药品中水分测定的实验室能力验证

目的: 评价参与能力验证实验室的药品中水分测定能力.方法: 依据ISO13528:2005、国际能力验证活动的规则(IUPAC)以及CNAS(中国合格评定国家认可委员会)规定的程序进行本次能力验证.结果: 采用单因子方差分析对制备的测试样品进行均匀性检验,采用ｔ检验对样品进行稳定性考察,均符合要求.采用Z比分数评价各参加实验室的测试结果,各参加实验室结果的中位值作为测试样品水分的指定值,以标准化四分位距(NIQR)作为变动性度量值(目标标准偏差).报告检测结果的166家实验室中,139家的结果为"满意",16家的结果"可疑",11家的结果为"不满意".结论: 通过研究,制备了均匀性和稳定性均符合能力验证要求的测试样品,并采用适当的统计方法评估了实验室药品中水分的检测能力.

Objective: To evaluate the capacity of the laboratories which participated in the proficiency testing for moisture determination in pharmaceuticals. Methods: The study was performed according to ISO13528:2005, protocol of International Union of Pure and Applied Chemistry(IUPAC)and procedure of China National Accreditation Service for Conformity Assessment(CNAS). Results: The one-way ANOVA was used to evaluate the homogeneity of the test samples, whose stability was confirmed with t-test.All results conformed to the requirements.Z-scores were used to evaluate results from each laboratory with the median of all results as the indicated value.NIQR was used as the variable metric value(target standard deviation).Among the 166 laboratories which reported their results, 139 laboratories had satisfactory results, 16 suspectable, and 11 unsatisfactory. Conclusion: Test samples were prepared with the homogeneity and the stability meeting the requirements of proficiency testing, and the capacity of the laboratories for moisture determination in pharmaceuticals was evaluated correctly by the suitable statistical method.

[1] LI Yun-long(李云龙).The SOP of Chinese Drug Test(中国药品检验标准操作规范)[M].Beijing(北京):China Medical Science Press(中国医药科技出版社),2010:223
[2] ISO/IEC 17025:2005 General Requirements for the Competence of Testing and Calibration Laboratories(检测和校准实验室能力的通用要求)[S].2005
[3] CNAS-RL02:2010 Rules for Proficiency Testing(能力验证规则)[S].2010
[4] CNAS-GL02:2006 Guidance on Statistic Treatment of Proficiency Testing Results and Performance Evaluation(能力验证结果的统计处理和能力评价指南)[S].2006
[5] CNAS-GL03:2006 Guidance on Evaluating the Homogeneity and Stability of Samples Used for Proficiency Testing(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 Inproficiency Testing by Interlaboratory Comparisions(通过实验室间比对进行能力验证的统计方法)[S].2005
[7] CNAS-CL03:2006 Accreditation Criteria for Providers of Proficiency Testing Schemes(能力验证计划提供者认可准则)[S].2010
[8] GB/T 28043-2011 Statistical Methods for Use Inproficiency Testing by Interlaboratory Comparisions(通过实验室间比对进行能力验证的统计方法)[S].2011
[9] GB/T 4091-2001 Shewhart Control Charts(常规控制图)[S].2001
[10] GB/T 27025-2008 General Requirements for the Competence of Testing and Calibration Laboratories(检测和校准实验室能力的通用要求)[S].2008
[11] 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
[12] WANG Jun(王君),HU Chang-qin(胡昌勤),HU Yu-zhu(胡育筑).Estimation of uncertainty on moisture determination by Karl Fischer's method(费休氏水分测定法的不确定度评定)[J].Chin J Pharm Anal(药物分析杂志),2006,26(5):674