药品中重金属及有害元素残留检测能力验证结果评价模式探讨
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摘要
该文旨在探讨药品中重金属及有害元素残留检测能力验证结果评价模式,为残留分析领域的能力验证计划实施和结果评价提供参考。以金银花中镉元素残留量测定能力验证(NIFDC-PT-141)结果为例,采用迭代算法A、四分位法、经验模型法(Horwitz函数),分别计算指定值和能力评定标准差,得出对应的Z值,|Z|≤2表明"满意"; 2<|Z|<3表明"有问题";|Z|≥3表明"不满意"。另外以中位值为指定值,采用百分相对差法(D%)计算,当-16%≤D%≤16%时,评价结果为"满意",否则"不满意"。结果显示,迭代算法A、四分位法统计计算的可疑或不满意的结果中,部分数据的偏离误差在标准规定范围内;而Horwitz函数法评价的满意实验室的结果中,部分数据的偏离误差远远超过了标准规定范围;百分相对差法的评价结果符合痕量分析误差要求,结合重金属及有害元素痕量分析方法的特点,该研究首次将百分相对差法应用于药品中重金属及有害元素残留检测能力验证结果评价,使其评价结果更加合理,对其他能力验证结果评价具有重要的参考意义。
This study aims to explore the evaluation model for the proficiency testing of heavy metal and harmful element residues in pharmaceuticals,and to provide reference for the proficiency testing program and proficiency testing result in the field of residue analysis. The proficiency test result of cadmium determination in honeysuckle as an example. The algorithm A,NIQR,and Horwitz function are used to calculate the assigned value and the standard deviation. Z was obtained at the same time. If | Z | ≤2,the result is satisfactory. If 2< | Z | <3,the result is questionable. If | Z | ≥3,the result is unsatisfactory. In addition,the median value is the assigned value,and deviation(D%) is used. If D% is not more than 16%,the result is satisfactory; if D% is more than 16%,the result is unsatisfactory. After analysis,in the results of questionable or dissatisfied laboratories calculated by algorithm A and NIQR,the deviation error of some data is within the scope of the standard. In the results of the satisfactory laboratory evaluated by the Horwitz function,some data deviation errors far exceed the standard range. The evaluation result of the D% meets the requirements. According to heavy metal and harmful element trace analysis methods,this study is the first to apply D% to the evaluation of the detection ability of heavy metals and harmful elements in pharmaceuticals. This method makes the evaluation result more reasonable,and has important reference significance for the evaluation of other proficiency test results.
This study aims to explore the evaluation model for the proficiency testing of heavy metal and harmful element residues in pharmaceuticals,and to provide reference for the proficiency testing program and proficiency testing result in the field of residue analysis. The proficiency test result of cadmium determination in honeysuckle as an example. The algorithm A,NIQR,and Horwitz function are used to calculate the assigned value and the standard deviation. Z was obtained at the same time. If | Z | ≤2,the result is satisfactory. If 2< | Z | <3,the result is questionable. If | Z | ≥3,the result is unsatisfactory. In addition,the median value is the assigned value,and deviation(D%) is used. If D% is not more than 16%,the result is satisfactory; if D% is more than 16%,the result is unsatisfactory. After analysis,in the results of questionable or dissatisfied laboratories calculated by algorithm A and NIQR,the deviation error of some data is within the scope of the standard. In the results of the satisfactory laboratory evaluated by the Horwitz function,some data deviation errors far exceed the standard range. The evaluation result of the D% meets the requirements. According to heavy metal and harmful element trace analysis methods,this study is the first to apply D% to the evaluation of the detection ability of heavy metals and harmful elements in pharmaceuticals. This method makes the evaluation result more reasonable,and has important reference significance for the evaluation of other proficiency test results.
引文
[1]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.
[2]伍恒,陈祝康,顾颂青.国内外化学检测领域能力验证结果统计方法的探讨[J].食品安全质量检测学报,2016,7(7):2622.
[3] CNAS-GL40:能力验证的选择核查与利用指南[S].2015.
[4] ISO 13528:实验室间比对能力验证用统计方法[S].2015.
[5] CNAS-GL02:能力验证结果的统计处理和能力评价指南[S].2015.
[6]王明娟,何风艳,郑笑为,等.消炎利胆片中穿心莲内酯、脱水穿心莲内酯及其总量测定能力验证项目的结果分析[J].中国药事,2014,28(9):981.
[7]赵新玥,赵文,陈华.pH测定检验能力验证及评价新方法的应用[J].药物分析杂志,2018,38(3):545.
[8]郭晓俊,朱岭峰,徐翀,等.传统统计法与稳健统计法评价医学检验实验室能力验证结果比较[J].检验医学,2017,32(5):435.
[9]何风艳,王明娟,胡晓茹,等.六味安消胶囊含量测定的能力验证研究[J].中国药事,2018,32(8):1120.
[10]张帆,刘胜楠,王海涛,等.能力验证中的稳健统计方法应用浅析[J].标准科学,2018(2):61.
[11]孙海容,李玉武.用经验模型判断能力验证统计分析结果的合理性[J].岩矿测试,2012(6):992.
[12]范玉兰,杨玮,王美华,等.Horwitz方程在比对试验质量评估中的应用[J].劳动医学,2001(4):209.
[13]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(8):809.
[14]乔菲,金红宇,项新华,等.人参中17种有机氯农药残留测定能力验证分析[J].药物分析杂志,2018,38(6):1024.
[15]中国药典.四部[S].2015.
[16]桑国卫.中国药品检验操作规范[M].北京:中国医药科技出版社,2010.
[2]伍恒,陈祝康,顾颂青.国内外化学检测领域能力验证结果统计方法的探讨[J].食品安全质量检测学报,2016,7(7):2622.
[3] CNAS-GL40:能力验证的选择核查与利用指南[S].2015.
[4] ISO 13528:实验室间比对能力验证用统计方法[S].2015.
[5] CNAS-GL02:能力验证结果的统计处理和能力评价指南[S].2015.
[6]王明娟,何风艳,郑笑为,等.消炎利胆片中穿心莲内酯、脱水穿心莲内酯及其总量测定能力验证项目的结果分析[J].中国药事,2014,28(9):981.
[7]赵新玥,赵文,陈华.pH测定检验能力验证及评价新方法的应用[J].药物分析杂志,2018,38(3):545.
[8]郭晓俊,朱岭峰,徐翀,等.传统统计法与稳健统计法评价医学检验实验室能力验证结果比较[J].检验医学,2017,32(5):435.
[9]何风艳,王明娟,胡晓茹,等.六味安消胶囊含量测定的能力验证研究[J].中国药事,2018,32(8):1120.
[10]张帆,刘胜楠,王海涛,等.能力验证中的稳健统计方法应用浅析[J].标准科学,2018(2):61.
[11]孙海容,李玉武.用经验模型判断能力验证统计分析结果的合理性[J].岩矿测试,2012(6):992.
[12]范玉兰,杨玮,王美华,等.Horwitz方程在比对试验质量评估中的应用[J].劳动医学,2001(4):209.
[13]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(8):809.
[14]乔菲,金红宇,项新华,等.人参中17种有机氯农药残留测定能力验证分析[J].药物分析杂志,2018,38(6):1024.
[15]中国药典.四部[S].2015.
[16]桑国卫.中国药品检验操作规范[M].北京:中国医药科技出版社,2010.