-oxazolidinone was 99.28% , the expanded uncertainty was 0.50% (k = 2).
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