药品中水分测定的实验室能力验证

Laboratory proficiency testing for moisture determination in pharmaceuticals

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,proto- col 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 re- sults, 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.