药品中核磁共振检测定性能力验证样品制备与评价结果分析

Sample Preparation and Analysis of Verification Results of Qualitative Proficiency Test of Nuclear Magnetic Resonance in Pharmaceuticals

目的:评价参与药品中核磁共振检测定性能力验证实验室的检测能力。方法:制备高纯阿魏酸纯度标准物质;参照国家标准物质研制技术规范采用单因素方差分析考察样品均匀性;采用t检验考察样品分别在高温和光照下储藏7天、14天的运输稳定性,采用标准曲线法考察样品在常温放置12个月的长期稳定性;按照CNAS规定的程序实施本次能力验证。结果:阿魏酸纯度标准物质在均匀性、稳定性方面均能满足药品中核磁共振检测定性能力验证使用的要求。在13家实验室16台仪器的反馈结果中,12家15台仪器的测定结果评定为合格,1家实验室的1台仪器结果为不合格,合格率为93.75%。结论:本次能力验证可以真实地反映参试单位的检测水平,绝大多数参加能力验证的实验室具备了药品中核磁共振检测定性能力。

Objective： To evaluate the testing capacities of laboratories involved in the qualitative proficiency test（PT） of nuclear magnetic resonance in pharmaceuticals. Methods： Purity reference material of high quality ferulic acid was prepared. The homogeneity of the samples was tested by ANOVA according to the technical specifications of national reference material development and t-test was used to investigate the transport stability of the samples stored at high temperature and under light for 7 days and 14 days respectively. The long-term stability of the samples at room temperature for 12 months was investigated by using the standard curve method. This proficiency test was performed according to the CNAS procedures. Results： The homogeneity and stability of ferulic acid purity reference material could meet the requirements of qualitative proficiency test of nuclearmagnetic resonance in pharmaceuticals. Out of the feedback results from 16 instruments in 13 laboratories, results from 15 instruments in 12 laboratories were qualified and results from 1 instrument in 1 laboratory were unqualified. The pass rate was 93.75%. Conclusion： This PT could truly reflect the level of participant laboratories and most laboratories involved in the PT had the qualitative capability of nuclear magnetic resonance testing in pharmaceuticals.