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Home , Acetamiprid, Tetramethrin

Results of EUPT-CF10 Incurred and spiked pesticides in rye

Mette Erecius Poulsen Holte, 20 September 2016 PTs on cereals/feed

2016 EUPT-CF10 Test material Rye flour Participants 178 (160) Compulsory target pesticides 134 Voluntary target pesticides 7 Incurred pesticides 10 Spiked pesticides 8 Total no. of pesticides 18

National Food Institute, Technical University of Denmark Advisory Group Quality Group Amadeo R. Fernández-Alba Antonio Valverde André de Kok Stewart Reynolds Antonio Valverde Magnus Jezussek Michelangelo Anastassiades Miguel Gamón Organising team at EURL Philippe Gros Mette Erecius Poulsen Ralf Lippold Susan Strange Herrmann Sonja Masselter Parvaneh Hajeb Stewart Reynolds Merete B. Ludwigsen Tuija Pihlström Lisbet Pilhkjær Finbarr Oregan Jens-Ole Frimann

National Food Institute, Technical University of Denmark National Food Institute, Technical University of Denmark Activity Dates Announcement Calendar December 2015 Target Pesticide List

EUPT-Registration Website 11 January 2016

Deadline for registration 1 February 2016

Release of Specific Protocol 29 February 2016

Distribution of Test items 7 March 2016

Deadline for Receipt and Acceptance of Test Materials within 24 hr on reciept 11 April 2016 Deadline for Result Submission at 13.00 CET Deadline for submission of additional method information for 15 April 2015 false negative results Preliminary Report (only compilation of results) 30 May 2015

Final Report December 2015

National Food Institute, Technical University of Denmark Target list - new pesticides and voluntary compounds

• From DIRECTIVE 2002/32/EC • • Biphenyl • Voluntary: • Bromuconazole • , cis- • • Chlordane, oxy • • Chlordane, trans- • Cymoxanil • • • • Famoxadone • Heptachlorepoxid-cis • Flutolanil • Heptachlorepoxid-trans • • Pencycuron • Propamocarb • Tau-Fluvalinate • • Tetraconazole •

National Food Institute, Technical University of Denmark Difenoconazole Prothioconazole-desthio Acetamiprid Iprodione Pyraclostrobin Aldrin Isocarbophos Pyrimethanil Azinphos-methyl Diniconazole Isoprothiolane Quinoxyfen Azoxystrobin -alpha Isoproturon Spiromesifen Endosulfan-beta Kresoxim-methyl Spiroxamine Biphenyl Endosulfan-sulfate Lambda- Tau-Fluvalinate Bixafen Epoxiconazole Tebuconazole Boscalid Linuron Bromuconazole Ethirimol Tefluthrin Buprofezin Famoxadone Terbuthylazine Fenbuconazole Mandipropamid Tetraconazole Carbendazim Fenhexamid Metconazole Tetramethrin Methacrifos Thiabendazole Carbofuran, 3-hydroxy Fenpropidin Methamidophos Carboxin Fenpropimorph Chlorantraniliprole Metolachlor Thiodicarb Fenthion- Metrafenone Thiophanate-methyl Chlorpropham (parent compound only) Fenthion-oxon-sulfone Metribuzin Triadimefon Fenthion-oxon-sulfoxide Triadimenol Chlorpyrifos-methyl Fenthion-sulfone Oxydemeton-methyl Triazophos Fenthion-sulfoxide Paclobutrazol Tricyclazole (sum of isomers) and Trifloxystrobin Cymoxanil (parent compound only) Penconazole Trifluralin (sum of isomers) Flonicamid Pencycuron Triticonazole Cyproconazole Fludioxonil Pendimethalin Vinclozolin (parent compound only) Cyprodinil Fluopyram (sum of isomers) DDD- p,p' Fluquinconazole Phenylphenol-ortho Voluntary DDE- p,p' Flusilazole Chlordane, cis- DDT- o,p' Flutolanil Chlordane, oxy DDT- p,p' Flutriafol Pirimicarb-desmethyl Chlordane, trans- -cis Fluxapyroxad Pirimiphos-methyl Endrin Demeton-S-methylsulfone HCH-alpha Prochloraz (parent compound only) Heptachlor HCH-beta Procymidone Heptachlorepoxid-cis Hexaconazole Propamocarb Heptachlorepoxid-trans National Food Institute, Technical University of Denmark Dieldrin Imazalil Propiconazole Participation Country # labs Country # labs Country # labs Albania 1 France 8 Poland 16 Argentina 1 Germany 24 Portugal 2 Australia 1 Greece 3 Romania 9 Austria 2 Hungary 4 Serbia 2 Belgium 3 Iceland 1 Singapore 1 Brazil 3 India 2 Slovakia 2 Bulgaria 2 Indonesia 1 Slovenia 5 China 1 Ireland 1 Spain 22 Croatia 7 Israel 1 Sweden 2 Cyprus 2 Italy 25 Switzerland 1 Czech Republic 3 Latvia 1 Tanzania 2 Denmark 1 Lithuania 1 Thailand 3 Egypt 1 Luxembourg 1 United Kingdom 3 Estonia 1 Netherlands 6 Finland 2 Norway 2 Total 178

National Food Institute, Technical University of Denmark Participation Country # labs Country # labs Country # labs Albania 1 France 8 Poland 16 Argentina 1 Germany 24 Portugal 2 Australia 1 Greece 3 Romania 9 Austria 2 Hungary 4 Serbia 2 Belgium 3 Iceland 1 Singapore 1 Brazil 3 India 2 Slovakia 2 Bulgaria 2 Indonesia 1 Slovenia 3 China 1 Ireland 1 Spain 22 Croatia 7 Israel 1 Sweden 2 Cyprus 2 Italy 25 Switzerland 1 Czech Republic 3 Latvia 1 Tanzania 2 Denmark 1 Lithuania 1 Thailand 1 Egypt 1 Luxembourg 1 United Kingdom 3 Estonia 1 Netherlands 6 Finland 2 Norway 2 Total 178

National Food Institute, Technical University of Denmark Rye

• Grown in Denmark in 2015

• Field treated by Aarhus University, Research Department Flakkebjerg

National Food Institute, Technical University of Denmark Pesticides in test material

Pesticide Field application Spike in laboratory Formulation or standard Azoxystrobin x Amistar Bixafen x Aviator Boscalid x Viverda Buprofezin x Analytical standard Carbendazim x Benlate Cypermethrin x x Cyperb Epoxiconazole x Viverda Fenpropidin x Tern Fluopyram x Propulse Isocarbophos x Analytical standard Metrafenone x Flexity Pencycuron x Analytical standard Pirimicarb-desmethyl x Analytical standard Prothioconazole x Aviator and Propulse Pyraclostrobin x Viverda Tebuconazole x Folicur Tetramethrin x Analytical standard Heptachlor x Analytical standard

National Food Institute, Technical University of Denmark Spike procedure

National Food Institute, Technical University of Denmark National Food Institute, Technical University of Denmark Sample shipment

• Samples were distributed on Monday 7 and 8 March 2016 (17 February to non-EU and EFTA Countries)

• Most samples were delivered to EU laboratories within one day

National Food Institute, Technical University of Denmark Homogeniety test

2 2 Mean, mg/kg Ss c Ss < c Azoxys trobin 0.087 0.00000 0.0001 Pass Bixafen 0.073 0.00000 0.0001 Pass Boscalid 0.422 0.00030 0.0020 Pass Buprofezin 0.048 0.00000 0.0000 Pass Carbendazim 0.077 0.00000 0.0001 Pass Cypermethrin 0.140 0.00011 0.0004 Pass Epoxiconazole 0.173 0.00005 0.0004 Pass Fenpropidin 0.313 0.00007 0.0012 Pass Fluopyram 0.257 0.00006 0.0007 Pass Heptachlor 0.031 0.00000 0.0000 Pass Isocarbophos 0.048 0 0.0000 Pass Metribuzin 0.351 0.00057 0.0016 Pass Metrafenone 0.086 0.00001 0.0001 Pass Pencycuron 0.032 0.00000 0.0000 Pass Pirimicarb desmethyl 0.050 0 0.0000 Pass Prothioconazole desthio 0.112 0.00001 0.0002 Pass Pyraclostrobin 0.098 0.00002 0.0001 Pass Tebuconazole 0.099 0.00002 0.0001 Pass National Food Institute, Technical University of Denmark Stability test

Storage at -18 degrees

| x1 - yi | ≤ Mean, mg/kg | x1 - yi | 0.3×σ 0.3×σ Azoxys trobin 0.089 0.001 0.007 Pass Bixafen 0.077 0.002 0.006 Pass Boscalid 0.436 0.029 0.031 Pass Buprofezin 0.044 0.002 0.004 Pass Carbendazim 0.077 0.003 0.006 Pass Cypermethrin 0.110 0.000 0.010 Pass Epoxiconazole 0.190 0.009 0.013 Pass Fenpropidin 0.382 0.003 0.026 Pass Fluopyram 0.262 0.014 0.019 Pass Heptachlor 0.057 0.001 0.002 Pass Isocarbophos 0.046 0.003 0.004 Pass Metrafenone 0.092 0.003 0.007 Pass Pencycuron 0.022 0.001 0.002 Pass Pirimicarb desmethyl 0.049 0.001 0.004 Pass Prothioconazole desthio 0.113 0.004 0.011 Pass Pyraclostrobin 0.101 0.005 0.007 Pass Tebuconazole 0.093 0.001 0.007 Pass Tetramethrin 0.096 0.003 0.000 Pass

National Food Institute, Technical University of Denmark Stability test

Storage at -18 degrees Storage at room temperature

| x1 - yi | ≤ | x1 - yi | ≤ Mean, mg/kg | x1 - yi | 0.3×σ 0.3×σ | x1 - yi | 0.3×σ 0.3×σ Azoxys trobin 0.089 0.001 0.007 Pass 0.001 0.007 Pass Bixafen 0.077 0.002 0.006 Pass 0.001 0.006 Pass Boscalid 0.436 0.029 0.031 Pass 0.001 0.031 Pass Buprofezin 0.044 0.002 0.004 Pass 0.002 0.004 Pass Carbendazim 0.077 0.003 0.006 Pass 0.002 0.006 Pass Cypermethrin 0.110 0.000 0.010 Pass 0.006 0.010 Pass Epoxiconazole 0.190 0.009 0.013 Pass 0.005 0.013 Pass Fenpropidin 0.382 0.003 0.026 Pass 0.020 0.026 Pass Fluopyram 0.262 0.014 0.019 Pass 0.004 0.019 Pass Heptachlor 0.057 0.001 0.002 Pass 0.031 0.002 Fail Isocarbophos 0.046 0.003 0.004 Pass 0.004 0.004 Fail Metrafenone 0.092 0.003 0.007 Pass 0.002 0.007 Pass Pencycuron 0.022 0.001 0.002 Pass 0.017 0.002 Fail Pirimicarb desmethyl 0.049 0.001 0.004 Pass 0.010 0.004 Fail Prothioconazole desthio 0.113 0.004 0.011 Pass 0.003 0.011 Pass Pyraclostrobin 0.101 0.005 0.007 Pass 0.003 0.007 Pass Tebuconazole 0.093 0.001 0.007 Pass 0.006 0.007 Pass Tetramethrin 0.096 0.003 0.000 Pass 0.005 0.000 Pass

National Food Institute, Technical University of Denmark National Food Institute, Technical University of Denmark Calculation of assigned values and uncertainty of assigned values

• Algoritm A mean of the results from EU laboratories (and EFTA) – Only result from participant that • Reported to add water to the samples before extration or • used mixture of solvent and water or • used ASE • Outliers • Only obvious uncorrect results • Uncertainty • =1.25 *( ) • s* is robust∗ standard deviation (Alg A standard deviation) 𝑢𝑢 𝑠𝑠 /√𝑛𝑛 • n is the number of participants

National Food Institute, Technical University of Denmark Assigned values only Assigned values water addition, PESTICIDES mg/kg Azoxystrobin 0.088 Bixafen 0.074 Boscalid 0.414 Buprofezin 0.048 Carbendazim 0.086 Cypermethrin 0.134 Epoxiconazole 0.177 Fenpropidin 0.347 Fluopyram 0.250 Isocarbophos 0.048 Metrafenone 0.088 Pencycuron 0.033 Pirimicarb-desmethyl 0.048 Prothioconazole-desthio 0.149 Pyraclostrobin 0.098 Tebuconazole 0.091 Tetramethrin 0.096 Heptachlor 0.032

National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark Reported results and false negatives

No. of reported Pesticide results No. of NA False negatives % results Azoxystrobin 135 19 2 88 Bixafen 89 65 3 58 Boscalid 137 17 0 89 Buprofezin 138 16 2 90 Carbendazim 116 38 1 75 Cypermethrin 136 18 4 88 Epoxiconazole 132 22 2 86 Fenpropidin 105 49 0 68 Fluopyram 99 55 1 64 Isocarbophos 99 55 1 64 Metrafenone 97 57 0 63 Pencycuron 117 37 3 76 Pirimicarb-desmethyl 99 55 3 64 Prothioconazole-desthio 107 47 2 69 Pyraclostrobin 121 33 1 79 Tebuconazole 139 15 0 90 Tetramethrin 103 51 3 67 Heptachlor 131 23 7 85 National Food Institute, Technical University of Denmark False positive results

National Food Institute, Technical University of Denmark Deltamethrin and lambda-cyhalothrin

Deltamethrin Lambda-cyhalothrin Level mg/kg 0.011 0.011 Analysed 135 137 Detected 40 72

National Food Institute, Technical University of Denmark 29

Calculations of z-scores • For each laboratory/pesticide combination :

z = (x-X) / σ

– x is the result reported by the participant or the specific reporting limit of the lab for those labs not having detected the pesticide present in the test material – X is the assigned value, Alg A mean without outliers – σ is the target standard deviation obtained by multiplying the median by the FFP RSD of 25%

• |z| ≤ 2 Acceptable • 2 < |z| < 3 Questionable • |z| ≥ 3 Unacceptable

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Azoxystrobin Not specified LPE 5,0 Acceptable 130 (96%) Questionable 2 (1%) Assigned value: 0.088 mg/kg 4,0 Unacceptable 3 (2%) Alg A STD: 17% Number of labs 135 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 2 False Negatives 2 1 -5,0 9 7 6 8 5 3 68 54 35 87 34 74 71 95 17 21 27 58 36 23 84 77 75 91 15 38 98 82 65 10 11 25 53 46 22 28 18 40 69 13 14 66 43 62 24 47 20 67 39 94 83 42 56 86 60 63 73 45 49 50 80 96 64 59 33 16 37 76 85 57 78 70 26 79 93 124 155 159 145 170 105 149 143 167 120 110 107 116 156 176 125 123 136 157 154 163 108 171 133 141 148 140 137 111 151 172 142 128 138 106 130 117 174 177 161 165 102 114 158 103 134 115 139 152 150 101 166 135 109 146 153 168 173

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Azoxystrobin Not specified LPE 5,0 Acceptable 130 (96%) Questionable 2 (1%) Assigned value: 0.088 mg/kg 4,0 Unacceptable 3 (2%) Alg A STD: 17% Number of labs 135 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 2 False Negatives 2 1 -5,0 9 7 6 8 5 3 68 54 35 87 34 74 71 95 17 21 27 58 36 23 84 77 75 91 15 38 98 82 65 10 11 25 53 46 22 28 18 40 69 13 14 66 43 62 24 47 20 67 39 94 83 42 56 86 60 63 73 45 49 50 80 96 64 59 33 16 37 76 85 57 78 70 26 79 93 124 155 159 145 170 105 149 143 167 120 110 107 116 156 176 125 123 136 157 154 163 108 171 133 141 148 140 137 111 151 172 142 128 138 106 130 117 174 177 161 165 102 114 158 103 134 115 139 152 150 101 166 135 109 146 153 168 173

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Bixafen Not specified LPE 5,0 Acceptable 84 (94%) Questionable 2 (2%) Assigned value: 0.074 mg/kg 4,0 Unacceptable 3 (3%) Alg A STD: 15% Number of labs 89 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 3 False Negatives

-5,0 5 2 7 6 8 9 1 91 22 69 65 14 18 10 25 43 82 64 23 35 45 27 56 95 60 49 50 66 83 39 73 13 46 16 54 80 42 20 87 85 47 21 57 36 58 84 63 70 59 26 37 79 68 78 62 71 110 153 125 123 143 133 132 140 163 152 137 172 134 148 177 142 154 159 117 105 150 138 174 139 103 120 115 155 147 170 135 109 106

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Boscalid Not specified LPE 5,0 Acceptable 134 (98%) Questionable 2 (1%) Assigned value: 0.414 mg/kg 4,0 Unacceptable 1 (1%) Alg A STD: 14% Number of labs 137 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 0 False Negatives 5 4 1 3 2 7 -5,0 9 6 8 34 94 87 47 95 43 85 35 17 33 58 59 11 57 75 62 74 78 26 67 79 37 23 27 21 18 84 20 24 63 39 50 76 49 71 83 77 60 73 70 68 16 36 15 93 82 65 91 98 86 45 53 46 38 64 40 25 28 66 54 14 56 22 13 42 80 96 10 69 151 177 103 117 166 106 153 161 105 154 143 135 102 145 170 128 159 139 134 172 101 158 146 115 130 152 107 138 109 140 116 150 120 176 167 168 165 147 173 125 136 157 156 114 163 137 108 110 132 123 148 155 111 133 122 142 174 141 171

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Buprofezin Not specified LPE 5,0 Acceptable 133 (96%) Questionable 2 (1%) Assigned value: 0.048 mg/kg 4,0 Unacceptable 3 (2%) Alg A STD: 16% Number of labs 138 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 2 False Negatives 5 4 3 2 9 8 7 1 -5,0 6 18 23 65 82 95 42 28 13 62 94 39 50 11 96 66 14 56 69 73 79 16 63 21 70 71 37 74 75 49 84 33 77 46 86 36 24 67 80 87 98 83 20 17 43 58 78 57 25 35 64 85 22 26 68 76 34 60 59 93 15 10 38 40 45 54 47 53 91 27 130 139 133 163 102 117 168 134 105 111 115 153 159 109 132 146 174 108 138 106 141 145 147 128 142 137 120 124 158 177 135 103 155 166 101 107 151 140 170 113 150 157 114 122 165 129 143 125 176 136 156 123 172 167 173 148 116 152 154 171

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Carbendazim Not specified LPE 5,0 Acceptable 102 (88%) Questionable 6 (5%) Assigned value: 0.086 mg/kg 4,0 Unacceptable 8 (7%) Alg A STD: 23% Number of labs 116 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 1 False Negatives 2 7 8 9 6 1 3 -5,0 5 38 16 24 27 14 65 53 86 49 18 28 11 25 78 62 95 73 39 83 10 45 58 87 82 13 17 56 59 64 63 36 69 85 47 71 20 57 35 23 70 67 79 46 37 84 21 22 66 74 54 15 26 43 80 93 68 91 50 75 106 110 116 114 123 146 173 166 136 176 158 141 138 171 168 134 154 105 159 142 172 133 177 120 147 152 139 150 103 174 170 108 128 115 163 135 155 153 161 137 157 102 140 143 132 151 109 148 117

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Carbendazim Not specified ASE EUPT-CF9 5,0 Acceptable 98 (91%) Questionable 5 (5%) Assigned value:0.452 mg/kg 4,0 Unacceptable 5 (5%) Alg A STD: 28% Number of labs 108 3,0

2,0

1,0

0,0 scores z - -1,0

-2,0

-3,0

-4,0 0 False Negatives

-5,0 329 361 373 288 247 387 214 212 278 273 293 232 276 217 331 300 347 356 306 350 320 365 259 225 381 216 280 226 279 223 235 304 318 245 275 246 249 229 406 240 260 252 272 332 343 284 355 346 362 231 213 233 351 277 253 310 298 340 330 234 256 282 269 363 228 321 290 344 222 309 377 281 265 254 327 294 339 378 352 271 262 341 242 215 258 338 305 334 237 312 285 379 268 283 323 385 274 302 386 250 241 314 263 236 301 303 291 307

National Food Institute, Technical University of Denmark Water added Acceptable 81 (84%) No water added Carbendazim Questionable 5 (4%) Not specified Unacceptable 11 (12%) ASE EUPT-CF8 Number of labs 97 5,0

Assigned value: 0.073 mg/kg 4,0

3,0

2,0

1,0

0,0 scores z - -1,0

-2,0

-3,0

-4,0 * False negatives

-5,0 7 4 3 5 2 8 87 53 29 26 91 19 13 11 82 16 56 55 99 95 97 33 81 38 74 40 35 28 83 44 17 30 32 43 59 65 84 42 49 70 14 47 88 80 27 64 18 48 67 76 45 92 98 21 63 20 61 89 34 31 66 78 22 36 39 73 46 96 71 141 161 147 156 122 160 126 140 104 136 110 145 123 105 143 107 109 157 111 121 120 124 112 159 150 134 142 106

National Food Institute, Technical University of Denmark Water added Acceptable 59 No water added Carbendazim Questionable 4 Not specified Unacceptable 6 ASE EUPT-CF7 Number of labs 69 5,0

Assigned value: 0.252 mg/kg 4,0

3,0 Low ,

2,0 In ethyl acetate 0.135 mg/ml

1,0 check if standard is dissolved

0,0 scores z - -1,0

-2,0

-3,0

-4,0

-5,0 054 002 120 056 032 126 128 068 037 107 014 034 036 060 074 020 028 007 105 009 087 063 050 125 071 127 101 064 092 043 121 059 061 094 132 029 076 051 016 086 025 075 093 083 065 017 005 096 039 023 067 027 033 124 069 123 030 035 070 021 113 026 015 073 019 085 006 122 055

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Cypermethrin Not specified LPE 5,0 Acceptable 127 (93%) Questionable 1 (1%) Assigned value: 0.134 mg/kg 4,0 Unacceptable 8 (6%) Alg A STD: 23% Number of labs 136 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 4 False Negatives 7 8 5 1 -5,0 4 6 2 9 3 56 43 66 15 78 60 62 65 94 45 19 25 53 97 68 10 27 75 85 47 54 14 98 40 28 86 11 69 71 80 21 13 46 82 36 50 91 26 20 33 22 87 42 49 92 96 35 76 34 70 39 58 93 95 84 23 24 18 37 63 73 79 83 59 77 16 17 64 143 170 109 115 141 113 116 156 168 166 154 106 136 167 176 123 173 125 148 102 120 145 108 114 133 131 132 150 151 157 171 134 163 105 142 174 103 124 128 126 153 101 158 110 138 140 155 159 122 177 107 111 139 135 152 172 117 130 137

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Epoxiconazole Not specified LPE 5,0 Acceptable 128 (97%) Questionable 2 (2%) Assigned value: 0.177mg/kg 4,0 Unacceptable 2 (2%) Alg A STD: 16% Number of labs 132 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 2 False Negatives 9 6 5 2 8 7 1 -5,0 3 20 71 83 85 95 96 13 47 58 21 27 42 78 23 36 16 24 66 74 35 87 33 57 26 70 15 67 93 37 62 75 18 80 39 76 77 28 34 84 43 60 45 50 59 73 49 91 38 69 82 11 65 86 54 98 10 46 25 64 14 22 56 17 79 63 68 94 177 103 161 106 115 134 124 174 153 145 139 105 120 170 146 135 114 137 128 168 111 117 102 130 166 107 150 152 140 101 142 172 141 109 173 157 123 125 136 156 176 133 163 116 154 151 138 132 158 148 155 159 171 143 110 147 167

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Fenpropidin Not specified LPE 5,0 Acceptable 98 (93%) Questionable 5 (5%) Assigned value: 0.347 mg/kg 4,0 Unacceptable 2 (2%) Alg A STD: 21% Number of labs 105 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 0 False Negatives 2 3 -5,0 6 8 9 1 7 5 91 11 65 22 15 46 60 98 16 82 67 28 14 17 78 54 79 80 20 84 56 50 64 94 74 35 58 70 75 37 68 71 63 23 66 39 87 69 21 43 36 10 13 18 26 83 25 59 73 95 57 45 62 42 85 27 47 49 132 106 156 176 154 133 163 159 138 174 120 105 115 109 139 114 170 177 143 147 135 145 103 172 102 134 140 137 151 123 141 152 150 142 155 166 117 148 158

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Fluopyram Not specified LPE 5,0 Acceptable 96 (97%) Questionable 2 (2%) Assigned value: 0.250 mg/kg 4,0 Unacceptable 1 (1%) Alg A STD: 17% Number of labs 99 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 1 False Negatives 2 1 7 6 9 5 -5,0 8 49 69 91 18 65 10 28 84 14 25 73 24 45 13 83 50 78 85 95 67 94 47 42 82 66 56 57 58 87 20 21 79 26 59 62 36 75 68 23 70 22 37 71 43 46 80 64 39 54 11 35 27 15 168 125 156 123 172 114 163 159 141 133 108 174 138 105 139 140 150 120 143 106 177 103 170 147 109 151 135 176 137 152 148 154 110 134 142 115 117 155 102

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Heptachlor Not specified LPE 5,0 Acceptable 121 (92%) Questionable 10 (8%) Assigned value: 0.032 mg/kg 4,0 Unacceptable 0 (0%) Alg A STD: 21% Number of labs 131 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 7 False Negatives 4 7 9 2 1 3 6 8 -5,0 5 35 56 80 33 70 83 58 91 93 73 39 34 10 40 54 55 22 28 27 82 14 49 75 96 60 11 63 98 67 23 37 36 94 71 79 20 50 15 17 47 19 64 26 46 65 74 87 18 12 76 77 59 78 99 21 62 69 84 16 25 68 38 45 85 92 43 97 95 145 137 138 129 176 141 157 131 132 162 128 120 117 143 142 169 105 133 174 163 146 103 122 124 152 102 106 153 101 107 139 177 150 155 151 164 170 111 130 126 159 158 115 140 173 119 113 114 156 168 167 127 135 149

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Isocarbophos Not specified LPE 5,0 Acceptable 95 (96%) Questionable 1 (1%) Assigned value: 0.048 mg/kg 4,0 Unacceptable 3 (3%) Alg A STD: 16% Number of labs 99 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 1 False Negatives 7 5 -5,0 2 8 9 1 6 79 42 21 64 84 63 60 15 36 16 23 59 35 78 70 18 47 45 49 10 11 27 13 65 82 56 43 71 69 85 22 26 37 39 66 73 28 80 67 83 14 54 17 62 91 98 68 20 58 87 25 46 109 153 117 135 159 174 140 155 170 158 143 114 168 133 163 148 156 147 177 102 110 154 106 115 137 142 150 120 152 151 138 172 134 105 103 125 176 136 139 123

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Metrafenone Not specified LPE 5,0 Acceptable 97 (100%) Questionable 0 (0%) Assigned value: 0.088mg/kg 4,0 Unacceptable 0 (0%) Alg A STD: 14% Number of labs 97 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 0 False Negatives 5 -5,0 2 6 8 9 7 1 85 79 25 68 70 26 27 23 94 59 10 65 64 43 22 73 39 62 83 71 13 17 87 42 54 78 95 21 36 50 20 35 37 58 75 63 66 57 84 91 98 46 82 14 56 69 60 45 47 67 80 18 150 139 159 120 140 115 135 106 176 136 141 138 103 170 161 114 177 153 174 134 143 158 123 154 102 172 148 163 117 152 155 133 137 151 171 142 105 109

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Pencycuron Not specified LPE 5,0 Acceptable 108 (92%) Questionable 8 (7%) Assigned value: 0.033 mg/kg 4,0 Unacceptable 1 (1%) Alg A STD: 16% Number of labs 117 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 3 False Negatives 7 3 2 5 8 1 9 -5,0 6 91 93 23 26 38 86 60 15 58 75 87 18 37 59 79 42 36 70 68 13 50 27 74 20 63 54 24 21 25 49 10 11 69 65 14 85 28 22 47 56 64 66 80 82 17 45 62 84 98 71 67 39 57 83 73 94 35 46 78 95 43 148 147 145 168 173 153 140 135 103 155 150 152 136 110 151 109 128 158 146 156 159 176 125 123 143 114 172 108 117 139 154 106 102 161 163 134 177 120 141 142 115 133 166 170 171 174 137 138

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Pirimicarb-desmethyl Not specified LPE 5,0 Acceptable 93 (94%) Questionable 2 (2%) Assigned value: 0.048 mg/kg 4,0 Unacceptable 4 (4%) Alg A STD: 15% Number of labs 99 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 3 False Negatives 3 7 6 8 5 -5,0 2 1 9 35 59 83 36 75 57 86 37 13 27 49 23 66 46 62 65 11 10 22 42 50 64 69 63 82 39 45 24 15 26 14 25 80 73 43 95 47 68 67 17 56 85 70 54 79 20 58 87 18 71 78 84 21 133 170 140 103 143 145 116 123 176 139 132 135 172 115 153 138 154 106 117 147 148 158 152 142 105 174 177 108 109 163 159 102 155 137 150 114 120 134

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Prothioconazole-desthio Not specified LPE 5,0 Acceptable 101 (94%) Questionable 1 (1%) Assigned value: 0.149 mg/kg 4,0 Unacceptable 5 (5%) Alg A STD: 16% Number of labs 107 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 2 False Negatives 2 8 5 1 7 -5,0 6 9 3 98 22 45 85 42 64 63 95 54 86 73 87 60 13 36 83 50 47 91 65 69 28 80 34 77 76 25 46 10 33 14 39 67 18 84 43 58 82 37 26 59 21 71 56 79 35 20 57 17 75 23 66 78 27 62 70 68 15 147 142 102 140 177 109 141 173 132 125 123 138 163 134 168 158 148 133 152 130 107 111 106 115 117 170 154 139 150 155 172 137 174 120 103 135 143 145 153 114 151

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Pyraclostrobin Not specified LPE 5,0 Acceptable 116 (96%) Questionable 3 (2%) Assigned value: 0.098 mg/kg 4,0 Unacceptable 2 (2%) Alg A STD: 22% Number of labs 121 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 1 False Negatives 4 7 3 1 6 5 -5,0 2 9 8 93 37 36 40 79 62 86 98 27 59 75 23 26 56 35 70 66 65 82 18 11 53 80 71 46 64 22 43 14 28 73 54 50 24 13 45 39 63 25 94 96 67 85 47 21 95 74 57 68 15 20 83 84 10 17 58 78 87 49 38 91 69 109 132 143 174 158 145 110 173 133 108 137 140 154 141 146 102 117 148 142 134 172 115 111 155 106 159 166 135 153 152 170 161 103 139 150 120 167 177 156 125 123 136 171 114 138 163 128 176 151 168

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Tebuconazole Not specified LPE 5,0 Acceptable 137 (99%) Questionable 1 (1%) Assigned value: 0.091 mg/kg 4,0 Unacceptable 1 (1%) Alg A STD: 15% Number of labs 139 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 0 False Negatives 4 3 -5,0 2 6 7 8 9 1 5 82 25 53 62 98 96 75 76 46 24 87 50 95 14 49 23 54 13 18 27 86 60 73 83 43 33 80 67 59 45 74 93 85 77 47 63 34 58 20 35 84 36 57 78 37 66 21 71 70 79 26 40 68 15 94 65 69 10 11 38 19 28 56 39 91 42 17 64 22 174 142 107 117 116 124 101 130 120 115 103 177 149 105 170 111 139 161 172 159 150 151 109 153 147 145 141 166 146 168 110 135 143 167 173 136 125 176 122 133 108 156 157 163 165 148 106 138 102 123 128 158 114 140 171 137 132 154 155 152 134

National Food Institute, Technical University of Denmark Water added EU and EFTA Laboratories No water added Tetramethrin Not specified LPE 5,0 Acceptable 99 (96%) Questionable 0 (0%) Assigned value: 0.096 mg/kg 4,0 Unacceptable 4 (4%) Alg A STD: 18% Number of labs 103 3,0

2,0

1,0

0,0 scores - z -1,0

-2,0

-3,0

-4,0 3 False Negatives 6 8 3 9 2 7 5 -5,0 1 56 60 27 54 69 26 73 95 25 23 75 97 78 16 85 53 14 71 46 65 82 10 98 84 19 28 62 67 59 64 22 20 47 68 17 83 39 45 66 36 49 24 96 57 35 21 43 50 79 87 18 70 80 37 154 109 155 124 138 170 166 134 159 168 125 176 156 163 171 106 152 139 149 114 142 103 143 150 148 120 131 141 158 151 102 115 133 135 174 172 153 177 137 140 117

National Food Institute, Technical University of Denmark Alg. A RSD

National Food Institute, Technical University of Denmark Acceptable, questionable and

135 89 137 138 116 136 132 105 99 99 97 117 99 107 121 139 103 131 100unacceptable results

90

80

70

60

50

40

30

20

10

0 Bixafen Boscalid Fluopyram Buprofezin Heptachlor Pencycuron Fenpropidin Metrafenone Carbendazim Azoxystrobin Tetramethrin Cypermethrin Isocarbophos Tebuconazole Epoxiconazole Pyraclostrobin Pirimicarb-desmethyl Prothioconazole-desthio National Food Institute, Technical University of Denmark Catagory A laboratories and combined z-scores • To be classified as Category A laboratory the labs had to report at least 90% of the pesticide present in the test material (≥15 pesticide residues), analyse for at least 90% of the pesticides on the Pesticide Target List and report no false positive.

• Evaluation of the overall performance, the Average of the Squared z-Score (AZn 2) are calculated: 2 ∑ Zi AZ 2 = i=1 n

• z ≤ 2 Good • 2 < z < 3 Satisfactory • z > 3 Unsatisfactory National Food Institute, Technical University of Denmark 5,0

OFL Catagory A: 75 labs (47%) NRL Good: 95% 4,0 Satisfactory: 3 % Unsatisfactory: 3%

3,0

2,0

1,0

0,0 NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL NRL National Food Institute, Technical University of Denmark EUPT-CF11

EUPT Tentative date Matrix Green beans FV-19 February 2016 or lemons

SRM-12 March 2016 To be decided

AO-12 April 2016 Eggs

CF-11 May 2016 Oat flour

National Food Institute, Technical University of Denmark Thank you very much

National Food Institute, Technical University of Denmark