EUPT-FV17Results.ppt [Modo de compatibilidad] · 2015. 10. 28. · André de Kok Ralf Lippold Sonja...

EUPT-FV17 Results

EUPT-FV17 Results Stuttgart 1st October 2015

DG SANTEMrs. Almut Bitterhof

ORGANISING GROUPAmadeo R. Fernández-AlbaMilagros MezcuaOctavio MalatoCarmen Ferrer

QUALITY CONTROL GROUPAntonio ValverdeStewart Reynolds

STATISTICAL GROUPCarmelo Rodríguez

ADVISORY GROUPMichelangelo AnastassiadesMiguel GamónMagnus JezussekAndré de KokRalf Lippold Sonja MasselterTuija Pihlström Mette Erecius PoulsenDarinka StajnbaherFinbarr O’ReganPhilippe Gros

EUPT-Panel

Mrs. Veerle Vanheusden


Broccoli


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


Before harvest the broccolis were treated with commercial formulations


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

Commercial products used to treat the sample


Preparation of the test item

EUPT-FV17 Results

ParticipationN

o of

Lab

s

EUPT-FV17 Results

Country No. of Labs Country No. of Labs Country No. of LabsAustria 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 11Total No. of Labs = 185Total No. of Non-EU countries Labs = 17Total No. of Countries = 44

EU countries. EFTA countries. Other countries

France 7 Portugal 2

Germany 29 Romania 4

Greece 10 Saudi Arabia 1


Total No. of Labs = 185

EU/EFTA Labs = 168

Other countries Labs = 17

Participation

(27 EU + 3 EFTA + 2 Candidate countries + 12 other countries)

Total No. of Countries = 44

EU/EFTA countries = 30

Other countries = 14


183 pesticides3-hydroxy-carbofuranAcephateAcetamipridAcrinathrinAldicarbAldicarb SulfoneAldicarb SulfoxideAzinphos-methylAzoxystrobinBenfuracarbBenomylBifenthrinBitertanolBoscalidBromopropylateBromuconazoleBupirimateBuprofezinCadusafosCarbarylCarbendazim CarbofuranCarbosulfanChlorfenapyrChlorfenvinphosChlorobenzilateChlorothalonilChlorpropham (only parent compound)ChlorpyrifosChlorpyrifos-methylClofentezine (only parent compound)ClothianidinCyfluthrin (cyfluthrin incl. other mixtures of constituent isomers (sum of isomers))Cypermethrin Cyproconazole Cyprodinil

DeltamethrinDemeton-S-methylsulfoneDesmethyl-pirimicarbDiazinonDichlofluanid (only parent compound)DichlorvosDicloranDicofolDiethofencarbDifenoconazoleDiflubenzuronDimethoateDimethomorphDimethylaminosulfotoluidide (DMST)DiniconazoleDiphenylamineEndosulfan alphaEndosulfan betaEndosulfan sulfateEPNEpoxiconazoleEthionEthirimolEthoprophosEtofenproxFenamidoneFenamiphosFenamiphos sulfoneFenamiphos sulfoxideFenarimolFenazaquinFenbuconazoleFenhexamidFenitrothionFenoxycarbFenpropathrin

FenpropimorphFenpyroximateFenthionFenthion oxonFenthion oxon sulfoneFenthion oxon sulfoxideFenthion sulfoneFenthion sulfoxideFenvalerate and EsfenvalerateFipronil (only parent compound)FludioxonilFlufenoxuronFluopicolide FluopyramFluquinconazoleFlusilazoleFlutolanil FlutriafolFosthiazateHexaconazoleHexythiazoxImazalilImidaclopridIndoxacarb (Indoxacarb as sum of the isomers S and R)IprodioneIprovalicarbIsocarbophosIsofenphos-methylIsoprothiolaneKresoxim-methylLambda-CyhalothrinLinuronLufenuronMalaoxonMalathion

MandipropamidMepanipyrim (only parent compound)MetaflumizoneMetalaxyl and metalaxyl-MMetconazoleMethamidophosMethidathionMethiocarbMethiocarb sulfoneMethiocarb sulfoxideMethomylMethoxyfenozideMonocrotophosMyclobutanilOmethoateOrthophenylphenolOxadixylOxamylOxydemeton-methylPaclobutrazoleParaoxon-methylParathion-ethylParathion-methyl PenconazolePencycuronPendimethalinPermethrinPhenthoatePhosalonePhosmet Phosmet oxonPhoximPirimicarbPirimiphos-methylProchloraz (only parent compound)Procymidone

ProfenofosPropargitePropiconazolePropyzamideProthioconazole (Prothioconazole-desthio)ProthiofosPyraclostrobinPyridabenPyrimethanilPyriproxyfenQuinoxyfenSpinosad (sum of spinosyn A and spinosyn SpirodiclofenSpiroxamineTau-FluvalinateTebuconazoleTebufenozideTebufenpyradTeflubenzuronTefluthrinTerbuthylazineTetraconazoleTetradifonThiabendazoleThiaclopridThiamethoxamThiodicarbThiophanate-methylTolclofos-methylTolylfluanidTriadimefonTriadimenolTriazophosTrichlorfon (only parent compound)TrifloxystrobinTriflumuronTrifluralinTriticonazoleVinclozolin (only parent compound)Zoxamide

Target List

12 New compounds


Pesticides used for thetreatment

Bupirimate PendimetalinCarbendazim Permethrin*Diazinon SpinosadDifenoconazole ThiabendazoleDiflubenzuron TrifloxystrobinMethoxyfenozide Total: 11

ALL INCLUDED IN MACPCOMMISSION IMPLEMENTING REGULATION (EU)

No 400/2014 of 22 April 2014concerning a coordinated multiannual controlprogramme of the Union for 2015, 2016 and 2017 toensure compliance with maximum residue levels ofpesticides and to assess the consumer exposureto pesticide residues in and on food of plant andanimal origin .

* New in the target list


ACTIVITY DATE

- Publishing the Target Pesticide List. Calendar and Matrix on the Web page. 15th December 2014

- Receiving Application Form from invited laboratories. 12th Jan-13th Feb 2015

- Specific Protocol published on the Web site. 23rd Feb 2015 at the latest

- Deadline for receiving Laboratory scope: Form 0 23rd Feb-6th March 2015

- Sample distribution. 16th March 2015

- Deadline for receiving sample acceptance: Form 1 20th March 2015

- Deadline for receiving results: Forms 2. 3 and 4 13th April 2015

- Filling in Form 5 20th-24th April 2015

- Preliminary Report: only results. no statistical treatment. May 2015

- Final Report distributed to the Laboratories. December 2015

Calendar


The homogeneity in the treated sample was studiedusing the 2006 Harmonised Protocol.

Homogeneity

All the pesticides passed the homogeneity test


Homogeneity

mg/kg


Stability

ISO 13528. Annex B

Sub-sample1

Sub-sample 2

Sub-sample 3

Sub-sample 4

Sub-sample 5

Sub-sample 6


Stability

2nd Analysis - after the deadline for reporting results

1st Analysis - prior to the sample shipment

3rd Analysis - reproducing the delivery conditions that the samples experienced during 48 hours

ISO 13528. Annex B

| x1 - yi | ≤ 0.3×σ

All the pesticides passed the stability test

EUPT-FV17 Results

Results


Pesticides Robust mean (mg/kg)

Uncertainty(mg/kg)

Spinosad 0.051 0.003Pendimethalin 0.062 0.003Diazinon 0.071 0.003Bupirimate 0.16 0.006Permethrin 0.17 0.007Diflubenzuron 0.32 0.019Methoxyfenozide 0.35 0.014Trifloxystrobin 0.47 0.016Carbendazim 0.51 0.023Difenoconazole 0.53 0.016Thiabendazole 1.90 0.071

Assigned valuesEU/EFTA Laboratories


Pesticides Robust mean (mg/kg)Spinosad 0.051Pendimethalin 0.062Diazinon 0.071Bupirimate 0.16Permethrin 0.17Diflubenzuron 0.32Methoxyfenozide 0.35Trifloxystrobin 0.47Carbendazim 0.51Difenoconazole 0.53Thiabendazole 1.90

0.051-0.100 mg/kg

EU/EFTA Laboratories



0.051-0.100 mg/kg

0.100-0.500 mg/kg




0.051-0.100 mg/kg

0.100-0.500 mg/kg

> 0.500 mg/kg



Bupirimate

mg/kg

Freq

uenc

y

0 0.3 0.6 0.9 1.2 1.5 1.80

20

40

60

80Mean: 0.165 mg/kg

Mean: 0.469 mg/kg

Distribution of data-HistogramsCarbendazim

mg/kg

Freq

uenc

y

0 1 2 3 4 50

10

20

30

40

50

60

Diazinon

mg/kg

Freq

uenc

y

0 0.03 0.06 0.09 0.12 0.15 0.180

10

20

30

40

50

60

Difenocozole

mg/kg

Freq

uenc

y

0 0.2 0.4 0.6 0.80

20

40

60

80

Mean: 0.512 mg/kg

Mean: 0.071 mg/kg Mean: 0.530 mg/kg



Distribution of data-HistogramsDiflubenzuron

mg/kg

Freq

uenc

y

0 0.4 0.8 1.2 1.6 20

10

20

30

40

Methoxyfenozide

mg/kg

Freq

uenc

y

0 0.2 0.4 0.6 0.80

10

20

30

40

50

60

Pendimethalin

mg/kg

Freq

uenc

y

0 0.05 0.1 0.15 0.2 0.250

20

40

60

80

100

Permethrin

mg/kg

Freq

uenc

y

0 0.2 0.4 0.6 0.8 10

10

20

30

40

50

60





Spinosad

mg/kg

Freq

uenc

y

0 0.05 0.1 0.15 0.2 0.25 0.30

10

20

30

40

50

Thiabendazole

mg/kg

Freq

uenc

y

0 1 2 3 4 5 60

20

40

60

80

Trifloxystrobin

mg/kg

Freq

uenc

y

0 0.2 0.4 0.6 0.8 10

10

20

30

40

50

60

Distribution of data-Histograms


Mean: 0.466 mg/kg



Pesticides MRRL (mg/kg) Robust mean (mg/kg) CV (%)

Bupirimate 0.010 0.165 18.2

Carbendazim 0.010 0.512 21.1

Diazinon 0.010 0.071 18.5

Difenoconazole 0.010 0.530 15.1

Diflubenzuron 0.010 0.319 25.6

Methoxyfenozide 0.010 0.349 17.7

Pendimethalin 0.010 0.062 21.6

Permethrin 0.010 0.174 21.4Spinosad (sum of spinosyn A a spinosyn D. expr. as spinosad) 0.010 0.051 24.0

Thiabendazole 0.010 1.900 18.0

Trifloxystrobin 0.010 0.466 17.5


Dispersion of Results


Dispersion of ResultsEU/EFTA Laboratories


PesticidesNo. of

Reported Results

No. of False Negative

Results

No. of Not Analysed

Results

Percentage of Reported Results

(out of 165)

Bupirimate 154 0 11 93Carbendazim 140 0 25 85Diazinon 160 2 3 97Difenoconazole 151 1 13 92Diflubenzuron 111 2 52 67Methoxyfenozide 128 0 37 78Pendimethalin 152 1 12 92Permethrin 152 1 12 92Spinosad 125 2 38 76Thiabendazole 143 2 20 87Trifloxystrobin 152 0 13 92


EUPT-FV17 Results

z-Scores


Acceptable Questionable Unacceptable

z-Scores classificationEU/EFTA Laboratories


Pesticides Robust Mean (mg/kg)

% Acceptable z-scores

% Questionable

z-scores

% Unacceptable z-scores

Bupirimate 0.165 93.5 1.9 4.5Carbendazim 0.512 86.4 5.7 7.9Diazinon 0.071 92.6 4.3 3.1Difenoconazole 0.530 97.4 1.3 1.3Diflubenzuron 0.319 84.1 8.0 8.0Methoxyfenozide 0.349 96.1 3.1 0.8Pendimethalin 0.062 92.2 5.9 2.0Permethrin 0.174 93.5 2.6 3.9Spinosad(sum of spinosyn A aspinosyn D. expr. as spinosad)

0.051 90.6 1.6 7.9

Thiabendazole 1.900 93.1 1.4 5.5Trifloxystrobin 0.466 96.7 1.3 2.0



Bupirimate

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab158Lab017Lab025Lab071Lab093Lab156Lab005Lab011Lab115Lab131Lab154Lab019Lab148Lab152Lab163Lab053Lab124Lab119Lab026Lab036Lab054Lab170Lab103Lab069Lab120Lab166Lab009Lab012Lab034Lab037Lab044Lab049Lab092Lab117Lab133Lab134Lab048Lab132Lab111Lab101Lab107Lab038Lab161Lab031Lab151Lab182Lab073Lab160Lab062Lab137Lab157Lab130Lab135Lab024Lab147Lab181Lab183Lab002Lab030Lab171Lab018Lab035Lab040Lab056Lab058Lab102Lab113Lab146Lab185Lab051Lab106Lab121Lab168Lab149Lab162Lab169Lab105Lab081Lab082Lab022Lab079Lab080Lab136Lab013Lab027Lab065Lab076Lab085Lab089Lab094Lab099Lab110Lab142Lab067Lab108Lab144Lab014Lab015Lab084Lab006Lab021Lab179Lab095Lab057Lab041Lab074Lab109Lab159Lab070Lab088Lab116Lab100Lab114Lab016Lab098Lab176Lab047Lab077Lab083Lab086Lab143Lab052Lab029Lab072Lab097Lab129Lab138Lab140Lab078Lab045Lab010Lab060Lab064Lab167Lab032Lab068Lab128Lab123Lab141Lab087Lab046Lab126Lab001Lab003Lab007Lab091Lab061Lab145Lab043Lab042Lab174Lab023Lab112Lab020

or L ≡ LCor G ≡ GCor B ≡ Both0 False Negative

93.5 % Acceptable1.9 % Questionable4.5 % Unacceptable

Robust Mean: 0.165 mg/kg


Carbendazim

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab158Lab112Lab045Lab119Lab038Lab017Lab169Lab128Lab154Lab015Lab003Lab133Lab101Lab143Lab168Lab111Lab025Lab134Lab093Lab011Lab031Lab034Lab064Lab107Lab183Lab019Lab012Lab024Lab135Lab179Lab009Lab014Lab067Lab160Lab105Lab156Lab087Lab043Lab167Lab013Lab044Lab077Lab095Lab048Lab079Lab046Lab076Lab126Lab026Lab049Lab065Lab040Lab042Lab171Lab174Lab007Lab170Lab018Lab070Lab072Lab138Lab185Lab060Lab030Lab086Lab147Lab032Lab097Lab117Lab137Lab053Lab102Lab027Lab148Lab084Lab144Lab159Lab123Lab140Lab023Lab162Lab010Lab020Lab069Lab006Lab091Lab108Lab050Lab182Lab098Lab089Lab094Lab114Lab099Lab161Lab181Lab083Lab100Lab036Lab056Lab078Lab082Lab109Lab058Lab005Lab073Lab047Lab029Lab074Lab124Lab041Lab080Lab068Lab120Lab035Lab136Lab062Lab037Lab071Lab116Lab176Lab121Lab106Lab057Lab022Lab021Lab113Lab132Lab061Lab088Lab145Lab052Lab054Lab173Lab085Lab166Lab150Lab103Lab110Lab142





Diazinon

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab110Lab169Lab158Lab017Lab150Lab025Lab011Lab173Lab071Lab166Lab148Lab075Lab005Lab026Lab044Lab092Lab131Lab077Lab133Lab008Lab043Lab015Lab038Lab101Lab124Lab128Lab163Lab120Lab062Lab009Lab019Lab031Lab037Lab039Lab054Lab117Lab134Lab152Lab168Lab183Lab144Lab001Lab160Lab012Lab049Lab088Lab041Lab029Lab102Lab113Lab105Lab013Lab022Lab127Lab174Lab048Lab149Lab179Lab182Lab045Lab083Lab142Lab145Lab035Lab052Lab111Lab121Lab126Lab157Lab021Lab034Lab087Lab093Lab115Lab119Lab185Lab002Lab014Lab036Lab042Lab051Lab076Lab082Lab132Lab040Lab171Lab147Lab137Lab027Lab053Lab072Lab162Lab073Lab078Lab081Lab086Lab106Lab130Lab151Lab018Lab024Lab109Lab135Lab138Lab139Lab159Lab079Lab010Lab064Lab069Lab098Lab099Lab100Lab136Lab058Lab091Lab094Lab108Lab067Lab003Lab020Lab046Lab097Lab154Lab047Lab023Lab032Lab056Lab084Lab089Lab114Lab156Lab164Lab167Lab181Lab080Lab176Lab030Lab129Lab103Lab161Lab123Lab143Lab016Lab085Lab095Lab065Lab140Lab068Lab118Lab116Lab007Lab070Lab006Lab050Lab057Lab061Lab074Lab060Lab112Lab141Lab107

or L ≡ LCor G ≡ GCor B ≡ Both*False Negative



**

GGGGGGL


Difenoconazole

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab059Lab164Lab158Lab025Lab011Lab071Lab094Lab173Lab114Lab163Lab169Lab001Lab026Lab124Lab131Lab133Lab148Lab009Lab043Lab019Lab005Lab079Lab185Lab037Lab048Lab168Lab183Lab031Lab032Lab087Lab160Lab154Lab101Lab111Lab132Lab103Lab073Lab083Lab036Lab012Lab024Lab034Lab054Lab147Lab120Lab171Lab077Lab060Lab135Lab067Lab166Lab085Lab093Lab113Lab105Lab121Lab015Lab053Lab151Lab107Lab029Lab035Lab128Lab108Lab021Lab145Lab014Lab082Lab013Lab040Lab072Lab146Lab174Lab069Lab137Lab064Lab136Lab027Lab017Lab038Lab138Lab050Lab142Lab022Lab046Lab052Lab065Lab078Lab062Lab170Lab159Lab157Lab102Lab097Lab106Lab112Lab080Lab076Lab057Lab074Lab126Lab045Lab056Lab081Lab116Lab091Lab047Lab100Lab010Lab075Lab161Lab020Lab041Lab003Lab042Lab088Lab099Lab061Lab119Lab098Lab176Lab049Lab084Lab115Lab095Lab030Lab143Lab044Lab109Lab140Lab181Lab002Lab018Lab086Lab092Lab162Lab123Lab068Lab089Lab110Lab007Lab070Lab156Lab144Lab167Lab182Lab058Lab141Lab016Lab179Lab117Lab006




*

GG L L L L L G L B G


Diflubenzuron

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab019Lab158Lab173Lab116Lab071Lab105Lab112Lab162Lab025Lab079Lab091Lab126Lab166Lab026Lab053Lab168Lab160Lab120Lab031Lab044Lab161Lab020Lab027Lab035Lab037Lab124Lab015Lab171Lab082Lab135Lab013Lab032Lab080Lab128Lab102Lab100Lab012Lab005Lab108Lab095Lab061Lab067Lab084Lab024Lab021Lab159Lab144Lab069Lab103Lab064Lab085Lab137Lab119Lab042Lab049Lab086Lab101Lab147Lab076Lab009Lab060Lab087Lab132Lab048Lab078Lab097Lab062Lab046Lab083Lab109Lab030Lab093Lab176Lab010Lab098Lab167Lab070Lab072Lab073Lab050Lab111Lab088Lab018Lab092Lab011Lab040Lab143Lab029Lab068Lab047Lab179Lab014Lab022Lab182Lab123Lab156Lab094Lab169Lab077Lab089Lab041Lab185Lab181Lab142Lab183Lab058Lab038Lab057Lab036Lab136Lab043Lab054Lab074




* *

L L L


Methoxyfenozide

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab045Lab158Lab094Lab034Lab103Lab079Lab162Lab019Lab026Lab054Lab025Lab092Lab160Lab111Lab119Lab085Lab185Lab161Lab120Lab088Lab022Lab083Lab148Lab107Lab114Lab174Lab073Lab005Lab132Lab168Lab035Lab009Lab121Lab038Lab093Lab171Lab043Lab135Lab137Lab183Lab053Lab062Lab024Lab142Lab080Lab095Lab128Lab147Lab082Lab110Lab087Lab106Lab145Lab017Lab048Lab067Lab101Lab011Lab013Lab029Lab037Lab049Lab071Lab014Lab091Lab167Lab020Lab108Lab027Lab032Lab072Lab097Lab105Lab127Lab100Lab061Lab046Lab126Lab084Lab144Lab010Lab156Lab036Lab098Lab042Lab069Lab159Lab047Lab143Lab064Lab109Lab018Lab056Lab086Lab077Lab176Lab169Lab057Lab052Lab012Lab070Lab181Lab058Lab078Lab089Lab116Lab123Lab074Lab030Lab179Lab102Lab007Lab044Lab068Lab113Lab041Lab076Lab140Lab050Lab015Lab060Lab112Lab040Lab141Lab124Lab136Lab182Lab021




L L L L L L L


Pendimethalin

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab169Lab158Lab025Lab011Lab115Lab148Lab054Lab003Lab015Lab039Lab071Lab131Lab152Lab037Lab170Lab034Lab075Lab049Lab073Lab005Lab030Lab120Lab127Lab133Lab029Lab038Lab077Lab019Lab031Lab101Lab117Lab126Lab132Lab183Lab143Lab111Lab142Lab145Lab147Lab009Lab021Lab069Lab121Lab157Lab044Lab026Lab168Lab056Lab124Lab144Lab149Lab102Lab105Lab053Lab097Lab160Lab179Lab041Lab045Lab094Lab103Lab134Lab154Lab182Lab185Lab012Lab062Lab084Lab106Lab017Lab027Lab036Lab085Lab137Lab047Lab013Lab035Lab128Lab135Lab171Lab022Lab040Lab061Lab082Lab146Lab151Lab048Lab130Lab162Lab018Lab052Lab058Lab083Lab139Lab010Lab076Lab081Lab099Lab156Lab078Lab086Lab107Lab167Lab176Lab080Lab014Lab043Lab067Lab023Lab032Lab060Lab089Lab092Lab100Lab110Lab159Lab181Lab002Lab042Lab050Lab001Lab108Lab109Lab112Lab079Lab024Lab088Lab095Lab164Lab098Lab114Lab161Lab046Lab072Lab116Lab068Lab091Lab138Lab065Lab007Lab064Lab087Lab070Lab057Lab123Lab141Lab093Lab113Lab119Lab074Lab136Lab016Lab166




*

L L L


Permethrin

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab019Lab119Lab025Lab011Lab052Lab008Lab038Lab115Lab183Lab111Lab120Lab071Lab145Lab148Lab173Lab139Lab093Lab036Lab031Lab049Lab017Lab126Lab069Lab103Lab121Lab009Lab039Lab113Lab118Lab134Lab152Lab185Lab157Lab168Lab143Lab094Lab048Lab073Lab034Lab021Lab029Lab037Lab054Lab133Lab012Lab132Lab005Lab164Lab022Lab124Lab130Lab171Lab053Lab105Lab075Lab135Lab159Lab015Lab144Lab160Lab077Lab142Lab010Lab026Lab032Lab078Lab097Lab162Lab001Lab059Lab062Lab030Lab079Lab002Lab045Lab102Lab137Lab013Lab018Lab027Lab035Lab099Lab107Lab110Lab117Lab127Lab131Lab169Lab100Lab149Lab156Lab088Lab147Lab174Lab098Lab040Lab086Lab179Lab023Lab041Lab044Lab068Lab084Lab151Lab060Lab076Lab108Lab128Lab057Lab042Lab046Lab064Lab082Lab080Lab065Lab138Lab072Lab083Lab070Lab114Lab024Lab087Lab161Lab116Lab061Lab067Lab051Lab167Lab091Lab056Lab089Lab182Lab014Lab050Lab109Lab081Lab047Lab003Lab146Lab074Lab043Lab123Lab176Lab181Lab058Lab141Lab092Lab112Lab095Lab163Lab007Lab016Lab166




*

GGG


Spinosad

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab054Lab128Lab158Lab103Lab114Lab071Lab082Lab142Lab079Lab031Lab037Lab005Lab034Lab025Lab026Lab119Lab087Lab011Lab019Lab068Lab109Lab124Lab185Lab015Lab077Lab029Lab048Lab120Lab123Lab133Lab085Lab092Lab111Lab093Lab168Lab083Lab088Lab107Lab144Lab147Lab161Lab009Lab080Lab062Lab038Lab069Lab078Lab101Lab110Lab174Lab017Lab049Lab105Lab121Lab135Lab183Lab013Lab136Lab171Lab176Lab041Lab072Lab023Lab106Lab181Lab022Lab126Lab024Lab160Lab007Lab053Lab086Lab097Lab162Lab010Lab058Lab073Lab108Lab046Lab061Lab116Lab067Lab003Lab014Lab074Lab084Lab100Lab112Lab047Lab098Lab102Lab132Lab137Lab030Lab060Lab064Lab056Lab095Lab141Lab179Lab032Lab113Lab182Lab027Lab089Lab159Lab035Lab143Lab167Lab012Lab148Lab040Lab156Lab057Lab070Lab169Lab094Lab021Lab018Lab127Lab036Lab044Lab043Lab091Lab042Lab050Lab076




*

L L

*


Thiabendazole

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab110Lab163Lab127Lab065Lab116Lab059Lab151Lab003Lab162Lab023Lab085Lab154Lab185Lab183Lab168Lab045Lab093Lab148Lab049Lab114Lab071Lab136Lab079Lab132Lab025Lab026Lab174Lab042Lab001Lab103Lab112Lab034Lab128Lab035Lab017Lab027Lab069Lab073Lab111Lab024Lab012Lab105Lab106Lab137Lab037Lab068Lab107Lab099Lab143Lab160Lab157Lab161Lab052Lab067Lab074Lab009Lab170Lab108Lab056Lab050Lab147Lab083Lab018Lab044Lab133Lab145Lab038Lab101Lab030Lab100Lab031Lab120Lab135Lab088Lab144Lab020Lab064Lab113Lab089Lab048Lab010Lab140Lab060Lab117Lab040Lab091Lab121Lab176Lab005Lab041Lab054Lab138Lab006Lab014Lab062Lab109Lab159Lab036Lab047Lab141Lab179Lab046Lab084Lab053Lab097Lab123Lab072Lab124Lab171Lab078Lab080Lab015Lab013Lab167Lab007Lab087Lab070Lab032Lab126Lab169Lab098Lab077Lab029Lab086Lab011Lab016Lab082Lab076Lab043Lab057Lab102Lab022Lab158Lab173Lab095Lab061Lab181Lab182Lab021Lab058Lab156Lab094Lab019Lab150Lab142




**

L L G L


Trifloxystrobin

-5,0

-4,0

-3,0

-2,0

-1,0

0,0

1,0

2,0

3,0

4,0

5,0

Lab127Lab158Lab023Lab019Lab075Lab053Lab163Lab011Lab094Lab170Lab111Lab119Lab026Lab124Lab025Lab015Lab135Lab009Lab113Lab115Lab133Lab148Lab048Lab098Lab073Lab183Lab005Lab134Lab174Lab132Lab012Lab145Lab047Lab168Lab037Lab049Lab101Lab102Lab001Lab083Lab121Lab120Lab054Lab157Lab185Lab093Lab062Lab105Lab179Lab069Lab160Lab031Lab103Lab079Lab106Lab038Lab143Lab029Lab117Lab147Lab154Lab017Lab043Lab128Lab077Lab144Lab013Lab092Lab142Lab151Lab107Lab087Lab041Lab035Lab036Lab080Lab146Lab130Lab171Lab003Lab108Lab072Lab057Lab034Lab081Lab082Lab137Lab002Lab061Lab126Lab014Lab078Lab112Lab018Lab052Lab097Lab152Lab099Lab044Lab067Lab070Lab089Lab116Lab176Lab100Lab076Lab136Lab064Lab084Lab159Lab169Lab010Lab123Lab088Lab162Lab086Lab156Lab140Lab046Lab110Lab030Lab060Lab042Lab024Lab022Lab027Lab109Lab032Lab065Lab138Lab016Lab074Lab045Lab050Lab161Lab056Lab114Lab059Lab141Lab040Lab091Lab167Lab068Lab095Lab006Lab007Lab085Lab129Lab182Lab181Lab058Lab021




EUPT-FV17 Results

Combined z-Scores


Average of Squared z-Scores

AZ2 ≤ 2.0 Good2.0 < AZ2 < 3.0 Satisfactory

AZ2 ≥ 3.0 Unsatisfactory


NRLs OfLs

AZ2 Representation

80 % Good 7 % Satisfactory 13 % Unsatisfactory

Category A: 68.5 % of the EU/EFTA Laboratories

(113 Laboratories out of 165)

EUPT-FV16: 92 % Good 5 % Satisfactory 3 % Unsatisfactory

EUPT-FV16: 59%



6 different laboratories from EU/EFTA countries reported 6 pesticides as false

positives


False Positives


Laboratory Code Pesticide Concentration

(mg/kg)Determination

Technique RL

(mg/Kg)MRRL

(mg/Kg)

Lab027 Bromopropylate 0.014 GC-MS/MS 0.01 0.01

Lab098 Bromopropylate 0.021 GC-MS 0.01 0.01

Lab051 Bromopropylate 0.039 GC-MS 0.01 0.01

Lab173 Carbaryl 0.020 GC-MS/MS 0.01 0.01

Lab158 Fenpropathrin 0.020 GC-MS 0.01 0.01

Lab164 Kresoxim-methyl 0.015 GC-MS/MS 0.01 0.01

Lab173 Orthophenylphenol 2.95 HPLC-UV 0.1 0.01

Lab173 Tetradifon 0.014 GC-MS/MS 0.01 0.01


False Positives


Bromopropylate

Carbaryl

Fenpropathrin

Kresoxim-methyl

Tetradifon

False Positives

HPLC-UVOrthophenylphenol

GC-MS or GC-MS/MS



Bromopropylate in FV17

EUPT-FV17 Blank 10 µg/kg Std in Broccoli EUPT-FV17 Sample

Ratio: 7.1%Ratio: 0.9%

MRM1: 341 > 185MRM2: 341 > 155


Bupirimate Carbendazim DiazinonDifenoconazole Diflubenzuron Methoxyfenozide Pendimetalin

Permethrin SpinosadThiabendazole Trifloxystrobin

Cyprodinil

Ethirimol

Fludioxonil

Concentrations below MRRL (0.01 mg/kg)

Overview of the EUPTs-FV

Stuttgart 1st October 2015Overview of the EUPTs-FV




1995-2004

• 5 PTs on MRM in FV

Proficiency Tests - History

2004 2005 2006 2007 2008 2009



Proficiency Tests - History

2010 2011 2012 2013 2014

ISO/IEC 17043

2015



Participant countries-Other countries (18)



EUPT Nº Matrices Nº of Participants

Nº of PossiblePesticides

Nº of pesticidesevaluated in test

item

1 Pepper 88 33 6

2 Apple 85 41 6

3 Cucumber 116 48 14

4 Orange 117 57 14

5 Lettuce 127 57 15

6 Tomato 130 57 13

7 Grape 128 65 16

8 Aubergine 129 68 16

9 Strawberry 137 82 19

10 Carrot 132 113 18

11 Cauliflower 151 128 21

12 Leek 153 144 17

13 Mandarin 154 144 19

14 Pear 167 175 18

15 Potato 175 175 18

16 Pepper 183 175 22

17 Broccoli 185 183 11

EUPT-FV1 to EUPT-FV17 in numbers



Acephate Difenoconazole Kresoxim-methyl PirimicarbAcetamiprid Diflubenzuron Lambda-Cyhalothrin Pirimphos-methylAcrinathrin Dimethoate Linuron ProchlorazAldicarb(sum) Diphenilamine Malathion ProcydimoneAmitraz (DMPF&DMF) Dithiocarbamates(CS2) Mecarbam PropoxurAzinphos-methyl Endosulfan Metalaxyl PropyzamideAzoxystrobin EPN Metamidophos ProthiofosBifenthrin Fenamiphos Methidathion PyraclostrobinBoscalid Fenamiphos sulfone Methiocarb sum PyridabenBromopropylate Fenamiphos sulfoxide Methiocarb PyrimethanilBupirimate Ethion Methomyl PyriproxifenBuprofezin Fenhexamid Methoxyfenozide QuinoxyfenCadusafos Fenitrothion Methyl-Tiophanate QuintozeneCaptan Fenpropathrin Mevinphos SpinosadCarbaryl Fludioxinil Monocrotophos SpirodiclofenCarbendazim Flufenoxuron Myclobutanil TebuconazoleCarbofuran sum Fluopicolide Omethoate Tetraconazole Chlorpropham Flutolanil Ortophenilphenol ThiabendazoleChlorpyrifos Folpet Oxamyl ThiaclopridChlorpyrifos-methyl Fosthiazate Oxydemeton-methyl Tolclofos-methylChlothalonil Hexythiazox Parathion TolyfluanidCypermethrin Imazalil Penconazole TriadimenolCyprodinil Imidacloprid Pencycuron TriazophosDelthamethrin Indoxacarb Pendimethalin TrifloxystrobinDiazinon Iprodione Permethrin TriflumuronDichlofluanid Iprovalicarb Phosalone VinclozolinDicofol Isofenphos-methyl Phosmet

Pesticides Used to Treat the Sample in last ten EUPT-FVs



Summary of Results



Number of results reported by extraction method

Extraction methods



Acceptable Ques tionable Inacceptable Acceptable Ques tionable Inacceptable Acceptable Ques tionable InacceptableE UPT ‐FV16 91,7 7,7 0,6 93,9 2,9 3,2 95,5 2,9 1,6E UPT ‐FV15 93,0 3,4 3,6 87,7 4,2 8,2 88,6 3,9 7,5E UPT ‐FV14 96,2 1,8 2 93,9 3,1 3 94,3 3 2,7

Acetone QuE C hE R S AcE t

Classification of z-scores by extraction method

Extraction methods



0

10

20

30

40

50

60

25% FFP RSD

(Qn

RSD

, %)

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

Dispersion of Results (RSD, %)



No.

Dispersion of Results (RSD, %)



Acceptable Questionable Unacceptable

%

1776results

1950results

1590results

2363results

1555results

2254results

2209results

2486results

3133results

Classification of z-scores



71 %

51 % 51 % 51 %

45 %

56 %52 % 52 %

59 %

%

Laboratories in Category A

68.5 %



False Negatives and Positives

EUPT-FV17Results.ppt [Modo de compatibilidad] · 2015. 10. 28. · André de Kok Ralf Lippold Sonja...

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