羟苯苄酯含量测定能力验证研究

Proficiency-testing of determination for benzyl hydroxybenzoate contents

目的:通过对辅料羟苯苄酯含量测定能力验证项目研究,评价分析各实验室的检验检测能力。方法:依据中国合格评定国家认可委员会能力验证规则(CNAS-RL02)和国家标准化管理委员会下达的《合格评定能力验证的通用要求》(ISO/IEC 17043)运作该实验室能力验证活动,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,根据中国合格评定国家认可委员会能力验证样品均匀性和稳定性评价指南(CNAS-GL03),对检测结果进行单因子方差分析、0. 3σ检验及t检验的结果对样品均匀性和稳定性进行评价,均符合要求。采用适当的统计方法评估了实验室对辅料羟苯苄酯含量的检测能力,采用Z比分数评价各参加实验室的测试结果,以结果的中位值作为测试样品含量的指定值,以标准化四分位距作为能力评判标准差,根据GB/T 28043-2011/ISO13528:2005及中国合格评定国家认可委员会能力验证结果的统计处理和能力评价指南(CNAS-GL02:2014),采用稳健统计分析方法。结果:167个单位参加实验室报告的结果进行统计分析,其中5个单位的检测结果比较可疑,12个单位结果不满意,总体满意率89. 82%。结论:大多数参加实验室都能较好掌握羟苯苄酯含量测定的方法,但部分单位由于平时接触此方法较少,需要进一步熟悉仪器和方法的要求。

Objective:To evaluate the laboratories’capacity by the proficiency-testing for assay-determination of benzyl hydroxybenzoate,one of the pharmaceutical excipients.Methods:The study was performed according to CNAS-RL02 and ISO/IEC 17043 to evaluate the laboratories which participated in the proficiency-testing.Testing samples were prepared with the homogeneity and stability meeting the requirements of proficiency-testing.The oneway ANOVA was used to evaluate the homogeneity of the test samples,whose stability was confirmed with t-test according to CNAS-GL03.The ability of laboratory to detect the content of benzyl hydroxybenzoate was assessed by appropriate statistical methods.The test results of the participating laboratories were evaluated by Z-score.The median of the test results was used as the specified value of the content of the test samples,and the NIQR was used as the standard deviation of the ability evaluation.The ability of the laboratory was tested based on GB/T 28043-2011/ISO13528:2005 and the National Accreditation Committee for Qualification Assessment of China.Guidelines for Statistical Processing and Capability Evaluation of Evidence Results(CNAS-GL02:2014),and robust statistical analysis was adopted.Results:Among 167 laboratories which reported their results,150 laboratories’results were satisfactory,5 were questionable,and 12 were unsatisfied.Overall,the satisfaction rate remains 89.82%.Conclusion:Most of the participating laboratories have a good grasp of the method for the determination of benzylhydroxybenzoate content,but some laboratories need to be more familiar with the requirements of the instrument and method.