摘要
目的对研制的二乙酰吗啡盐酸盐标准物质进行定值,并评定定值结果的不确定度。方法采用定量核磁共振法和质量平衡法进行定值;采用液质联用法用于有机物杂质的定性分析,采用电感耦合等离子质谱法、离子色谱法、顶空-气质联用法和卡尔费休滴定法测定无机阳离子、阴离子、挥发性有机溶剂残留和水分等杂质的含量。结果定量核磁共振法的纯度为95.6%,不确定度为0.13%;质量平衡法的纯度为95.3%,不确定度为0.93%。结论二乙酰吗啡盐酸盐标准物质的纯度值为95.6%,扩展不确定度为1.2%(k=2)。
Objective To characterize the prepared diacetylmorphine hydrochloride reference material, and to evaluate the uncertainty of assessment of purity. Methods Diacetylmorphine hydrochloride was characterized by both quantitative-NMR (qNMR) and mass balance method. The organic impurities were identified by LC/MS-IT-TOF, and the contents of inorganic cations and anions, residual of volatile organic solvents and water in the reference material were assayed by ICP-MS, ion chromatography, Head-space GC-MS, Karl-Fischer titration methods, resPectively. Results The qNMR purity was calculated to be 95.6% with standard uncertainty of 0.13%, while the mass-balance purity was 95.3 % with standard uncertainty of 0.93 %. Conclusion The certified purity value of diacetylmorphine hydrochloride was 95.6%, with the expanded uncertainty of 1.2 % (k= 2).
出处
《刑事技术》
2013年第5期9-14,共6页
Forensic Science and Technology
关键词
二乙酰吗啡盐酸盐
标准物质
定值
定量核磁共振法
质量平衡法
不确定度评定
Diamorphine hydrochloride
reference material
characterization
quantitative nuclear magnetic resonance (qN-MR)
mass balance
uncertainty evaluation