eupt-cf8 incurred and spiked pesticides in wheat · eupt-cf8 incurred and spiked pesticides in...

EUPT-CF8 Incurred and spiked pesticides in wheat

Mette Erecius Poulsen, Gitte Andersen and Susan Strange Herrmann Copenhagen, 18 December 2014

National Food Institute, Technical University of Denmark

PTs on cereals/feed – overview

2007 2008 2009 2010 2011 2012 2013 2014EUPT-C1 /SRM2

EUPT-C2 EUPT-C3 /SRM4

EUPT-C4 EUPT-C5 /SRM6

EUPT-C6 EUPT-CF7 EUPT-CF8

Test material Wheat flourWheat flour Oat flour Rye flour Rice flour Barley Feed Wheat flour

no. of participants 64 74 111 118 155 (133) 149 (127) 120 (106) 160 (141)

No. of target pesticides 37 55 60 72 104 107 116 111MRM no. of incurred pesticides 3 9 14 13 10 8 19 14

no. of spiked pesticides 4 4 3 7 10 4 5SRM no. of incurred pesticides 2 2 2 2

no. of spiked pesticides 1 2 1 7

Total no. of pesticides in test item 10 15 18 19 24 18 23 19


Organising team at EURL

•Mette Erecius Poulsen, Senior Chemist •Anne Kruse Lykkeberg, Senior Chemist •Gitte Andersen, Chemist •Merete B. Ludwigsen, Chemical Technician •Inge Schröder, Chemical Technician •Lisbet Pilhkjær, Chemical Technician •Jens-Ole Frimann, System Developer

3


Scientific Group

Advisory Group

Amadeo R. Fernández-Alba

André de Kok

Antonio Valverde

Darinka Štajnbaher

Magnus Jezussek

Michelangelo Anastassiades

Miguel Gamón

Ralf Lippold

Dr. Sonja Masselter

Stewart Reynolds

Tuija Pihlström

Quality Group

Antonio Valverde

Stewart Reynolds


Participation Country # labs Country # labs Country # labsArgentina 3 Germany 23 Poland 15Austria 2 Greece 3 Portugal 2Belgium 3 Hungary 4 Republic of Belarus 1Brasil 5 Iceland 1 Romania 8Bulgaria 3 India 2 Serbia 2Burkina Faso 1 Indonesia 1 Singapore 1Croatia 5 Ireland 1 Slovakia 2Cyprus 2 Italy 20 Slovenia 3Czech Republic 3 Kenya 2 Spain 18Denmark 1 Lithuania 1 Sweden 2Egypt 1 Luxembourg 1 Tanzania 1Estonia 1 Netherlands 6 Thailand 1Finland 1 New Zealand 1 United Kingdom 3France 6 Norway 1 Total 163


Target Pesticide List • 111 pesticides • 4 new

– Bixafen – Flonicamid – Fluxapyroxad – Metrafenone

• 9 deleted – Aldrin – Chlordane, cis- – Chlordane, oxy – Chlordane, trans- – Dieldrin – Endrin – Heptachlor – Heptachlorepoxid-cis – Heptachlorepoxid-trans


• Grown in Denmark in 2013

• Field treated by Aarhus University, Research Department

Flakkebjerg

Wheat


Incurred and spiked pesticides Pesticide

Application on cereals in the field Spike in laboratory

Azoxystrobin xBixafen xBoscalid xCarbendazim xChlorothalonil x xCypermethrin x xDeltamethrin-cis x xEndosulfan-sulfate xEpoxiconazole xFlonicamid xFluxapyroxad xLindane xLinuron xMetconazole xMetrafenone x xProthioconazole xPyraclostrobin xSpiroxamine x xTrifluralin x


Spike procedure


Spike procedure

13


Homogenisation


Milling and futher homogenisation


• Samples were distributed on Monday 19 May 2014 (13 May to Third

Countries

• Most samples were delivered to EU laboratories on 20 or 21 May 2014

Sample shipment


Homogeniety test

Mean, mg/kg Ss2 c Ss

2 < c Azoxystrobin 0.211 0.00000 0.0033 PassBixafen 0.082 0.00005 0.0001 PassBoscalid 0.324 0 0.0063 PassCarbendazim 0.055 0.00001 0.0001 PassChlorthalonil 0.029 0.00001 0.0001 PassCypermethrin 0.891 0 0.0482 PassDeltamethrin 0.053 0 0.0002 PassEndosulfan-sulfate 0.057 0 0.0002 PassEpoxiconazole 0.122 0 0.0008 PassFlonicamid 0.102 0 0.0003 PassFluxapyroxade 0.179 0.00017 0.0004 PassLindane 0.035 0 0.0000 PassLinuron 0.069 0.00002 0.0003 PassMetconazole 0.110 0.00014 0.0001 PassMetrafenone 0.381 0 0.0081 PassProthioconazole desthio 0.179 0.00040 0.0004 PassPyraclostrobin 0.070 0.00004 0.0001 PassSpiroxamin 0.064 0.00006 0.0001 PassTrifluralin 0.058 0 0.0001 Pass


Stability test

Mean, mg/kgFreezer| x1 - yi | 0.3×σ

| x1 - yi | ≤ 0.3×σ

Azoxystrobin 0.243 0.017 0.017 PassBixafen 0.071 0.001 0.006 PassBoscalid 0.305 0.015 0.025 PassCarbendazim 0.058 0.000 0.000 PassChlorothalonil 0.027 0.003 0.003 PassCypermethrin 0.908 0.053 0.057 PassDeltamethrin 0.042 0.003 0.003 PassEndosulfan-sulfate 0.034 0.000 0.003 PassEpoxiconazole 0.118 0.005 0.009 PassFlonicamid 0.088 0.004 0.008 PassFluxapyroxade 0.150 0.012 0.012 PassLindane 0.038 0.003 0.003 PassLinuron 0.065 0.004 0.006 PassMetconazole 0.098 0.005 0.008 PassMetrafenone 0.362 0.015 0.028 PassProthioconazole-desthio 0.159 0.005 0.015 PassPyraclostrobin 0.061 0.004 0.006 PassSpiroxamin 0.057 0.003 0.005 PassTrifluralin 0.034 0.002 0.003 Pass


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 • 𝑢=1.25 *(𝑠∗ /√𝑛) • s* is robust standard deviation (Alg A standard deviation) • N is the number of participants


Assigned values

PESTICIDES

Assigned values only water addition,

mg/kgAzoxystrobin 0.228Bixafen 0.079Boscalid 0.328Carbendazim 0.073Chlorothalonil 0.042Cypermethrin 0.766Deltamethrin-cis 0.040Endosulfan-sulfate 0.040Epoxiconazole 0.117Flonicamid 0.104Fluxapyroxad 0.165Lindane 0.038Linuron 0.074Metconazole 0.101Metrafenone 0.376Prothioconazole-desthio 0.201Pyraclostrobin 0.074Spiroxamine 0.060Trifluralin 0.040

0.00

0.10

0.20

0.30

0.40

0.50

0.60

0.70

0.80

0.90

Lin

dan

eEn

do

sulf

an-s

ulf

ate

Del

tam

eth

rin

-cis

Trif

lura

lin

Ch

loro

thal

onil

Sp

irox

amin

eC

arb

end

azim

Pyr

aclo

stro

bin

Lin

uro

nB

ixaf

enM

etco

naz

ole

Flo

nic

amid

Epox

icon

azol

eFl

uxa

pyr

oxad

Pro

thio

con

azol

e-…

Azo

xyst

rob

inB

osca

lid

Met

rafe

non

eC

yper

met

hri

n

mg/kg

Assigned values


Reported results and false negatives Pesticide

No. of reported

results No. of NAFalse

negatives % resultsAzoxystrobin 116 19 2 85Bixafen 67 68 0 49Boscalid 117 18 1 86Carbendazim 97 38 1 71Chlorothalonil 90 45 22 66Cypermethrin 125 10 1 92Deltamethrin-cis 123 12 10 90Endosulfan-sulfate 126 9 7 93Epoxiconazole 110 25 1 81Flonicamid 79 56 0 58Fluxapyroxad 60 75 3 44Lindane 126 10 5 93Linuron 95 40 2 70Metconazole 87 48 2 64Metrafenone 83 52 1 61Prothioconazole-desthio 86 49 3 63Pyraclostrobin 97 38 2 71Spiroxamine 97 38 4 71Trifluralin 106 29 2 78


False positive results

Lab code Pesticide Concentration

mg/kg Determination

technique RL,

mg/kg 104 Captan 0.209 LC-MS/MS QQQ 0.06

1 Fenvalerate and Esfenvalerate 0.01 GC-Ion Trap 0.01 147 HCH-beta 0.0294 GC-MS/MS (QQQ) 0.01 111 Quinoxyfen 0.01 75 * Permethrin 0.0946 GC- (µ) ECD 0.005 69 * Tebuconazole 0.057 LC-MS/MS QQQ 0.01


28

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


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

13 28 35 41 42 45 46 53 56 71 78 86 89 91 97 99 106

111

118

140

150

156

119

143 96 108 55 19 147 36 159 47 161 4

107 50 64 110

134 59 124 18 114 73 126

121

109

163 21 38 72 76 74 16 120 40 17 70 82 20 5 14 84 34 29 26 3 33 67 141 66 87 31 95 112 58 61 2 49 30 48 65 43 63 122 11 83 104 15 92

z-sc

ores

Chlorothalonil Acceptable Questionable Unacceptable Number of labs

Water added No water added Not specified ASE

0.042 Assigned value: mg/kg

51 (56%)

* * * * * * * * * * * * * * * * * * * * * * * False negatives

30 (34%) 9 (10%)

90

Alg. A RSD = 49%


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 86 127

147 85 99 50 46 18 41 163 39 22 36 55 92 122

107 64 35 160

140 8

106 74 59 84 44 72 32 57 108

136

134 89 126 82 135 21 83 132

161 80 138 7 76 10 40 96 23 114 70 34 24 111 4 66 63 20 43 51 65 17 31 68 15 104 1

141 5 25 77 128

112

148

117 11 52 58 120

123

159 37 13 38 71 73 142 2 88 14 30 45 47 87 48 124 19 9 98 109

150 61 49 53 78 119

144 16 67 79 97 121 3 6 91 33 95 110 26 118

145

133

146 27

z-sc

ores

Lindane Acceptable Questionable Unacceptable Number of labs



112 (90%)

****** False negatives

9 (7%) 4 (3%)

125

Alg. A RSD = 16%


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 55 140 99 95 97 33 81 104

136 38 74 40 35 110

145

123 28 83 7 44 17 105

143

107 30 32 4

141 87 161 53 29 147 26 156 91 122 19 160 13 11 82 16 126 3 43 109

157 59 65 84 5 42 49 111 70 14 47 88 121 80 27 64 120

124 18 48 2 67 76 45 92 98 21 63 20 61 112 89 159 34 31 66 150

134

142 8 78 22 106 36 39 73 46 96 71

z-sc

ores

Carbendazim Acceptable Questionable Unacceptable Number of labs



81 (84%)

* False negatives

5 (4%) 11 (12%)

97


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

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

z-sc

ores




59 4 6

69 EUPT-CF7


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 55 140 99 95 97 33 81 104

136 38 74 40 35 110

145

123 28 83 7 44 17 105

143

107 30 32 4

141 87 161 53 29 147 26 156 91 122 19 160 13 11 82 16 126 3 43 109

157 59 65 84 5 42 49 111 70 14 47 88 121 80 27 64 120

124 18 48 2 67 76 45 92 98 21 63 20 61 112 89 159 34 31 66 150

134

142 8 78 22 106 36 39 73 46 96 71

z-sc

ores




81 (84%)

* False negatives

5 (4%) 11 (12%)

97

Low solubility,

In ethyl acetate 0.135 mg/ml

check if standard is dissolved


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

38 140 74 107 73 63 17 111 80 150 99 27 84 11 58 76 4 30 10 44 89 87 142

126 20 59 71 64 65 57 32 53 109 14 2 51 106 48 49 77 39 66 34

z-sc

ores

Prothioconazole-desthio Acceptable Questionable Unacceptable Number of labs



78 (91%)

* * * False negatives

4 (5%) 4 (5%)

86


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 95 97 55 35 23 74 147

111 24 17 51 92 25 4 52 134

163

136

143 76 140 8

120

142

122 54 77 64 107 27 36 37 3 47 21 91 80 141

132 31 44 63 159 84 13 40 5

104 58 71 99 157 34 67 145 89 100

112

124

110

123 70 126 29 38 43 121 72 150 1 20 98 26 50 109 45 160 30 73 49 53 61 83 57 105

161 78 82 87 19 96 16 14 11 2 66 10 65 59 46 88 106 79 133 7 15 81 33 32 18 42 39 48 156

127

z-sc

ores

Azoxystrobin Acceptable Questionable Unacceptable Number of labs



113 (97%)

* * False negatives

1 (1%) 2 (2%)

116


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 55 97 35 95 58 10 74 108 21 80 136 17 92 76 3

119 54 27 51 36 122

132 25 37 73 84 24 141

111 34 134 47 77 159 64 66 23 104 52 143

145

107 13 89 91 1 63 140 19 96 5

109

126 29 71 161 43 163 59 4 30 40 105 31 99 147 20 123

150 38 120 61 72 78 82 133 70 98 121 16 87 156 7 46 53 44 142 49 26 57 67 124 2 65 88 160 14 157

100 11 83 106 18 110 32 81 39 45 33 8 42 48 15 50 112

127

z-sc

ores

Boscalid Acceptable Questionable Unacceptable Number of labs



112 (97%)

* False negatives

3 (1%) 2 (2%)

117


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 55 95 35 36 46 97 73 58 84 29 134

107

111 23 92 147 21 27 140 80 63 156 1 17 91 124

112 11 13 38 40 47 96 141 3 70 76 25 126

132

159 4 43 72 89 161 51 34 150 61 77 120

133

142 32 59 66 31 67 74 123 15 24 44 121

145 14 37 78 7 30 98 82 64 5 52 19 109

110 26 2 16 143 10 20 57 79 157

160 49 83 71 53 99 105

122

106 88 48 65 87 33 81 18 39 45 8 42 22

z-sc

ores

Epoxiconazole Acceptable Questionable Unacceptable Number of labs



104 (95%)

* False negatives

3 (3%) 3 (2%)

110


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

120 95 99 18 74 35 122

145 91 160

126 40 3 83 161

159

107 58 92 5 44 38 141 30 121

110 70 53 71 13 43 96 143 14 134 63 67 119 17 32 57 76 147 66 109 19 88 1 65 87 89 112

124 4 34 21 80 82 106

111 49 2 59 150 11 20 16 26 33 42 61 98 48 73 64 45 84 97 47

z-sc

ores

Flonicamid Acceptable Questionable Unacceptable Number of labs



75 (96%)

1 (0%) 3 (4%)

79


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

23 56 55 97 95 73 119 35 120

140

111 80 107 29 76 27 67 105

134

141 13 92 31 72 147 91 7

145 8

124

104 44 3 84 99 121 46 63 47 64 150

161

112 70 58 71 98 143 11 5

142 10 21 2 96 14 53 88 59 4

126 49 30 106 19 40 81 100 48 136 38 26 82 109 43 89 45 65 17 20 16 83 160 32 159

110

157 61 87 39 34 18 74 33 66 42 122

127

z-sc

ores

Pyraclostrobin Acceptable Questionable Unacceptable Number of labs



89 (92%)

* * False negatives

4 (4%) 4 (4%)

97


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

55 97 35 96 74 34 111

120

107 73 76 1 67 124 13 134 87 99 161 91 84 43 47 70 38 44 63 150 11 4 17 20 53 160 3 5 71 66 14 30 110

145 21 98 106 82 83 2

126 59 49 121 46 89 112

159 61 78 19 64 48 65 122 18 80 109 16

z-sc

ores

Bixafen Acceptable Questionable Unacceptable Number of labs



65 (97%)

2 (3%) 0 (0%)

67


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

33 111 96 35 97 17 34 64 120

134

124 63 67 107 84 13 112 87 30 66 150 1 5 44 141 43 126 91 70 89 121 11 21 71 16 76 4 80 19 73 122

145 61 47 159 49 106 98 2 38 160 83 53 109 65 14 59 110 18 48

z-sc

ores

Fluxapyroxad Acceptable Questionable Unacceptable Number of labs



57 (95%)

* * * False negatives

0 (0%) 3 (5%)

60


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

85 163

142

147 97 89 119 46 134

135 55 99 18 59 33 41 108 76 7

146 1 65 64 29 19 136 91 112

143 35 107 74 10 156 16 83 63 160 44 122 66 92 32 54 5 4 24 72 161

123 34 57 51 56 84 109

110 14 100 43 47 53 11 37 13 77 21 138 48 105 25 73 17 49 106

132

104 58 157 52 114 38 23 26 87 121 40 159 96 70 45 82 150

133 20 126

141

111 2

145 88 42 80 61 71 3 98 118 67 95 36 140

124 30 79 39 78 120 50 144 22 127 8 27 15

z-sc

ores

Cypermethrin Acceptable Questionable Unacceptable Number of labs



106 (84%)

* False negatives

11 (10%) 8 (6%)

125


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

85 56 79 99 104

122

133

150

156

163

147

118 29 97 50 46 72 43 119

161 40 15 112 38 92 8 91 36 11 143 96 21 53 23 74 111

142 1 70 18 141 89 59 134 35 84 157 76 34 3 24 63 160 51 108

123

136

146 13 159 41 82 66 138 37 19 25 107 54 32 45 71 77 140 4 64 65 73 121

114 52 132 61 88 98 144 55 10 16 67 80 14 87 110 30 135 2

106 5 47 49 48 58 126 20 83 109 57 26 120 17 7 33 124 44 100

145 39 95 22 42 78 27

z-sc

ores

Deltamethrin-cis Acceptable Questionable Unacceptable Number of labs



102 (83%)

*********** False negatives

14 (11%) 7 (6%)

123


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 71 78 86 127

133 85 54 111

146 33 30 96 50 41 156

142

147 92 119

140 74 11 99 7 89 55 35 135 18 64 17 8 21 29 159

160 32 47 76 84 136

150

161 34 63 80 4

109

106 13 16 77 108 91 107 72 3 5 65 82 126 14 20 24 38 45 52 141 22 1 10 25 70 134 26 36 43 51 66 97 98 123 19 61 53 57 144 67 112 2 9

122

118

163 37 49 44 6

138 87 59 58 83 132 40 68 117 39 42 120

110

128

114

145

124 48 46 79 148

121 95 73 157

105 27

z-sc

ores

Endosulfan-sulfate Acceptable Questionable Unacceptable Number of labs



110 (87%)

******** False negatives

15 (13%) 1 (1%)

126


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

30 56 46 59 84 18 160 10 11 147 64 92 140 8 35 99 40 74 21 143 82 70 20 111 96 32 110 13 55 91 122 76 112 72 161 66 36 80 19 63 106 5 29 38 65 78 1

134 4

109

107 2 48 61 57 58 87 157

141 89 45 83 150

159 47 79 121

123 95 49 14 105 16 44 71 98 142

145

144 34 67 24 26 42 43 53 3

120 17 7 73 124

126

132

156 77 86 39 51 23 104 33 133 52 97 27 136

z-sc

ores

Trifluralin Acceptable Questionable Unacceptable Number of labs



102 (96%)

* * False negatives

1 (1%) 3 (3%)

106


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

56 120

104 92 97 55 95 35 82 15 27 107 7 19 74 159 4

143 8 64 141 99 91 134

122 38 80 17 147 42 40 145 13 83 84 88 111

142 76 44 73 140

157 30 70 26 32 53 109

161 96 63 5 71 87 59 61 3

160 21 43 49 98 29 124 14 47 65 81 89 106 58 136 46 67 11 110 2 57 10 150

121 66 16 123 20 78 34 18 39 126 33 48 112 45

z-sc

ores

Linuron Acceptable Questionable Unacceptable Number of labs



91 (97%)

* * False negatives

2 (1%) 2 (2%)

95


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

21 56 157 35 97 92 107

126 4 74 19 17 156 84 121

111 96 13 159 27 134 73 38 64 47 88 63 3 67 161 76 30 34 40 141 99 80 124 87 26 89 91 5 43 58 110

120 14 32 70 98 123

133

143 7 44 150 46 71 11 65 78 142 42 106

145 59 2 10 49 66 160 16 109 20 57 83 82 18 112 39 33 53 61 122 48 31

z-sc

ores

Metconazole Acceptable Questionable Unacceptable Number of labs



82 (94%)

* * False negatives

2 (1%) 3 (2%)

87


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

142 42 97 99 80 96 92 76 35 107

143

104

111

147

145 19 161 10 91 58 21 134 84 141 55 159 73 122 32 38 13 43 17 5 14 1 57 109 87 26 70 63 150 95 110

123 47 49 106

124 67 82 4 11 53 71 74 16 20 30 112 66 65 98 160 3

121 83 34 61 64 89 44 88 2 45 18 59 126

120 48 33 31

z-sc

ores

Metrafenone Acceptable Questionable Unacceptable Number of labs



79 (95%)

* False negatives

1 (1%) 3 (4%)

83


-5.0

-4.0

-3.0

-2.0

-1.0

0.0

1.0

2.0

3.0

4.0

5.0

23 56 95 119 97 92 15 147

156

121 27 99 40 134 38 21 81 120

141 20 53 8 73 91 72 111

140

161

106 43 17 124

107 47 80 89 71 143 44 19 11 35 126 5 32 49 70 42 87 88 13 3

142 59 160 76 10 145 61 2 14 4 16 39 83 109 7 26 84 98 150 64 45 122 65 46 30 67 82 74 96 36 57 18 78 31 157 48 110 66 34 63 123

159

112 33 133

z-sc

ores

Spiroxamine Acceptable Questionable Unacceptable Number of labs



89 (92%)

* * * * False negatives

2 (2%) 6 (6%)

97


Alg. A RSD

0

0.25

Azo

xyst

robi

n

Bix

afen

Bos

calid

Car

bend

azim

Chl

orot

halo

nil

Cyp

erm

ethr

in

Del

tam

ethr

in-c

is

Endo

sulfa

n-su

lfate

Epox

icon

azol

e

Flon

icam

id

Flux

apyr

oxad

Lind

ane

Linu

ron

Met

cona

zole

Met

rafe

none

Prot

hioc

onaz

ole-

dest

hio

Pyra

clos

trob

in

Spi

roxa

min

e

Trifl

ural

in


No. of reported results Assigned values Acceptable Questionable Unacceptable False negatives

Azoxystrobin 117 0.228 114 1 2 2Bixafen 67 0.079 65 2 0 0Bosca l id 117 0.328 112 3 2 1Carbendazim 98 0.073 81 5 12 1Chlorothalonil 91 0.042 51 31 9 23Cypermethrin 126 0.766 106 12 8 1Deltamethrin-cis 124 0.040 102 14 8 11Endosul fan-sul fate 127 0.040 110 16 1 8Epoxiconazole 110 0.117 104 3 3 1Flonicamid 79 0.104 75 1 3 0Fluxapyroxad 60 0.165 57 0 3 3Lindane 126 0.038 112 10 4 6Linuron 95 0.074 91 2 2 2Metconazole 87 0.101 82 2 3 2Metrafenone 83 0.376 79 1 3 1Prothioconazole-desthio 86 0.201 78 4 4 3Pyraclostrobin 97 0.074 89 4 4 2Spiroxamine 97 0.060 89 2 6 4Tri flura l in 106 0.040 102 1 3 2

Acceptable, questionable and unacceptable results


• To be classified as Category A laboratory the labs had to report at least 90% of the pesticide present in the test material (≥17 pesticide residues) and report no false positive.

• Evaluation of the overall performance, the Average of the Squared z-Score (AZ2) are calculated:

• z ≤ 2 Good • 2 < z < 3 Satisfactory • z > 3 Unsatisfactory

Catagory A laboratories and combined z-scores

n

ZAZ

n

ii∑

== 1

2

2


0.0

1.0

2.0

3.0

4.0

5.05 70 14 98 13 4 3 19 2 49 32 26 43 67 141 82 65 160 87 11 109 76 91 161 89 63 64 20 121 53 80 59 126 44 83 84 159 61 16 110 17 107

124

134

150 34 145 66 21 30 74 18 38 106 35 112 47 99 71 122 92 73 48 120 96 42 33 97

OFL

NRL AZ2 Catagory A: 67 labs (50%)

Good: 85%

Satisfactory: 10 %

Unsatisfactory: 4%


• Test Item

– Maize. Kernels from a fodder variety

• Planned shipment date – 13 April 2015

EUPT-CF9


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