EUPT-Panel. DG SANTE Mrs. Almut Bitterhof Mrs. Veerle Vanheusden

Transcription

1 EUPT-FV17 Results

2 ORGANISING GROUP Amadeo R. Fernández-Alba Milagros Mezcua Octavio Malato Carmen Ferrer STATISTICAL GROUP Carmelo Rodríguez QUALITY CONTROL GROUP Antonio Valverde Stewart Reynolds EUPT-Panel DG SANTE Mrs. Almut Bitterhof Mrs. Veerle Vanheusden ADVISORY GROUP Michelangelo Anastassiades Miguel Gamón Magnus Jezussek André de Kok Ralf Lippold Sonja Masselter Tuija Pihlström Mette Erecius Poulsen Darinka Stajnbaher Finbarr O Regan Philippe Gros

3 Broccoli

4 Organic broccolis were grown in a greenhouse in Almería. Spain.

5

6 Before harvest the broccolis were treated with commercial formulations

7 Commercial products used to treat the sample Pesticide Type Commercial Product Bupirimate Commercial Formulation Nimrod Quattro Carbendazim Commercial Formulation Bengu 50 Flow Diazinon Commercial Formulation Zoogama-D Difenoconazole Commercial Formulation Core Diflubenzuron Commercial Formulation Dimilin 25 Methoxyfenozide Commercial Formulation Runner Pendimetalin Commercial Formulation Stonp LE Permethrin Commercial Formulation Defendog Spinosad Commercial Formulation Spintor 480 SG Thiabendazole Commercial Formulation Textar 60 Trifloxystrobin Commercial Formulation Flint

8 Preparation of the test item

9 EUPT-FV17 Results Participation No of Labs

10 EUPT-FV17 Results Country No. of Labs Country No. of Labs Country No. of Labs Austria 2 Hungary 4 Serbia 2 Belgium 3 Iceland 1 Singapore 1 Brazil 2 Ireland 1 Slovakia 2 Bulgaria 2 Italy 23 Slovenia 3 China 1 Jamaica 1 Spain 32 Costa Rica 1 Kenya 2 Sweden 2 Croatia 6 Latvia 1 Switzerland 2 Cyprus 1 Lebanon 1 Thailand 1 Czech Republic 3 Lithuania 1 The Netherlands 4 Denmark 2 Luxembourg 1 Turkey 1 Egypt 1 Norway 1 United Kingdom 4 Estonia 2 Peru 1 Uruguay 1 Finland 2 Poland 11 France 7 Portugal 2 Germany 29 Romania 4 Greece 10 Saudi Arabia 1 Total No. of Labs = 185 Total No. of Non-EU countries Labs = 17 Total No. of Countries = 44 EU countries. EFTA countries. Other countries

11 Participation Total No. of Labs = 185 EU/EFTA Labs = 168 Other countries Labs = 17 Total No. of Countries = 44 EU/EFTA countries = 30 Other countries = 14 (27 EU + 3 EFTA + 2 Candidate countries + 12 other countries)

12 183 pesticides 3-hydroxy-carbofuran Acephate Acetamiprid Acrinathrin Aldicarb Aldicarb Sulfone Aldicarb Sulfoxide Dichlorvos Azinphos-methyl Dicloran Azoxystrobin Dicofol Benfuracarb Diethofencarb Benomyl Difenoconazole Bifenthrin Diflubenzuron Bitertanol Dimethoate Boscalid Dimethomorph Bromopropylate Bromuconazole Diniconazole Bupirimate Diphenylamine Buprofezin Endosulfan alpha Cadusafos Endosulfan beta Carbaryl Endosulfan sulfate Carbendazim EPN Carbofuran Epoxiconazole Carbosulfan Ethion Chlorfenapyr Ethirimol Chlorfenvinphos Ethoprophos Chlorobenzilate Etofenprox Chlorothalonil Fenamidone Chlorpropham (only parent compound) Chlorpyrifos Chlorpyrifos-methyl Clofentezine (only parent Fenarimol compound) Deltamethrin Demeton-S-methylsulfone Desmethyl-pirimicarb Diazinon Dichlofluanid (only parent compound) Fenamiphos Fenamiphos sulfone Fenamiphos sulfoxide Fenpropimorph Fenpyroximate Fenthion Fenthion oxon Target List Fenthion oxon sulfone Metconazole Fenthion oxon sulfoxidemethamidophos Fenthion sulfone Methidathion Fenthion sulfoxide Methiocarb Fenvalerate and Esfenvalerate Methiocarb sulfone Fipronil (only parent compound) Fludioxonil Flufenoxuron Fluopicolide Dimethylaminosulfotoluidide Fluopyram (DMST) Fluquinconazole Flusilazole Flutolanil Flutriafol Fosthiazate Hexaconazole Hexythiazox Imazalil Imidacloprid Parathion-methyl Indoxacarb (Indoxacarb as sum of the isomers S and R) Iprodione Iprovalicarb Isocarbophos Isofenphos-methyl Isoprothiolane Kresoxim-methyl Mandipropamid Prothioconazole (Prothioconazole-desthio) Mepanipyrim (only parent compound) Metaflumizone Metalaxyl and metalaxyl-m Methiocarb sulfoxide Methomyl Methoxyfenozide Monocrotophos Myclobutanil Omethoate Orthophenylphenol Oxadixyl Oxamyl Oxydemeton-methyl Paclobutrazole Paraoxon-methyl Parathion-ethyl Penconazole Pencycuron Pendimethalin Permethrin Phenthoate Phosalone Phosmet Phosmet oxon Phoxim Pirimicarb Pirimiphos-methyl Profenofos Propargite Propiconazole Propyzamide Prothiofos Pyraclostrobin Pyridaben Pyrimethanil Pyriproxyfen Quinoxyfen Spinosad (sum of spinosyn A and spinosyn Spirodiclofen Spiroxamine Tau-Fluvalinate Tebuconazole Tebufenozide Tebufenpyrad Teflubenzuron Tefluthrin Terbuthylazine Tetraconazole Tetradifon Thiabendazole Thiacloprid Thiamethoxam Thiodicarb 12 New compounds Thiophanate-methyl Tolclofos-methyl Tolylfluanid Triadimefon Triadimenol Triazophos Trichlorfon (only parent compound) Trifloxystrobin Triflumuron Trifluralin Clothianidin Fenazaquin Lambda-Cyhalothrin Cyfluthrin (cyfluthrin incl. Fenbuconazole other mixtures of constituent Linuron isomers (sum of isomers)) Fenhexamid Lufenuron Cypermethrin Fenitrothion Malaoxon Cyproconazole Fenoxycarb Malathion Triticonazole Cyprodinil Prochloraz (only parent compound) Fenpropathrin Vinclozolin (only parent compound) Procymidone EUPT-FV17 Results Zoxamide Stuttgart 1 st October 2015

13 Bupirimate Pesticides used for the treatment Carbendazim Diazinon Difenoconazole Diflubenzuron Pendimetalin Permethrin* Spinosad Thiabendazole Trifloxystrobin Methoxyfenozide Total: 11 ALL INCLUDED IN MACP COMMISSION IMPLEMENTING REGULATION (EU) No 400/2014 of 22 April 2014 concerning a coordinated multiannual control programme of the Union for 2015, 2016 and 2017 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin. * New in the target list

14 Calendar ACTIVITY - Publishing the Target Pesticide List. Calendar and Matrix on the Web page. DATE 15 th December Receiving Application Form from invited laboratories. 12 th Jan-13 th Feb Specific Protocol published on the Web site. 23 rd Feb 2015 at the latest - Deadline for receiving Laboratory scope: Form 0 23 rd Feb-6 th March Sample distribution. 16 th March Deadline for receiving sample acceptance: Form 1 20 th March Deadline for receiving results: Forms 2. 3 and 4 13 th April Filling in Form 5 20 th -24 th April Preliminary Report: only results. no statistical treatment. May Final Report distributed to the Laboratories. December 2015

15 Homogeneity The homogeneity in the treated sample was studied using the 2006 Harmonised Protocol. All the pesticides passed the homogeneity test

16 Homogeneity mg/kg

17 Stability ISO Annex B Sub-sample1 Sub-sample 2 Sub-sample 3 Sub-sample 4 Sub-sample 5 Sub-sample 6

18 Stability ISO Annex B 1 st Analysis - prior to the sample shipment 2 nd Analysis - after the deadline for reporting results 3 rd Analysis - reproducing the delivery conditions that the samples experienced during 48 hours x 1 -y i 0.3 σ All the pesticides passed the stability test

19 EUPT-FV17 Results Results

20 Assigned values EU/EFTA Laboratories Pesticides Robust mean (mg/kg) Uncertainty (mg/kg) Spinosad Pendimethalin Diazinon Bupirimate Permethrin Diflubenzuron Methoxyfenozide Trifloxystrobin Carbendazim Difenoconazole Thiabendazole

21 EU/EFTA Laboratories mg/kg Pesticides Robust mean (mg/kg) Spinosad Pendimethalin Diazinon Bupirimate 0.16 Permethrin 0.17 Diflubenzuron 0.32 Methoxyfenozide 0.35 Trifloxystrobin 0.47 Carbendazim 0.51 Difenoconazole 0.53 Thiabendazole 1.90

22 EU/EFTA Laboratories mg/kg mg/kg Pesticides Robust mean (mg/kg) Spinosad Pendimethalin Diazinon Bupirimate 0.16 Permethrin 0.17 Diflubenzuron 0.32 Methoxyfenozide 0.35 Trifloxystrobin 0.47 Carbendazim 0.51 Difenoconazole 0.53 Thiabendazole 1.90

23 EU/EFTA Laboratories mg/kg mg/kg > mg/kg Pesticides Robust mean (mg/kg) Spinosad Pendimethalin Diazinon Bupirimate 0.16 Permethrin 0.17 Diflubenzuron 0.32 Methoxyfenozide 0.35 Trifloxystrobin 0.47 Carbendazim 0.51 Difenoconazole 0.53 Thiabendazole 1.90

24 Distribution of data-histograms Bupirimate Carbendazim EU/EFTA Laboratories Frequency Mean: mg/kg Frequency Mean: mg/kg mg/kg Diazinon Difenocozole mg/kg Frequency Mean: mg/kg Mean: mg/kg Frequency Mean: mg/kg mg/kg mg/kg

25 Distribution of data-histograms Diflubenzuron Methoxyfenozide EU/EFTA Laboratories Frequency Mean: mg/kg Frequency Mean: mg/kg mg/kg Pendimethalin mg/kg Permethrin Frequency Mean: mg/kg Frequency Mean: mg/kg mg/kg mg/kg

26 Distribution of data-histograms Spinosad Thiabendazole EU/EFTA Laboratories 50 Mean: mg/kg 80 Mean: 1.90 mg/kg Frequency Frequency mg/kg Trifloxystrobin mg/kg Mean: mg/kg Frequency mg/kg

27 Dispersion of Results EU/EFTA Laboratories Pesticides MRRL (mg/kg) Robust mean (mg/kg) CV (%) Bupirimate Carbendazim Diazinon Difenoconazole Diflubenzuron Methoxyfenozide Pendimethalin Permethrin Spinosad (sum of spinosyn A a spinosyn D. expr. as spinosad) Thiabendazole Trifloxystrobin

28 Dispersion of Results EU/EFTA Laboratories

29 EU/EFTA Laboratories Pesticides No. of Reported Results No. of False Negative Results No. of Not Analysed Results Percentage of Reported Results (out of 165) Bupirimate Carbendazim Diazinon Difenoconazole Diflubenzuron Methoxyfenozide Pendimethalin Permethrin Spinosad Thiabendazole Trifloxystrobin

30 EUPT-FV17 Results z-scores

31 z-scores classification EU/EFTA Laboratories Acceptable Questionable Unacceptable

32 EU/EFTA Laboratories Pesticides Robust Mean (mg/kg) % Acceptable z-scores % Questionable z-scores % Unacceptable z-scores Bupirimate Carbendazim Diazinon Difenoconazole Diflubenzuron Methoxyfenozide Pendimethalin Permethrin Spinosad (sum of spinosyn A a spinosyn D. expr. as spinosad) Thiabendazole Trifloxystrobin

33 Bupirimate Robust Mean: mg/kg 93.5 % Acceptable 1.9 % Questionable 4.5 % Unacceptable 5,0 4,0 3,0 2,0 1,0 0,0-1,0-2,0-3,0 or L LC or G GC or B Both -4,0 0 False Negative -5,0 Lab020 Lab112 Lab023 Lab174 Lab042 Lab043 Lab145 Lab061 Lab091 Lab007 Lab003 Lab001 Lab126 Lab046 Lab087 Lab141 Lab123 Lab128 Lab068 Lab032 Lab167 Lab064 Lab060 Lab010 Lab045 Lab078 Lab140 Lab138 Lab129 Lab097 Lab072 Lab029 Lab052 Lab143 Lab086 Lab083 Lab077 Lab047 Lab176 Lab098 Lab016 Lab114 Lab100 Lab116 Lab088 Lab070 Lab159 Lab109 Lab074 Lab041 Lab057 Lab095 Lab179 Lab021 Lab006 Lab084 Lab015 Lab014 Lab144 Lab108 Lab067 Lab142 Lab110 Lab099 Lab094 Lab089 Lab085 Lab076 Lab065 Lab027 Lab013 Lab136 Lab080 Lab079 Lab022 Lab082 Lab081 Lab105 Lab169 Lab162 Lab149 Lab168 Lab121 Lab106 Lab051 Lab185 Lab146 Lab113 Lab102 Lab058 Lab056 Lab040 Lab035 Lab018 Lab171 Lab030 Lab002 Lab183 Lab181 Lab147 Lab024 Lab135 Lab130 Lab157 Lab137 Lab062 Lab160 Lab073 Lab182 Lab151 Lab031 Lab161 Lab038 Lab107 Lab101 Lab111 Lab132 Lab048 Lab134 Lab133 Lab117 Lab092 Lab049 Lab044 Lab037 Lab034 Lab012 Lab009 Lab166 Lab120 Lab069 Lab103 Lab170 Lab054 Lab036 Lab026 Lab119 Lab124 Lab053 Lab163 Lab152 Lab148 Lab019 Lab154 Lab131 Lab115 Lab011 Lab005 Lab156 Lab093 Lab071 Lab025 Lab017 Lab158

34 Carbendazim 5,0 Robust Mean: mg/kg 86.4 % Acceptable 5.7 % Questionable 7.9 % Unacceptable 4,0 3,0 2,0 1,0 0,0-1,0-2,0-3,0 or L LC or G GC or B Both -4,0 0 False Negative -5,0 Lab142 Lab110 Lab103 Lab150 Lab166 Lab085 Lab173 Lab054 Lab052 Lab145 Lab088 Lab061 Lab132 Lab113 Lab021 Lab022 Lab057 Lab106 Lab121 Lab176 Lab116 Lab071 Lab037 Lab062 Lab136 Lab035 Lab120 Lab068 Lab080 Lab041 Lab124 Lab074 Lab029 Lab047 Lab073 Lab005 Lab058 Lab109 Lab082 Lab078 Lab056 Lab036 Lab100 Lab083 Lab181 Lab161 Lab099 Lab114 Lab094 Lab089 Lab098 Lab182 Lab050 Lab108 Lab091 Lab006 Lab069 Lab020 Lab010 Lab162 Lab023 Lab140 Lab123 Lab159 Lab144 Lab084 Lab148 Lab027 Lab102 Lab053 Lab137 Lab117 Lab097 Lab032 Lab147 Lab086 Lab030 Lab060 Lab185 Lab138 Lab072 Lab070 Lab018 Lab170 Lab007 Lab174 Lab171 Lab042 Lab040 Lab065 Lab049 Lab026 Lab126 Lab076 Lab046 Lab079 Lab048 Lab095 Lab077 Lab044 Lab013 Lab167 Lab043 Lab087 Lab156 Lab105 Lab160 Lab067 Lab014 Lab009 Lab179 Lab135 Lab024 Lab012 Lab019 Lab183 Lab107 Lab064 Lab034 Lab031 Lab011 Lab093 Lab134 Lab025 Lab111 Lab168 Lab143 Lab101 Lab133 Lab003 Lab015 Lab154 Lab128 Lab169 Lab017 Lab038 Lab119 Lab045 Lab112 Lab158

35 Diazinon 5,0 Robust Mean: mg/kg 92.6 % Acceptable 4.3 % Questionable 3.1 % Unacceptable 4,0 3,0 2,0 1,0 GGGGGGL 0,0-1,0-2,0-3,0 ** or L LC or G GC or B Both -4,0 *False Negative -5,0 Lab107 Lab141 Lab112 Lab060 Lab074 Lab061 Lab057 Lab050 Lab006 Lab070 Lab007 Lab116 Lab118 Lab068 Lab140 Lab065 Lab095 Lab085 Lab016 Lab143 Lab123 Lab161 Lab103 Lab129 Lab030 Lab176 Lab080 Lab181 Lab167 Lab164 Lab156 Lab114 Lab089 Lab084 Lab056 Lab032 Lab023 Lab047 Lab154 Lab097 Lab046 Lab020 Lab003 Lab067 Lab108 Lab094 Lab091 Lab058 Lab136 Lab100 Lab099 Lab098 Lab069 Lab064 Lab010 Lab079 Lab159 Lab139 Lab138 Lab135 Lab109 Lab024 Lab018 Lab151 Lab130 Lab106 Lab086 Lab081 Lab078 Lab073 Lab162 Lab072 Lab053 Lab027 Lab137 Lab147 Lab171 Lab040 Lab132 Lab082 Lab076 Lab051 Lab042 Lab036 Lab014 Lab002 Lab185 Lab119 Lab115 Lab093 Lab087 Lab034 Lab021 Lab157 Lab126 Lab121 Lab111 Lab052 Lab035 Lab145 Lab142 Lab083 Lab045 Lab182 Lab179 Lab149 Lab048 Lab174 Lab127 Lab022 Lab013 Lab105 Lab113 Lab102 Lab029 Lab041 Lab088 Lab049 Lab012 Lab160 Lab001 Lab144 Lab183 Lab168 Lab152 Lab134 Lab117 Lab054 Lab039 Lab037 Lab031 Lab019 Lab009 Lab062 Lab120 Lab163 Lab128 Lab124 Lab101 Lab038 Lab015 Lab043 Lab008 Lab133 Lab077 Lab131 Lab092 Lab044 Lab026 Lab005 Lab075 Lab148 Lab166 Lab071 Lab173 Lab011 Lab025 Lab150 Lab017 Lab158 Lab169 Lab110

36 Difenoconazole 5,0 Robust Mean: mg/kg 97.4 % Acceptable 1.3 % Questionable 1.3 % Unacceptable 4,0 3,0 2,0 1,0 GG L L L L L G L B G 0,0-1,0-2,0-3,0 or L LC or G GC or B Both * -4,0 *False Negative -5,0 Lab006 Lab117 Lab179 Lab016 Lab141 Lab058 Lab182 Lab167 Lab144 Lab156 Lab070 Lab007 Lab110 Lab089 Lab068 Lab123 Lab162 Lab092 Lab086 Lab018 Lab002 Lab181 Lab140 Lab109 Lab044 Lab143 Lab030 Lab095 Lab115 Lab084 Lab049 Lab176 Lab098 Lab119 Lab061 Lab099 Lab088 Lab042 Lab003 Lab041 Lab020 Lab161 Lab075 Lab010 Lab100 Lab047 Lab091 Lab116 Lab081 Lab056 Lab045 Lab126 Lab074 Lab057 Lab076 Lab080 Lab112 Lab106 Lab097 Lab102 Lab157 Lab159 Lab170 Lab062 Lab078 Lab065 Lab052 Lab046 Lab022 Lab142 Lab050 Lab138 Lab038 Lab017 Lab027 Lab136 Lab064 Lab137 Lab069 Lab174 Lab146 Lab072 Lab040 Lab013 Lab082 Lab014 Lab145 Lab021 Lab108 Lab128 Lab035 Lab029 Lab107 Lab151 Lab053 Lab015 Lab121 Lab105 Lab113 Lab093 Lab085 Lab166 Lab067 Lab135 Lab060 Lab077 Lab171 Lab120 Lab147 Lab054 Lab034 Lab024 Lab012 Lab036 Lab083 Lab073 Lab103 Lab132 Lab111 Lab101 Lab154 Lab160 Lab087 Lab032 Lab031 Lab183 Lab168 Lab048 Lab037 Lab185 Lab079 Lab005 Lab019 Lab043 Lab009 Lab148 Lab133 Lab131 Lab124 Lab026 Lab001 Lab169 Lab163 Lab114 Lab173 Lab094 Lab071 Lab011 Lab025 Lab158 Lab164 Lab059

37 Diflubenzuron 5,0 Robust Mean: mg/kg 84.1 % Acceptable 8.0 % Questionable 8.0 % Unacceptable 4,0 3,0 2,0 1,0 L L L 0,0-1,0-2,0-3,0 or L LC or G GC or B Both * * -4,0 *False Negative -5,0 Lab074 Lab054 Lab043 Lab136 Lab036 Lab057 Lab038 Lab058 Lab183 Lab142 Lab181 Lab185 Lab041 Lab089 Lab077 Lab169 Lab094 Lab156 Lab123 Lab182 Lab022 Lab014 Lab179 Lab047 Lab068 Lab029 Lab143 Lab040 Lab011 Lab092 Lab018 Lab088 Lab111 Lab050 Lab073 Lab072 Lab070 Lab167 Lab098 Lab010 Lab176 Lab093 Lab030 Lab109 Lab083 Lab046 Lab062 Lab097 Lab078 Lab048 Lab132 Lab087 Lab060 Lab009 Lab076 Lab147 Lab101 Lab086 Lab049 Lab042 Lab119 Lab137 Lab085 Lab064 Lab103 Lab069 Lab144 Lab159 Lab021 Lab024 Lab084 Lab067 Lab061 Lab095 Lab108 Lab005 Lab012 Lab100 Lab102 Lab128 Lab080 Lab032 Lab013 Lab135 Lab082 Lab171 Lab015 Lab124 Lab037 Lab035 Lab027 Lab020 Lab161 Lab044 Lab031 Lab120 Lab160 Lab168 Lab053 Lab026 Lab166 Lab126 Lab091 Lab079 Lab025 Lab162 Lab112 Lab105 Lab071 Lab116 Lab173 Lab158 Lab019

38 Methoxyfenozide 5,0 Robust Mean: mg/kg 96.1 % Acceptable 3.1 % Questionable 0.8 % Unacceptable 4,0 3,0 2,0 1,0 L L L L L L L 0,0-1,0-2,0-3,0 or L LC or G GC or B Both -4,0 0 False Negative -5,0 Lab021 Lab182 Lab136 Lab124 Lab141 Lab040 Lab112 Lab060 Lab015 Lab050 Lab140 Lab076 Lab041 Lab113 Lab068 Lab044 Lab007 Lab102 Lab179 Lab030 Lab074 Lab123 Lab116 Lab089 Lab078 Lab058 Lab181 Lab070 Lab012 Lab052 Lab057 Lab169 Lab176 Lab077 Lab086 Lab056 Lab018 Lab109 Lab064 Lab143 Lab047 Lab159 Lab069 Lab042 Lab098 Lab036 Lab156 Lab010 Lab144 Lab084 Lab126 Lab046 Lab061 Lab100 Lab127 Lab105 Lab097 Lab072 Lab032 Lab027 Lab108 Lab020 Lab167 Lab091 Lab014 Lab071 Lab049 Lab037 Lab029 Lab013 Lab011 Lab101 Lab067 Lab048 Lab017 Lab145 Lab106 Lab087 Lab110 Lab082 Lab147 Lab128 Lab095 Lab080 Lab142 Lab024 Lab062 Lab053 Lab183 Lab137 Lab135 Lab043 Lab171 Lab093 Lab038 Lab121 Lab009 Lab035 Lab168 Lab132 Lab005 Lab073 Lab174 Lab114 Lab107 Lab148 Lab083 Lab022 Lab088 Lab120 Lab161 Lab185 Lab085 Lab119 Lab111 Lab160 Lab092 Lab025 Lab054 Lab026 Lab019 Lab162 Lab079 Lab103 Lab034 Lab094 Lab158 Lab045

39 Pendimethalin 5,0 Robust Mean: mg/kg 92.2 % Acceptable 5.9 % Questionable 2.0 % Unacceptable 4,0 3,0 2,0 1,0 L L L 0,0-1,0-2,0-3,0 * or L LC or G GC or B Both -4,0 *False Negative -5,0 Lab166 Lab016 Lab136 Lab074 Lab119 Lab113 Lab093 Lab141 Lab123 Lab057 Lab070 Lab087 Lab064 Lab007 Lab065 Lab138 Lab091 Lab068 Lab116 Lab072 Lab046 Lab161 Lab114 Lab098 Lab164 Lab095 Lab088 Lab024 Lab079 Lab112 Lab109 Lab108 Lab001 Lab050 Lab042 Lab002 Lab181 Lab159 Lab110 Lab100 Lab092 Lab089 Lab060 Lab032 Lab023 Lab067 Lab043 Lab014 Lab080 Lab176 Lab167 Lab107 Lab086 Lab078 Lab156 Lab099 Lab081 Lab076 Lab010 Lab139 Lab083 Lab058 Lab052 Lab018 Lab162 Lab130 Lab048 Lab151 Lab146 Lab082 Lab061 Lab040 Lab022 Lab171 Lab135 Lab128 Lab035 Lab013 Lab047 Lab137 Lab085 Lab036 Lab027 Lab017 Lab106 Lab084 Lab062 Lab012 Lab185 Lab182 Lab154 Lab134 Lab103 Lab094 Lab045 Lab041 Lab179 Lab160 Lab097 Lab053 Lab105 Lab102 Lab149 Lab144 Lab124 Lab056 Lab168 Lab026 Lab044 Lab157 Lab121 Lab069 Lab021 Lab009 Lab147 Lab145 Lab142 Lab111 Lab143 Lab183 Lab132 Lab126 Lab117 Lab101 Lab031 Lab019 Lab077 Lab038 Lab029 Lab133 Lab127 Lab120 Lab030 Lab005 Lab073 Lab049 Lab075 Lab034 Lab170 Lab037 Lab152 Lab131 Lab071 Lab039 Lab015 Lab003 Lab054 Lab148 Lab115 Lab011 Lab025 Lab158 Lab169

40 Permethrin 5,0 Robust Mean: mg/kg 93.5 % Acceptable 2.6 % Questionable 3.9 % Unacceptable 4,0 3,0 2,0 1,0 GGG 0,0-1,0-2,0-3,0 or L LC or G GC or B Both * -4,0 *False Negative -5,0 Lab166 Lab016 Lab007 Lab163 Lab095 Lab112 Lab092 Lab141 Lab058 Lab181 Lab176 Lab123 Lab043 Lab074 Lab146 Lab003 Lab047 Lab081 Lab109 Lab050 Lab014 Lab182 Lab089 Lab056 Lab091 Lab167 Lab051 Lab067 Lab061 Lab116 Lab161 Lab087 Lab024 Lab114 Lab070 Lab083 Lab072 Lab138 Lab065 Lab080 Lab082 Lab064 Lab046 Lab042 Lab057 Lab128 Lab108 Lab076 Lab060 Lab151 Lab084 Lab068 Lab044 Lab041 Lab023 Lab179 Lab086 Lab040 Lab098 Lab174 Lab147 Lab088 Lab156 Lab149 Lab100 Lab169 Lab131 Lab127 Lab117 Lab110 Lab107 Lab099 Lab035 Lab027 Lab018 Lab013 Lab137 Lab102 Lab045 Lab002 Lab079 Lab030 Lab062 Lab059 Lab001 Lab162 Lab097 Lab078 Lab032 Lab026 Lab010 Lab142 Lab077 Lab160 Lab144 Lab015 Lab159 Lab135 Lab075 Lab105 Lab053 Lab171 Lab130 Lab124 Lab022 Lab164 Lab005 Lab132 Lab012 Lab133 Lab054 Lab037 Lab029 Lab021 Lab034 Lab073 Lab048 Lab094 Lab143 Lab168 Lab157 Lab185 Lab152 Lab134 Lab118 Lab113 Lab039 Lab009 Lab121 Lab103 Lab069 Lab126 Lab017 Lab049 Lab031 Lab036 Lab093 Lab139 Lab173 Lab148 Lab145 Lab071 Lab120 Lab111 Lab183 Lab115 Lab038 Lab008 Lab052 Lab011 Lab025 Lab119 Lab019

41 Spinosad 5,0 Robust Mean: mg/kg 90.6 % Acceptable 1.6 % Questionable 7.9 % Unacceptable 4,0 3,0 2,0 1,0 L L 0,0-1,0-2,0-3,0 * * or L LC or G GC or B Both -4,0 *False Negative -5,0 Lab076 Lab050 Lab042 Lab091 Lab043 Lab044 Lab036 Lab127 Lab018 Lab021 Lab094 Lab169 Lab070 Lab057 Lab156 Lab040 Lab148 Lab012 Lab167 Lab143 Lab035 Lab159 Lab089 Lab027 Lab182 Lab113 Lab032 Lab179 Lab141 Lab095 Lab056 Lab064 Lab060 Lab030 Lab137 Lab132 Lab102 Lab098 Lab047 Lab112 Lab100 Lab084 Lab074 Lab014 Lab003 Lab067 Lab116 Lab061 Lab046 Lab108 Lab073 Lab058 Lab010 Lab162 Lab097 Lab086 Lab053 Lab007 Lab160 Lab024 Lab126 Lab022 Lab181 Lab106 Lab023 Lab072 Lab041 Lab176 Lab171 Lab136 Lab013 Lab183 Lab135 Lab121 Lab105 Lab049 Lab017 Lab174 Lab110 Lab101 Lab078 Lab069 Lab038 Lab062 Lab080 Lab009 Lab161 Lab147 Lab144 Lab107 Lab088 Lab083 Lab168 Lab093 Lab111 Lab092 Lab085 Lab133 Lab123 Lab120 Lab048 Lab029 Lab077 Lab015 Lab185 Lab124 Lab109 Lab068 Lab019 Lab011 Lab087 Lab119 Lab026 Lab025 Lab034 Lab005 Lab037 Lab031 Lab079 Lab142 Lab082 Lab071 Lab114 Lab103 Lab158 Lab128 Lab054

42 Thiabendazole 5,0 Robust Mean: 1.90 mg/kg 93.1 % Acceptable 1.4 % Questionable 5.5 % Unacceptable 4,0 3,0 2,0 1,0 L L G L 0,0-1,0-2,0-3,0 or L LC or G GC or B Both ** -4,0 *False Negative -5,0 Lab142 Lab150 Lab019 Lab094 Lab156 Lab058 Lab021 Lab182 Lab181 Lab061 Lab095 Lab173 Lab158 Lab022 Lab102 Lab057 Lab043 Lab076 Lab082 Lab016 Lab011 Lab086 Lab029 Lab077 Lab098 Lab169 Lab126 Lab032 Lab070 Lab087 Lab007 Lab167 Lab013 Lab015 Lab080 Lab078 Lab171 Lab124 Lab072 Lab123 Lab097 Lab053 Lab084 Lab046 Lab179 Lab141 Lab047 Lab036 Lab159 Lab109 Lab062 Lab014 Lab006 Lab138 Lab054 Lab041 Lab005 Lab176 Lab121 Lab091 Lab040 Lab117 Lab060 Lab140 Lab010 Lab048 Lab089 Lab113 Lab064 Lab020 Lab144 Lab088 Lab135 Lab120 Lab031 Lab100 Lab030 Lab101 Lab038 Lab145 Lab133 Lab044 Lab018 Lab083 Lab147 Lab050 Lab056 Lab108 Lab170 Lab009 Lab074 Lab067 Lab052 Lab161 Lab157 Lab160 Lab143 Lab099 Lab107 Lab068 Lab037 Lab137 Lab106 Lab105 Lab012 Lab024 Lab111 Lab073 Lab069 Lab027 Lab017 Lab035 Lab128 Lab034 Lab112 Lab103 Lab001 Lab042 Lab174 Lab026 Lab025 Lab132 Lab079 Lab136 Lab071 Lab114 Lab049 Lab148 Lab093 Lab045 Lab168 Lab183 Lab185 Lab154 Lab085 Lab023 Lab162 Lab003 Lab151 Lab059 Lab116 Lab065 Lab127 Lab163 Lab110

43 Trifloxystrobin 5,0 Robust Mean: 0.47 mg/kg 96.7 % Acceptable 1.3 % Questionable 2.0 % Unacceptable 4,0 3,0 2,0 1,0 0,0-1,0-2,0-3,0 or L LC or G GC or B Both -4,0 0 False Negative -5,0 Lab021 Lab058 Lab181 Lab182 Lab129 Lab085 Lab007 Lab006 Lab095 Lab068 Lab167 Lab091 Lab040 Lab141 Lab059 Lab114 Lab056 Lab161 Lab050 Lab045 Lab074 Lab016 Lab138 Lab065 Lab032 Lab109 Lab027 Lab022 Lab024 Lab042 Lab060 Lab030 Lab110 Lab046 Lab140 Lab156 Lab086 Lab162 Lab088 Lab123 Lab010 Lab169 Lab159 Lab084 Lab064 Lab136 Lab076 Lab100 Lab176 Lab116 Lab089 Lab070 Lab067 Lab044 Lab099 Lab152 Lab097 Lab052 Lab018 Lab112 Lab078 Lab014 Lab126 Lab061 Lab002 Lab137 Lab082 Lab081 Lab034 Lab057 Lab072 Lab108 Lab003 Lab171 Lab130 Lab146 Lab080 Lab036 Lab035 Lab041 Lab087 Lab107 Lab151 Lab142 Lab092 Lab013 Lab144 Lab077 Lab128 Lab043 Lab017 Lab154 Lab147 Lab117 Lab029 Lab143 Lab038 Lab106 Lab079 Lab103 Lab031 Lab160 Lab069 Lab179 Lab105 Lab062 Lab093 Lab185 Lab157 Lab054 Lab120 Lab121 Lab083 Lab001 Lab102 Lab101 Lab049 Lab037 Lab168 Lab047 Lab145 Lab012 Lab132 Lab174 Lab134 Lab005 Lab183 Lab073 Lab098 Lab048 Lab148 Lab133 Lab115 Lab113 Lab009 Lab135 Lab015 Lab025 Lab124 Lab026 Lab119 Lab111 Lab170 Lab094 Lab011 Lab163 Lab053 Lab075 Lab019 Lab023 Lab158 Lab127

44 EUPT-FV17 Results Combined z-scores

45 Average of Squared z-scores AZ Good 2.0 < AZ 2 < 3.0 Satisfactory AZ Unsatisfactory

46 AZ 2 Representation NRLs OfLs EU/EFTA Laboratories Category A: 68.5 % of the EU/EFTA Laboratories EUPT-FV16: 59% (113 Laboratories out of 165) 80 % Good 7 % Satisfactory 13 % Unsatisfactory EUPT-FV16: 92 % Good 5 % Satisfactory 3 % Unsatisfactory

47 False Positives EU/EFTA Laboratories 6 different laboratories from EU/EFTA countries reported 6 pesticides as false positives

48 False Positives EU/EFTA Laboratories Laboratory Code Pesticide Concentration (mg/kg) Determination Technique RL (mg/kg) MRRL (mg/kg) Lab027 Bromopropylate GC-MS/MS Lab098 Bromopropylate GC-MS Lab051 Bromopropylate GC-MS Lab173 Carbaryl GC-MS/MS Lab158 Fenpropathrin GC-MS Lab164 Kresoxim-methyl GC-MS/MS Lab173 Orthophenylphenol 2.95 HPLC-UV Lab173 Tetradifon GC-MS/MS

49 GC-MS or GC-MS/MS False Positives HPLC-UV EU/EFTA Laboratories Bromopropylate Orthophenylphenol Carbaryl Fenpropathrin Kresoxim-methyl Tetradifon

50 Bromopropylate in FV17 EUPT-FV17 Blank 10 µg/kg Std in Broccoli EUPT-FV17 Sample Ratio: 7.1% Ratio: 0.9% MRM1: 341 > 185 MRM2: 341 > 155

51 Bupirimate Carbendazim Diazinon Difenoconazole Diflubenzuron Methoxyfenozide Pendimetalin Permethrin Spinosad Thiabendazole Trifloxystrobin Cyprodinil Ethirimol Concentrations below MRRL (0.01 mg/kg) Fludioxonil

52 Overview of the EUPTs-FV Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

53 Proficiency Tests - History PTs on MRM in FV Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

54 Proficiency Tests - History ISO/IEC Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

55 Participant countries-other countries (18) Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

56 EUPT-FV1 to EUPT-FV17 in numbers EUPT Nº Matrices Overview of the EUPTs-FV Nº of Participants Nº of Possible Pesticides Nº of pesticides evaluated in test item 1 Pepper Apple Cucumber Orange Lettuce Tomato Grape Aubergine Strawberry Carrot Cauliflower Leek Mandarin Pear Potato Pepper Overview of the EUPTs-FV 17 Broccoli Stuttgart 1 st October 2015

57 Acephate Difenoconazole Kresoxim-methyl Pirimicarb Acetamiprid Diflubenzuron Lambda-Cyhalothrin Pirimphos-methyl Acrinathrin Dimethoate Linuron Prochloraz Aldicarb(sum) Diphenilamine Malathion Procydimone Amitraz (DMPF&DMF) Dithiocarbamates(CS2) Mecarbam Propoxur Azinphos-methyl Endosulfan Metalaxyl Propyzamide Azoxystrobin EPN Metamidophos Prothiofos Bifenthrin Fenamiphos Methidathion Pyraclostrobin Boscalid Fenamiphos sulfone Methiocarb sum Pyridaben Bromopropylate Fenamiphos sulfoxide Methiocarb Pyrimethanil Bupirimate Ethion Methomyl Pyriproxifen Buprofezin Fenhexamid Methoxyfenozide Quinoxyfen Cadusafos Fenitrothion Methyl-Tiophanate Quintozene Captan Fenpropathrin Mevinphos Spinosad Carbaryl Fludioxinil Monocrotophos Spirodiclofen Carbendazim Flufenoxuron Myclobutanil Tebuconazole Carbofuran sum Fluopicolide Omethoate Tetraconazole Chlorpropham Flutolanil Ortophenilphenol Thiabendazole Chlorpyrifos Folpet Oxamyl Thiacloprid Chlorpyrifos-methyl Fosthiazate Oxydemeton-methyl Tolclofos-methyl Chlothalonil Hexythiazox Parathion Tolyfluanid Cypermethrin Imazalil Penconazole Triadimenol Cyprodinil Imidacloprid Pencycuron Triazophos Delthamethrin Indoxacarb Pendimethalin Trifloxystrobin Diazinon Iprodione Permethrin Triflumuron Dichlofluanid Iprovalicarb Phosalone Vinclozolin Dicofol Isofenphos-methyl Phosmet Overview of the EUPTs-FV Overview of the EUPTs-FV Pesticides Used to Treat the Sample in last ten EUPT-FVs Stuttgart 1 st October 2015

58 Summary of Results Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

59 Extraction methods Number of results reported by extraction method Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

60 Extraction methods Classification of z-scores by extraction method Acetone QuE C he R S AcE t Acceptable Questionable Inacceptable Acceptable Questionable Inacceptable Acceptable Questionable Inacceptable EUPT FV16 91,7 7,7 0,6 93,9 2,9 3,2 95,5 2,9 1,6 EUPT FV15 93,0 3,4 3,6 87,7 4,2 8,2 88,6 3,9 7,5 EUPT FV14 96,2 1,8 2 93,9 3,1 3 94,3 3 2,7 Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

61 60 Dispersion of Results (RSD, %) (Qn RSD, %) Overview of the EUPTs-FV 20 25% FFP RSD 10 0 Overview of the EUPTs-FV EUPT 1 EUPT 2 EUPT 3 EUPT 4 EUPT 5 EUPT 6 EUPT 7 EUPT 8 EUPT 9 EUPT 10 EUPT 11 EUPT 12 EUPT 13 EUPT 14 EUPT 15 EUPT 16 Stuttgart 1 st October 2015

62 Dispersion of Results (RSD, %) No. Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

63 Classification of z-scores 1776 results 1950 results 1590 results 2363 results 1555 results 2254 results 2209 results 2486 results 3133 results Overview of the EUPTs-FV % Acceptable Questionable Unacceptable Overview of the EUPTs-FV Stuttgart 1 st October 2015

64 Laboratories in Category A 71 % 68.5 % 51 % 51 % 51 % 56 % 52 % 52 % 59 % % 45 % Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

65 False Negatives and Positives Overview of the EUPTs-FV Overview of the EUPTs-FV Stuttgart 1 st October 2015

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