苯甲醇含量测定能力验证研究
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摘要
目的:评价参与药用辅料苯甲醇含量测定的实验室的能力。方法:依据CNAS-RL02《能力验证规则》和ISO/IEC 17043《合格评定能力验证的通用要求》实施实验室能力验证活动。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,根据CNAS-GL03《能力验证样品均匀性和稳定性评价指南》,对检测结果进行单因子方差分析和t检验分析,结果显示样品均匀性和稳定性均符合要求。以结果的中位值作为测试样品含量的指定值,以整体标准差作为能力评判标准差,根据GB/T 28043-2011/ISO13528:2005,利用稳健统计分析,用Z比分数进行结果判定,对190家参加实验室的报告结果进行评价。结果与结论:190家实验室中有4家实验室的检测结果可疑,4家实验室结果不满意,整体满意率95.8%;通过本次能力验证数据分析和研究,多数参加能力验证苯甲醇含量测定的检测结果满意,不满意结果有仪器、称量、人员等方面引入的误差,并要求相关实验室结合自身情况查找原因进行整改。
Objective: To evaluate the capability of the laboratory involved in the determination of Benzyl Alcohol content in pharmaceutical excipients. Methods: The laboratory's capability-verification activities are conducted based on the CNAS-RL02 Rules for Proficiency Testing and ISO/IEC 17043 Conformity Assessment--General Requirements for Proficiency Testing. ANOVA and t-test analysis were used to evaluate the homogeneity and stability of the testing results, which were confirmed with the requirements according to CNAS-GL03 Guidance on Evaluating the Homogeneity and Stability of Samples Used for Proficiency Testing. The robust statistical method and the Z score results were used to analyze the results of the 190 laboratories' reports. Results and Conclusion: Among the 190 laboratories, 4 laboratories' results were suspicious and 4 laboratories' results were unsatisfactory. The overall satisfaction rate was 95.8%. Some errors in instruments, weighing, personnel,etc. were found, though most of the laboratories results for the determination of Benzyl Alcohol content were satisfactory through the proficiency testing. The relevant laboratories should find out the reasons and rectify the errors according to their own conditions.
Objective: To evaluate the capability of the laboratory involved in the determination of Benzyl Alcohol content in pharmaceutical excipients. Methods: The laboratory's capability-verification activities are conducted based on the CNAS-RL02 Rules for Proficiency Testing and ISO/IEC 17043 Conformity Assessment--General Requirements for Proficiency Testing. ANOVA and t-test analysis were used to evaluate the homogeneity and stability of the testing results, which were confirmed with the requirements according to CNAS-GL03 Guidance on Evaluating the Homogeneity and Stability of Samples Used for Proficiency Testing. The robust statistical method and the Z score results were used to analyze the results of the 190 laboratories' reports. Results and Conclusion: Among the 190 laboratories, 4 laboratories' results were suspicious and 4 laboratories' results were unsatisfactory. The overall satisfaction rate was 95.8%. Some errors in instruments, weighing, personnel,etc. were found, though most of the laboratories results for the determination of Benzyl Alcohol content were satisfactory through the proficiency testing. The relevant laboratories should find out the reasons and rectify the errors according to their own conditions.
引文
[1]中国合格评定国家认可委员会.CNAS-RL01:2011实验室认可规则[S].2011.
[2]滕俊江,乔艳辉.相转移催化合成苯甲醇的工艺研究[J].自动化应用,2006,(3):35-36.
[3]郭海东.两步法合成苯甲醇的工艺研究[D].南京:南京工业大学,2004.
[4]葛海生,刘元瑞,赵康虎,等.HPLC法测定克林霉素磷酸酯注射液中抑菌剂苯甲醇的含量[J].中国药房,2010,(25):2376-2377.
[5]李茜,刘英.HPLC法检测醋酸奥曲肽注射剂中5种抑菌剂[J].中国药事,2017,(1):62-68.
[6]刘青,陈文锐,吴宏中,等.气相色谱法测定化妆品中的防腐剂苯甲醇和苯氧基乙醇[J].检验检疫科学,2002,12(1):34-35.
[7]周耀斌,彭亚锋,雷涛,等.应用毛细管气相色谱技术测定化妆品中防腐剂苯甲醇含量[J].香料香精化妆品,2009,(4):9-10.
[8]王高峰,苏桂兰,胡冠时,等.利多卡因和苯甲醇对人体肌注青霉素的药动学及生物利用度的影响[J].现代应用药学,1989,(1):34-35.
[9]中国药典:二部[M].北京:中国医药科技出版社,2010.
[10]中国药典:四部[M].北京:中国医药科技出版社,2015.
[11]中国合格评定国家认可委员会.CNAS-RL02:2010能力验证规则[S].2010.
[12]中国合格评定国家认可委员会.CNAS-GL02:2014能力验证结果的统计处理和能力评价指南[S].2014.
[13]中国合格评定国家认可委员会.CNAS-GL03:2006能力验证样品均匀性和稳定性评价指南[S].2006.
[14]李慧义,张启明.欧洲药典引湿性试验方法简介[J].中国药品标准,2003,4(6):59,62.
[15]GB/T 28043-2011/ISO13528:2005利用实验室间比对进行能力验证的统计方法[S].2005.
[16]PDA.数据处理和峰的积分[S]//PDA TR 80实验室数据完整性管理体系,2018.
[2]滕俊江,乔艳辉.相转移催化合成苯甲醇的工艺研究[J].自动化应用,2006,(3):35-36.
[3]郭海东.两步法合成苯甲醇的工艺研究[D].南京:南京工业大学,2004.
[4]葛海生,刘元瑞,赵康虎,等.HPLC法测定克林霉素磷酸酯注射液中抑菌剂苯甲醇的含量[J].中国药房,2010,(25):2376-2377.
[5]李茜,刘英.HPLC法检测醋酸奥曲肽注射剂中5种抑菌剂[J].中国药事,2017,(1):62-68.
[6]刘青,陈文锐,吴宏中,等.气相色谱法测定化妆品中的防腐剂苯甲醇和苯氧基乙醇[J].检验检疫科学,2002,12(1):34-35.
[7]周耀斌,彭亚锋,雷涛,等.应用毛细管气相色谱技术测定化妆品中防腐剂苯甲醇含量[J].香料香精化妆品,2009,(4):9-10.
[8]王高峰,苏桂兰,胡冠时,等.利多卡因和苯甲醇对人体肌注青霉素的药动学及生物利用度的影响[J].现代应用药学,1989,(1):34-35.
[9]中国药典:二部[M].北京:中国医药科技出版社,2010.
[10]中国药典:四部[M].北京:中国医药科技出版社,2015.
[11]中国合格评定国家认可委员会.CNAS-RL02:2010能力验证规则[S].2010.
[12]中国合格评定国家认可委员会.CNAS-GL02:2014能力验证结果的统计处理和能力评价指南[S].2014.
[13]中国合格评定国家认可委员会.CNAS-GL03:2006能力验证样品均匀性和稳定性评价指南[S].2006.
[14]李慧义,张启明.欧洲药典引湿性试验方法简介[J].中国药品标准,2003,4(6):59,62.
[15]GB/T 28043-2011/ISO13528:2005利用实验室间比对进行能力验证的统计方法[S].2005.
[16]PDA.数据处理和峰的积分[S]//PDA TR 80实验室数据完整性管理体系,2018.