Microsoft Word 伍恒-二校出2626

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1 7 7 Vol. 7 No Journal of Food Safety and Quality Jul., 2016 伍恒, 陈祝康 *, 顾颂青 (, ) 摘要 :,,, ISO/IEC17043 ISO 13528,,, 关键词 : ; ; Discussion on statistical methods used in analytical chemistry proficiency testing both in China and abroad WU Heng, CHEN Zhu-Kang *, GU Song-Qing (Shanghai Institute for Food and Drug Control, Shanghai , China) ABSTRACT: It is very important for the successful implementation of proficiency testing program to select and apply the statistical methods correctly. The domestic and overseas reference protocols for proficiency testing of analytical chemistry were searched, and the critical statistical techniques of each protocol or standard, such as the assigned value, the standard deviation for proficiency assessment, performance statistics and graphical methods were analyzed. It is found that different organizations had similarities as well as characteristics in statistical techniques. The proficiency testing statistical standards or protocols made by these organizations were mostly based on ISO/IEC17043, ISO 13528, but were not the same with varing elaboration, expansion or limitation. The retrieval resources and essential points of the study can provide theory references for organizing proficiency testing program as proficiency testing provider for the first time, and provide proficiency testing statistician more valuable information on the right selection and employment of statistical techniques. KEY WORDS: profiency testing: statistical techniques: profiency testing provider * 通讯作者 :,, great310g@sina.cn *Corresponding author: CHEN Zhu-Kang, Senior Pharmacist, Shanghai Institute for Food and Drug Control, Shanghai , China. great310g@sina.cn

2 7, : 引言,,,,,, (mutual recognition arrangement, MRA),, 2 国内能力验证机构结果统计方法 : (China National Accreditation Service for Conformity Assessment, CNAS) (Certification and Accreditation Administration of the People s Republic of China, CNCA) CNAS CNAS-CL03: 2010 [1] ( B, GB/T B) CNAS-GL02: 2014 [2] ( GB/T-27043, GB/T 28043) GB/T [3] ( ISO13528) GB/T [4] ( ISO/IEC 17043) 4,,, :, ;, ;, D D% Z Z En ξ EZ ;, CNAS-GL02 GB/T GB/T (International Union of Pure and Applied Chemistry, IUPAC) 1, CNAS-GL02; GB/T27043; GB/T Table 1 表 1 国内能力验证结果统计及能力评价相关指南标准的比较 Comparison of relative guidance and standards on statistic treatment of proficiency testing results and performance evaluation in China CNAS-CL03 [1] CNAS-GL02 [2] GB/T28043 [3] GB/T [4] GB/T-27043, A, / / GB/T-27043,,,,

3 国外能力验证机构结果统计方法 : (Asia Pacific Laboratory Accreditation Cooperation, APLAC) (National Association of Testing Authorities, NATA)(Association of Official Agricultural Chemists, AOAC) (The Food and Environment Research Agency, FERA) (International Laboratory Accreditation Cooperation, ILAC) (International Union of Pure and Applied Chemistry, IUPAC), 2 APLAC NATA ILAC ISO 13528: 2005 ISO/IEC 17043: 2010,, 2, 3, AOAC FERA IUPAC 3.1 美国分析化学家协会 (Association of Official Agricultural Chemists, AOAC) AOAC International [15-22] AOAC,,, AOAC, ISO 13528,, ISO Z, 3 Z, 1 表 2 国际化学检测领域能力验证结果统计及能力评价依据的相关指南 Table 2 The international chemical testing guidance on statistic treatment of proficiency testing results and performance evaluation APLAC ISO 13528: 2005 [5] ISO/IEC 17043: 2010 [6] ISO 5725: [7] APLAC PT002 [8] NATA ISO/IEC17043: 2010 AOAC ISO 13528: 2005 FERA ISO/IEC 17043: 2010 Protocol for proficiency testing scheme Part 1-Part 5 [9-13] IUPAC TechnicalReport [14] ILAC ISO/IEC 17043: 2010 IUPAC IUPAC TechnicalReport ISO 13528: 2005 ISO Guide 43( ISO/IEC 17043: 2010 ) Table 3 表 3 国外能力验证机构结果统计及能力评价方法的比较 Comparison of the method of international organizations on statistic treatment of proficiency testing results and performance evaluation AOAC FERA IUPAC / (CRM) CRM (ISO 13528: 2005 ),,, mode / (ISO 13528: 2005 ) (Horwitz ) fitness-for-purpose σ p (Horwitz ), Z Z, Q Z Z L En EZ, Z ξ Z Z 2, 2< Z <3, Z 3

4 7, : 2625 AOAC FERA IUPAC 续表 3,,, / / / Z, Z Z ( ), Schewhart chart J-chart 1 AOAC ZZ Fig. 1 ZZ-score distribution graph of proficiency testing results in the AOAC meat chemistry program Z Z Z Z, Z, Z 50%,,,, 1.5, 3.2 英国环境与科学研究院 (The Food and Environment Research Agency, FERA), (British Central Science Laboratory, CSL),, 2009 CSL FERA (protocol for proficiency testing scheme) 5, common principles FAPAS PT ;, FAPAS (Food analysis performance assessment scheme, ) FEPAS(Food examination performance assessment scheme, ) GeMMA(Scheme the genetically modified materials analysis scheme, ) LEAP(Scheme the laboratory environmental analysis proficiency scheme, ) 指定值的赋值及其不确定度 3,,,,, 3, 表 4 FERA 能力验证草案中指定值不确定度计算方法 Table 4 The methods of determining uncertainty on the assigned value in FERA protocol for proficiency testing scheme X a υ υ= ˆ / Mode υ=smad( )/ n SEM(Mode ) 能力评定标准差的赋值 FERA HorwitZ, ( 3) 能力验证性能统计量及结果评价 FERA, Z Q, Z FERA n

5 Q,,,,, Z Q : Z=(x-x a )/σ p Q=(x-x a )/x a x= ; x a =; Q= σ p = 定量结果的图示法 FERA Z ( 2) 3.3 国际纯粹与应用化学联合会 (International Union of Pure and Applied Chemistry, IUPAC) IUPAC AOAC ISO IUPAC, IUPAC, Z fitness-for-purpose, IUPAC, 指定值的赋值及其不确定度的推算 3,,,, mode, ( ISO13528 [5] C A),,, mode,,,, 15,, IUPAC, 3: 能力评定标准差的赋值方法 HorwitZ, ( 3) 定量结果的评价, : Z L Z ξ En EZ Z L fitness for purpose,,, IUPAC fitness for purpose,,, σ ffp, Z L Z L =(x-x a )/ σ ffp 2 FAPAS A ZZ Fig. 2 ZZ-scores distribution diagram of ochratoxin A in wheat flour for FAPAS proficiency test

6 7, : IUPAC Fig.3 The flow chart of determining the uncertainty on the assigned value in IUPAC technical report ISO ( μ(x a )>0.3σ p ) Z, Z, Z, ξ,, 长期能力评价 Z Z (1) Z Z : 2 SZ, rs Zi / n SZZ Z i i i Z, Z,, (2),, Schewhart chart J-chart, Z, 0 Z ; 2 Z <3, Z 3 J-chart, Z J, J Z J, J 8, If Z 3 then J=8 If 2 Z<3 then J=4 If 1 Z<2 then J=2 If -1<Z<1 then J=0 If -2<Z -1 then J=-2 If -3<Z -2 then J=-4 If Z -3 then J=-8 4 结语,,,

7 IUPAC Fig.4 Schewhart chart in IUPAC technical report 5 IUPAC J-chart Fig 5. J-chart in IUPAC technical report,,,,,, 参考文献 [1] CNAS-CL03 [S]. CNAS-CL03 Accreditation criteria for proficiency testing providers [S]. [2] CNAS-GL02 [S]. CNAS-GL02 Guidance on statistic treatment of proficiency testing results and performance evaluation [S] [3] GB/T [S]. GB/T Statistical methods foruse in proficiency testing by interlaboratory comparisons [S]. [4] GB/T [S]. GB/T Conformity assessment-general requirements for proficiency testing [S]. [5] BS ISO 13528:2005 Statistical methods foruse in proficiency testingbyinterlaboratory comparisons [S]. [6] Proficiency testing scheme providers ISO/IEC standard application document [Z].

8 7, : 2629 [7] ISO 5725: 1994 Accuracy (trueness and precision) of measurement methods and results [Z]. [8] Testing Interlaboratory Comparisons-APLAC PT 002 [Z]. [9] The Food and Environment Research Agency. Protocol for proficiency testing scheme,version 4, Part 1 Common principles [Z]. [10] The Food and Environment Research Agency. Protocol for proficiency testing scheme,version 3, Part 2 FAPAS [Z]. [11] The Food and Environment Research Agency. Protocol for proficiency testing scheme,version 3, Part 3 FEPAS [Z]. [12] The Food and Environment Research Agency. Protocol for proficiency testing scheme,version 3, Part 4 GeMMA Scheme [Z]. [13] The Food and Environment Research Agency. Protocol for proficiency testing scheme,version 4, Part 5 LEAP Scheme [Z]. [14] 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): [15] Report to participants in the AOAC laboratory proficiency testing program, Meat chemistry program [Z]. [16] Report to participants in the AOAC laboratory proficiency testing program, Pathogen-free microbiology program [Z]. [17] Report to participants in the AOAC laboratory proficiency testing program,combination pathogen program in meat matrix, Salmonella, E.coli O157: H7 and L. monocytogenes [Z]. [18] Report to participants in the AOAC laboratory proficiency testing program, Combination pathogen program in meat matrix, Salmonella and L. monocytogenes [Z]. [19] Report to participants in the AOAC laboratory proficiency testing program, Standard microbiology program without E.coli O157:H7&Listeria [Z]. [20] Report to participants in the AOAC laboratory proficiency testing program, Standard microbiology program [Z]. [21] Report to participants in the AOAC laboratory proficiency testing program, Pesticide residues in fruits & vegetables program, [Z]. [22] Report to participants in the AOAC laboratory proficiency testing program, Salmonella in liquid egg program [Z]. [23] FAPAS Proficiency Test Report Ochratoxin A in Wheat Flour [Z]. 作者简介 ( 责任编辑 : 姚菲 ) 伍恒, 硕士, 主要研究方向为食品安全与实验室质量管理 @qq.com 陈祝康, 硕士, 主任药师, 主要研究方向为能力验证计划实施与质量管理 great310g@sina.cn

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Microsoft Word 伍 恒-二校出2626

Microsoft Word 伍恒-二校出2626