依据国际纯粹与应用化学联合会(IUPAC) 国际能力验证活动的规则以及中国合格评定国家认可委员会(CNAS) 规定的程序，对参与药品中氮含量测定能力验证的实验室进行能力评价，并提供技术分析和建议。采用单因子方差分析对制备的能力验证样品( 甘氨酸) 进行均匀性检验，采用t 检验考察样品稳定性，结果均符合要求。采用中位值和标准化四分位距法的稳健统计方法，用Z 比分数评价各参加实验室的测试结果。报告检测结果的84 家实验室中，76 家的结果为“满意”，4 家的结果为“有问题”，4 家的结果为“不满意”。本次能力验证研究客观评价了实验室药品中氮含量的检测能力，提供了全面深入的技术分析，帮助实验室查找原因，采取措施，提高检测能力。
Abstract
According to the protocol of International Union of Pure and Applied Chemistry (IUPAC) and procedure of China National Accreditation Service for Conformity Assessment (CNAS), the pharmaceutical nitrogen determination capacity of the laboratories which participated in the proficiency-testing was evaluated, and some technical analyses and advices were provided. The one-way ANOVA was used to evaluate the homogeneity of the proficiencytesting samples (glycine), whose stability was confirmed with t-test. All results conformed to the requirements. The median value and the normalized interquartile range (NIQR) of robust statistical method was adopted and Z-scores were used to evaluate the results from each laboratory. Among 84 laboratories which reported their results, 76 laboratories'
results were ''satisfactory'', four were ''questionable'', and four were ''unsatisfied''. The in-depth comprehensive technical analysis could help the laboratories to find out the causes, take measures, and improve the detection capability.
关键词
甘氨酸 /
氮含量测定 /
实验室能力验证
{{custom_keyword}} /
Key words
glycine /
nitrogen determination /
proficiency-testing for laboratory
{{custom_keyword}} /
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] 武晗燕, 苏 芳, 郭 雷. 自动定氮仪测定人血白蛋白中的总氮含量[J] 生命科学仪器, 2013, (6): 41—42.
[2] ISO/IEC 17025: 2005 General requirements for the competence of testing and calibration laboratories [S] . Geneva: Switzerland, 2005.
[3] 中国合格评定国家认可委员会. CNAS-RL02, 能力验证规则[S]. 2010.
[4] 中国合格评定国家认可委员会. CNAS-GL02, 能力验证结果的统计处理和能力评价指南[S]. 2014.
[5] 中国合格评定国家认可委员会. CNAS-GL03, 能力验证样品均匀性和稳定性评价指南[S]. 2006. [6] ISO 13528: 2005 Statistical methods for use in proficiency testing by interlaboratory comparisions [S] . Geneva: Switzerland, 2005.
[7] Thompson M, Ellison SLR, Wood R. The international harmonized protocol for the proficiency testing of analytical chemistry laboratories [J]. Pure Appl Chem, 2006, 78(1):145—196.
[8] 王林波, 杨美成, 翟培军, 等. 药品检测能力验证常用统计方法的探讨[J]. 中国药事, 2012, 26(8): 809—813.
[9] 李 晶, 项新华, 张河战. 实验室比对统计分析方法的比较[J]. 中国药学杂志, 2016, 51(2): 139—143.
[10] 中国药品生物制品检定所. 中国药品检验标准操作规范[ Ｍ ]. 2010 年版, 北京: 中国医药科技出版社, 2010:181—183.
[11] GB/T 28043-2011. 利用实验室间比对进行能力验证的统计方法[S]. 2011.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}
基金
中国合格评定国家认可委员会项目(CNAS T0804)
{{custom_fund}}
PDF(6695 KB)
