european union proficiency test in fruits and vegetables ... · european union proficiency test in...

48
European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Upload: vodan

Post on 26-Apr-2018

215 views

Category:

Documents


1 download

TRANSCRIPT

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Preparation of the test item

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

ACTIVITY DATE

Publishing the Calendar and Matrix on the EURL-FV Web page. 15th November 2013

Submission of Application Form by invited laboratories.23rd Dec 2013

-

31st Jan 2014

Specific Protocol published on the Web site. 3rd Feb 2014 at the latest

Sample distribution. 24th February 2014

Submission of sample receipt and acceptance - Form 0.As soon as sample is

received

Deadline for receiving results - Form172 hours after receiving

the sample

Preliminary Report. End of April 2014

Final Report distributed to the Laboratories. November 2014

Calendar

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

EUROPEAN PROFICIENCY TEST - FRUITS AND VEGETABLES -

MASS SCREENING 06- Participants

COUNTRY No. COUNTRY No.

Austria 1* Ireland 1*

Belgium 1*+2 Italy 6

China 2 Latvia 1*

Croatia 1 Romania 2*+1

Czech Republic 1*+1 Serbia 1

Denmark 1* Slovenia 1*

Egypt 1 Spain 12

Estonia 1* Sweden 1*+1

Finland 1* Switzerland 1*+1

France 1*+6 The Netherlands 1*+1

Germany 1*+8 Turkey 1

Greece 1 UK 1*+2

Hungary 1*+1

18 NRLs*

Participants

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

EUROPEAN PROFICIENCY TEST - FRUITS AND VEGETABLES -

MASS SCREENING 06- Participants

COUNTRY No. COUNTRY No.

Austria 1* Ireland 1*

Belgium 1*+2 Italy 6

China 2 Latvia 1*

Croatia 1 Romania 2*+1

Czech Republic 1*+1 Serbia 1

Denmark 1* Slovenia 1*

Egypt 1 Spain 12

Estonia 1* Sweden 1*+1

Finland 1* Switzerland 1*+1

France 1*+6 The Netherlands 1*+1

Germany 1*+8 Turkey 1

Greece 1 UK 1*+2

Hungary 1*+1

18 NRLs*

67

Participants

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

21 EU/EFTA

Countries

China

Egypt

Serbia

Turkey

4 Non EU Countries

Austria

Belgium

Croatia

Czech Republic

Denmark

Estonia

Finland

France

Germany

Greece

Hungary

Ireland

Italy

Latvia

Netherlands

Romania

Slovenia

Spain

Sweden

Switzerland

United Kingdom

8 EU Countries

Not

Participating

Bulgaria

Cyprus

Lithuania

Luxembourg

Malta

Poland

Portugal

Slovakia

Participants

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Participants

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Pesticides used for the treatment

Atrazine

Cadusafos

Carbetamide

Demeton-S-methylsulfone

Dinocap

Dodemorph

Endrin

Ethoprophos

Fenpropidin

Fipronil

Flubendiamide

Fluometuron

Fuberidazole

Furathiocarb

HCB

Metosulam

Phorate

Prosulfocarb

Secbueton

Spiromesifen

Terbufos

Pesticides

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Pesticides used for the treatment

Atrazine

Cadusafos

Carbetamide

Demeton-S-methylsulfone

Dinocap

Dodemorph

Endrin

Ethoprophos

Fenpropidin

Fipronil

Flubendiamide

Fluometuron

Fuberidazole

Furathiocarb

HCB

Metosulam

Phorate

Prosulfocarb

Secbueton

Spiromesifen

Terbufos

Concentrations lower than 0.1 mg/kg

for most of them

Pesticides

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Submission of Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Preliminary Report

Lab

ora

tory

Co

de

Atra

zine

Ca

du

safo

s

Ca

rbe

tam

ide

De

me

ton

-S-m

eth

ylsu

lfon

e

Din

oc

ap

Do

de

mo

rph

En

drin

Eth

op

rop

ho

s

Fe

np

rop

idin

Fip

ron

il

Flu

be

nd

iam

ide

Flu

om

etu

ron

Fu

be

rida

zole

Fu

rath

ioc

arb

HC

B

Me

tosu

lam

Ph

ora

te

Pro

sulfo

ca

rb

Se

cb

um

eto

n

Sp

irom

esife

n

Terb

ufo

s

Re

po

rted

pe

sticid

es

by

Lab

ora

tory

% o

f Re

po

rted

Pe

sticid

es b

y a

bo

rato

ry

001 R R R R R R R R R R R R R R R R R 17 81002 R R R R R R 6 29003 R R R R R R R R R R R R R R R R R R R 19 90004* R R R R R R R R R R R R 12 57006* R R R R R R R R R R R R R R R R R R 18 86007* R R R R R R R R R R R R R R R R R R R R 20 95008 R R R R R R R R R R R R R R R R R R R 19 90009 R R R R R R R R R R R R R R R R R R 18 86010* R R R R R R R R R R R R R R R R R 17 81011 R R R R R R R R R R R R R R R R R R R R 20 95012 R R R R R R R R R R R R 12 57013 R R R R R R R R R R R R R R R R R R R 19 90014 R R R R R R R R R R R R R R 14 67015 R R R R R R R R R R R R R R R R R R R R R 21 100016* R R R R R R R R R R R R R R R R R R R R R 21 100017 R R R R R 5 24018 R R R R R R R R R R R R R R R R 16 76019* R R R R R 5 24020 R R R R R R R R R R R R R 13 62021 R R R R R R R R R R 10 48

Evaluated Pesticides:21 Total No of Reporting Laboratories = 67 (* NRL-FV)

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Preliminary Report

Lab

ora

tory

Co

de

Atra

zine

Ca

du

safo

s

Ca

rbe

tam

ide

De

me

ton

-S-m

eth

ylsu

lfon

e

Din

oc

ap

Do

de

mo

rph

En

drin

Eth

op

rop

ho

s

Fe

np

rop

idin

Fip

ron

il

Flu

be

nd

iam

ide

Flu

om

etu

ron

Fu

be

rida

zole

Fu

rath

ioc

arb

HC

B

Me

tosu

lam

Ph

ora

te

Pro

sulfo

ca

rb

Se

cb

um

eto

n

Sp

irom

esife

n

Terb

ufo

s

Re

po

rted

pe

sticid

es

by

Lab

ora

tory

% o

f Re

po

rted

Pe

sticid

es b

y a

bo

rato

ry

022 R R R R R 5 24023 R R R R R R 6 29024* R R R R R R R R R R R R R R R R R R R R R 21 100025* R R R R R R R R R R R R R R R 15 71026 R R R R R R R R R R R R R R R R R R R R 20 95027 R R R R R R R R R R R R R R R R R R R 19 90028* R R R R R R R R R R R R R R R 15 71029 R R R R R R R R R R R R R R R R R R R R 20 95030 R R R R R R R R R R R R R R R R 16 76031 R R R R R R R R R R R R R R R R 16 76032 R R R R R R R R R R R R R R R R R R 18 86033* R R R R R R R R R 9 43034 R R R R R R R R R 9 43035 R R R R R R R R R R R R R R R R R R R R 20 95036 R R R R R R R R R R R R R R R R R R 18 86037 R R R R R R R R R R R R R R R R R R R R R 21 100038 R R R R R R R R R R R R R R R R R R R R R 21 100039* R R R R R R R R R R R R R R R R 16 76040 R R R R R R R R R R R R R R R R 16 76041* R R R R R R R R R R R R R R R R R 17 81

Evaluated Pesticides:21 Total No of Reporting Laboratories = 67 (* NRL-FV)

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Preliminary Report

Lab

ora

tory

Co

de

Atra

zine

Ca

du

safo

s

Ca

rbe

tam

ide

De

me

ton

-S-m

eth

ylsu

lfon

e

Din

oc

ap

Do

de

mo

rph

En

drin

Eth

op

rop

ho

s

Fe

np

rop

idin

Fip

ron

il

Flu

be

nd

iam

ide

Flu

om

etu

ron

Fu

be

rida

zole

Fu

rath

ioc

arb

HC

B

Me

tosu

lam

Ph

ora

te

Pro

sulfo

ca

rb

Se

cb

um

eto

n

Sp

irom

esife

n

Terb

ufo

s

Re

po

rted

pe

sticid

es

by

Lab

ora

tory

% o

f Re

po

rted

Pe

sticid

es b

y a

bo

rato

ry

042 R R R R R R R R R R R R R R R R R R R 19 90043 R R R R R R R R R R R R 12 57044* R R R R R R R R R R R R R R R R R R R R 20 95045 R R R R R R R R R R 10 48046* R R R R R R R R R R R R R R R R R R R R 20 95047 R R R R R R R R R R R R R R R R 16 76048 R R R R R R R R R R R R R R R R R R 18 86049* R R R R R R R R R R R R R R R 15 71050 R R R R R R R R R R R R R R R R R 17 81051* R R R R R R R R R R R R R R R R 16 76052 R R R R R R R R R R R R R R R 15 71053 R R R R R R R R R R R R R R R R R R R R 20 95054 R R R R R R R R R R R R 12 57055 R R R R R R R R R R R R R R R R R R 18 86056 R R R R R R R R R R R R 12 57057* R R R R R R R R R R R R R R R R R R R R R 21 100058 R R R R R R R R R R R R R R R R R R R 19 90059 R R R R R R R R R 9 43060 R R R R R R R R R R R R R R R R R R R 19 90

Evaluated Pesticides:21 Total No of Reporting Laboratories = 67 (* NRL-FV)

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Preliminary Report

Lab

ora

tory

Co

de

Atra

zine

Ca

du

safo

s

Ca

rbe

tam

ide

De

me

ton

-S-m

eth

ylsu

lfon

e

Din

oc

ap

Do

de

mo

rph

En

drin

Eth

op

rop

ho

s

Fe

np

rop

idin

Fip

ron

il

Flu

be

nd

iam

ide

Flu

om

etu

ron

Fu

be

rida

zole

Fu

rath

ioc

arb

HC

B

Me

tosu

lam

Ph

ora

te

Pro

sulfo

ca

rb

Se

cb

um

eto

n

Sp

irom

esife

n

Terb

ufo

s

Re

po

rted

pe

sticid

es

by

Lab

ora

tory

% o

f Re

po

rted

Pe

sticid

es b

y a

bo

rato

ry

061 R R R 3 14062 R R R R R R R R R R R R R 13 62063 R R R 3 14064 R R R R R R R R R R R R R R R 15 71065 R R R R R R R R R R R R R R R 15 71066 R R R R R R R R R R R R R 13 62067 R R R R R R R R R R R R R R R 15 71068 R R R R R R R R R 9 43

Re

po

rted

Pe

sticid

es

60 64 37 57 25 39 54 66 56 62 33 35 39 55 52 34 50 56 35 52 53

% o

f Re

po

rted

Pe

sticid

es

90 96 55 85 37 58 81 99 84 93 49 52 58 82 78 51 75 84 52 78 79

Evaluated Pesticides:21 Total No of Reporting Laboratories = 67 (* NRL-FV)

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Atr

azi

ne

Ca

du

safo

s

Ca

rbe

tam

ide

De

me

ton

-S-

me

thy

lsu

lfo

ne

Din

oc

ap

Do

de

mo

rph

En

dri

n

Eth

op

rop

ho

s

Fe

np

rop

idin

Fip

ron

il

Flu

be

nd

iam

ide

Flu

om

etu

ron

Fu

be

rid

azo

le

Fu

rath

ioc

arb

HC

B

Me

tosu

lam

Ph

ora

te

Pro

sulfo

ca

rb

Se

cb

um

eto

n

Sp

iro

me

sife

n

Terb

ufo

s

Total Number

of Reported

Pesticides60 64 37 57 25 39 54 66 56 62 33 35 39 55 52 34 50 56 35 51 53

% of Reported

Pesticides 90 96 55 85 37 58 81 99 84 93 49 52 58 82 78 51 75 84 52 76 79

21 Evaluated Pesticides67 Laboratories

21 Pesticides= 2+6+13

Preliminary Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Dinocap

C14H20N2O5

295.1299

ESI (-)

Low percentage of detections

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

\\192.168.211.26\Xcalibur\...\SM06_pos 4/4/2014 10:14:29 AM

RT: 8.99 - 11.96 SM: 7B

9.0 9.2 9.4 9.6 9.8 10.0 10.2 10.4 10.6 10.8 11.0 11.2 11.4 11.6 11.8

Time (min)

0

200000

400000

600000

800000

1000000

Re

lative

Ab

un

da

nce

9.63 9.62

9.00 11.3810.32 11.1110.699.03 11.4610.829.30 10.91 11.28 11.7611.0310.279.829.529.12 11.949.87 9.989.37 10.12 10.5610.44

NL:

1.07E6

Base Peak

m/z=

683.0256-

683.0356

MS

Pimiento_100

ppb_pos

RT: 8.99 - 11.96 SM: 7B

9.0 9.2 9.4 9.6 9.8 10.0 10.2 10.4 10.6 10.8 11.0 11.2 11.4 11.6 11.8

Time (min)

0

100000

200000

300000

400000

500000

600000

Re

lative

Ab

un

da

nce

9.61

9.71

9.0711.8110.26 11.809.18 10.629.55 10.8010.579.26 10.959.95 10.509.34 9.86 10.08 10.169.38 11.1511.10 11.49 11.5410.68 11.29

NL:

6.75E5

Base Peak

m/z=

683.0256-

683.0356

MS

SM06_pos

Pimiento_100ppb_pos #2159 RT: 9.64 AV: 1 NL: 1.13E6

T: FTMS + p ESI Full ms [100.00-800.00]

682.5 683.0 683.5 684.0 684.5 685.0 685.5 686.0 686.5 687.0 687.5 688.0 688.5 689.0 689.5 690.0 690.5 691.0 691.5

m/z

0

20

40

60

80

100

Re

lative

Ab

un

da

nce

683.0320

684.0344

682.6320684.2032 691.0363 691.4369685.0288

689.1022686.4626

XIC Flubendiamide 683.0306± 5 ppm. Spiked at 100µg/kg

XIC Flubendiamide 683.0306± 5 ppm. SM06 Sample

Flubendiamide LC-Orbitrap-MS

Analytical Standard

EUPT-SM06 Sample

Low percentage of detections

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Flubendiamide

XIC Flubendiamide 683.0306 ± 50 ppm spiked at 50 µg/kg

XIC Flubendiamide 683.0306 ± 50 ppm. SM06 Sample

LC-TOF-MS

Low percentage of detections

50 ppb Analytical Standard

EUPT-SM06 Sample

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

25

33 34 35

35 37 39

39

50 51 52 53 54 55 56

56 57 6

0 62 64 66

0

10

20

30

40

50

60

70

80

Din

oc

ap

Flu

be

nd

iam

ide

Me

tosu

lam

Flu

om

etu

ron

Se

cb

um

eto

n

Ca

rbe

tam

ide

Do

de

mo

rph

Fu

be

rida

zole

Ph

ora

te

Sp

irom

esife

n

HC

B

Terb

ufo

s

En

drin

Fu

rath

ioc

arb

Fe

np

rop

idin

Pro

sulfo

ca

rb

De

me

ton

-S-

me

thy

lsulfo

ne

Atra

zine

Fip

ron

il

Ca

du

safo

s

Eth

op

rop

ho

sN

o o

f R

ep

ort

s

SM06 Reported Pesticides(67 Laboratories Reported Data)

Preliminary Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

37

49 51 52

52 55 58

58

75 76 78 79 81 82 84

84 85 9

0 93 96 99

0

10

20

30

40

50

60

70

80

90

100

Din

oc

ap

Flu

be

nd

iam

ide

Me

tosu

lam

Fluo

me

turo

n

Se

cb

um

eto

n

Ca

rbe

tam

ide

Do

de

mo

rph

Fu

be

rida

zole

Ph

ora

te

Sp

irom

esife

n

HC

B

Terb

ufo

s

En

drin

Fu

rath

ioc

arb

Fe

np

rop

idin

Pro

sulfo

ca

rb

De

me

ton

-S-

me

thy

lsulfo

ne

Atra

zine

Fip

ron

il

Ca

du

safo

s

Eth

op

rop

ho

s

% o

f R

ep

ort

s

SM06 % of Reported Pesticides

(67 Laboratories Reported Data)

Preliminary Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

14

14

24

24

24

29

29

43

43

43

43

48

48

52

57

57

57

57

62

62

62

67

71

71

71

71

71

71

71

76

76

76

76

76

76

76

81

81

81

81

86

86

86

86

86

86

90

90

90

90

90

90

90

95

95

95

95

22

95

95

95

10

01

00

10

01

00

10

0100

0

10

20

30

40

50

60

70

80

90

100

Lab

061

Lab

063

Lab

017

Lab

019*

Lab

022

Lab

002

Lab

023

Lab

033*

Lab

034

Lab

059

Lab

068

Lab

021

Lab

045

Lab

054

Lab

004*

Lab

012

Lab

043

Lab

056

Lab

020

Lab

062

Lab

066

Lab

014

Lab

025*

Lab

028*

Lab

049*

Lab

052

Lab

064

Lab

065

Lab

067

Lab

018

Lab

030

Lab

031

Lab

039

Lab

040

Lab

047

Lab

051*

Lab

001

Lab

010*

Lab

041*

Lab

050

Lab

006*

Lab

009

Lab

032

Lab

036

Lab

048

Lab

055

Lab

003

Lab

008

Lab

013

Lab

027

Lab

042

Lab

058

Lab

060

Lab

007*

Lab

011

Lab

026

Lab

029

Lab

035

Lab

044*

Lab

046*

Lab

053

Lab

015

Lab

016*

Lab

024*

Lab

037

Lab

038

Lab

057*

% o

f P

est

icid

es

SM06 % of Reported Pesticides

(21 Pesticides)81% 67% 31%

Preliminary Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

90 92 92 90

81

60

7376

65 67

20 20 22 24

31

0

10

20

30

40

50

60

70

80

90

100

SM02 SM03 SM04 SM05 SM06

% laboratories with more than 50% of pesticides reported

% laboratories with more than 70% of pesticides reported

% laboratories with more than90% of pesticides reported

Preliminary Results

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Non reported pesticides

22

4

16

44

21

17

15

32

22

24 24

31

25

23

14

40

2119

16

43

0

5

10

15

20

25

30

35

40

45

50

0-1 Not Reported 2-3 Not Reported 4-5 Not Reported >5 Not Reported

SM 02

SM 03

SM 04

SM 05

SM06

% labora

tories

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

• Atrazine-desethyl-2-hydroxy

• Carbofuran

• Difenoconazole

• Dimefuron

• Endrin ketone

• Fenamiphos

• Fenamiphos sulfoxide

• Fipronil sulfide

• Fipronil sulfone

• Phorate sulfoxide

• Terbufos sulfoxide

• Triadimenol

Other compounds have been detected or identified and quantified in the sample

by the organizer at concentrations below 10 µg/kg:

Not spiked pesticides in test item

Atrazine Cadusafos Carbetamide Demeton-S-methylsulfone

Dinocap Dodemorph Endrin Ethoprophos Fenpropidin

Fipronil Flubendiamide Fluometuron Fuberidazole Furathiocarb

HCB Metosulam Phorate Prosulfocarb Secbueton

Spiromesifen Terbufos

Not quantified

Detected in the

blank and in

the sample

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Atrazine–desethyl-2-hydroxy

XIC Atrazine-deshetyl-2-hydroxy 170.1036 ± 5 ppm. SM06

Not spiked pesticides in test item

EUPT-SM06 Sample

LC-Orbitrap-MS

Tentative identification

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Mass spectrum Tentative

Identification

ENDRIN KETONE

MW

Exact mass 377.8706

Endrin

Rt 23.851 min

Rt 24.946 min

C12H8Cl6O

C12H8Cl6O

Endrin Ketone

SAMPLE 82 SM06

Not spiked pesticides in test item

GC-TOF-NCI-MS

Tentative identification

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Fipronil sulfide

XIC Fipronil sulfide 418.9365 5 ± 5 ppm. SM06 Sample

ESI (-)

Not spiked pesticides in test item

EUPT-SM06 Sample

LC-Orbitrap-MS

Tentative identification

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Not spiked pesticides in test item

Carbofuran

10 ppb

Analytical Standard

EUPT-SM06 Sample

LC-Orbitrap-MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Error 1.018 ppm

Dimefuron

MS Spectra SM06

Concentration level

<10 µg/kg

Not spiked pesticides in test item

100 ppb Analytical Standard

EUPT-SM06 Sample

Blank Pepper

10 ppb Analytical Standard

LC-Orbitrap-MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Fenamiphos

XIC Fenamiphos 304.1125 ± 20 ppm. SM06 Sample

MS Spectra SM06

Concentration level

<10 µg/kg

LC-TOF-MS

Not spiked pesticides in test item

EUPT-SM06 Sample

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

LC-TOF-MS

XIC Fenamiphos sulfoxide 320.108±20 ppm. SM06 Sample

MS Spectra SM06

Concentration

level

<10 µg/kg

Fenamiphos sulfoxide

Not spiked pesticides in test item

EUPT-SM06 Sample

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Fipronil sulfone

Concentration level

<10 µg/kg

Not spiked pesticides in test item

10 ppb Analytical Standard

EUPT-SM06 Sample

LC-Orbitrap-MS

ESI (-)

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Phorate sulfoxide

MS Spectra SM06

Concentration level

<10 µg/kg

Not spiked pesticides in test item

10 ppb Analytical Standard

EUPT-SM06 Sample

LC-Orbitrap-MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Terbufos

sulfoxide

LC-TOF -MS

Concentration level

<10 µg/kg

Not spiked pesticides in test item

10 ppb Analytical Standard

EUPT-SM06 Sample

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

\\192.168.211.26\Xcalibur\...\SM06_pos 4/4/2014 10:14:29 AM

RT: 7.98 - 12.03 SM: 7B

8.0 8.2 8.4 8.6 8.8 9.0 9.2 9.4 9.6 9.8 10.0 10.2 10.4 10.6 10.8 11.0 11.2 11.4 11.6 11.8 12.0

Time (min)

0

10

20

30

40

50

60

70

80

90

100

Re

lativ

e A

bu

nd

an

ce

10.17

10.3110.41

10.50 10.70 10.78 10.91 11.8911.29 11.7911.4911.17 11.719.949.90

NL:

2.43E6

Base Peak

m/z=

406.0694-

406.0734

MS

Blanco_pos

RT: 7.97 - 12.10 SM: 7B

8.0 8.2 8.4 8.6 8.8 9.0 9.2 9.4 9.6 9.8 10.0 10.2 10.4 10.6 10.8 11.0 11.2 11.4 11.6 11.8 12.0

Time (min)

0

10

20

30

40

50

60

70

80

90

100

Re

lativ

e A

bu

nd

an

ce

10.16 10.17

10.4210.46 10.73 10.91 11.7211.14 11.28 11.6411.50 12.1012.029.91 9.99

NL:

2.22E6

Base Peak

m/z=

406.0694-

406.0734

MS

SM06_pos

SM06_pos #2278 RT: 10.17 AV: 1 SB: 217 1.42-2.38 NL: 1.97E6

T: FTMS + p ESI Full ms [100.00-800.00]

404.0 404.5 405.0 405.5 406.0 406.5 407.0 407.5 408.0 408.5 409.0 409.5 410.0 410.5 411.0 411.5

m/z

0

20

40

60

80

100

120

140

160

Re

lativ

e A

bu

nd

an

ce 406.071

C11 H14 O 11 N6

408.068

C17 H10 O 6 N7

409.072

C26 H9 O 2 N4

407.075

C19 H7 O 2 N10

408.237

C20 H32 O 5 N4

411.274

C22 H33 O N7

410.066

C23 H6 O N8

404.300

C19 H40 O 5 N4

405.262

C22 H35 O 4 N3

406.280

C20 H40 O 7 N

Difenoconazole

Spectra SM06

Concentration level <10 µg/kg

Not spiked pesticides in test item

Blank Pepper

EUPT-SM06 Sample

Present in the blank material

LC-Orbitrap-MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Triadimenol

LC-TOF-MS

Concentration level

<10 µg/kg

Not spiked pesticides in test item

Blank Pepper

EUPT-SM06 Sample

Present in the blank material

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

2 Pesticides in the blank:

DIFENOCONAZOLE

TRIADIMENOL

Concentrations below 10 µg/kg

Pesticides in the Blank material

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Pesticides repoted by 3 or more laboratories but not

detected by the organizer:

• Diuron

• Formetanate

• Prometon

• Terbumeton

Other reported pesticides

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Diuron

LC-TOF -MS

Diuron

Fluometuron (spiked)

Other reported pesticides

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

XIC Secbumeton 226.1662± 20 ppm spiked at 50 µg/kg

MS Spectra SM06

XIC Secbumeton 226.1662± 20 ppm. SM06 sample

C10H19N5OC10H19N5OC10H19N5O

Spiked

Other reported pesticides

50 ppb Analytical Standard

EUPT-SM06 Sample

LC-TOF -MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Formetanate

Other reported pesticides

10 ppb Analytical Standard

EUPT-SM06 Sample

LC-Orbitrap-MS

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Analytical Techniques

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

LA

B.

CO

DE

Lab001

Lab002

Lab003

Lab004*

Lab006*

Lab007*

Lab008

Lab009

Lab010*

Lab011

Lab012

Lab013

Lab014

Lab015

Lab016*

Lab017

Lab018

Lab019*

Lab020

Lab021

Lab022

Lab023

Lab024*

Lab025*

Lab026

Lab027

Lab028*

Lab029

Lab030

Lab031

Lab032

Lab033*

Lab034

Lab035

Lab036

Lab037

Lab038

Lab039

Lab040

Lab041*

Lab042

Lab043

Lab044*

Lab045

Lab046*

Lab047

Lab048

Lab049*

Lab050

Lab051*

Lab052

Lab053

Lab054

Lab055

Lab056

Lab057*

Lab058

Lab059

Lab060

Lab061

Lab062

Lab063

Lab064

Lab065

Lab066

Lab067

Lab068

To

tal

Dete

ctio

ns

18 6 19171820191817351229142121 5 16 5 1310 5 6 211520191520161618 9 9 201832221616171912251020161815171615201218122119 9 19 3 13 3 15151315 9

GC

Dete

ctio

ns

12 0 4 9 16 3 8 4 7 6 7 18 0 1612 5 1 3 12 0 5 6 8 6 4 7 11 7 11 8 5 5 3 3 8 14 4 5 2 2 6 5 19 7 1 12 6 4 3 11 8 5 4 1 12 9 14 4 6 2 13 0 1211 3 10 4

LC

Dete

ctio

ns

6 6 15 8 2 1711141029 5 1114 5 9 0 15 2 1 10 0 0 13 9 1612 4 13 5 8 13 4 6 1710181811141513 7 6 3 19 4 121114 5 7 15 8 17 0 12 5 5 13 1 0 3 3 4 10 5 5

To

tal

Fu

ll S

can

0 0 0 7 0 18 0 15 0 20 5 0 1420 0 5 0 0 1 0 5 6 14 0 16 0 0 7 11 8 0 1 0 0 0 32 0 2 1117 0 0 19 0 14 3 18 0 3 2 152016 1 12 5 19 0 6 0 13 0 1511 0 0 4

GC

Fu

ll S

can

0 0 0 0 0 2 0 2 0 4 4 0 0 16 0 5 0 0 0 0 5 6 8 0 0 0 0 7 11 8 0 1 0 0 0 14 0 2 0 2 0 0 19 0 0 3 6 0 3 2 8 5 4 1 12 4 14 0 6 0 13 0 1211 0 0 4

LC

Fu

ll S

can

0 0 0 7 0 16 0 13 0 16 1 0 14 4 0 0 0 0 1 0 0 0 6 0 16 0 0 0 0 0 0 0 0 0 0 18 0 0 1115 0 0 0 0 14 0 12 0 0 0 7 1512 0 0 1 5 0 0 0 0 0 3 0 0 0 0

Analytical Techniques

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

LA

B.

CO

DE

Lab001

Lab002

Lab003

Lab004*

Lab006*

Lab007*

Lab008

Lab009

Lab010*

Lab011

Lab012

Lab013

Lab014

Lab015

Lab016*

Lab017

Lab018

Lab019*

Lab020

Lab021

Lab022

Lab023

Lab024*

Lab025*

Lab026

Lab027

Lab028*

Lab029

Lab030

Lab031

Lab032

Lab033*

Lab034

Lab035

Lab036

Lab037

Lab038

Lab039

Lab040

Lab041*

Lab042

Lab043

Lab044*

Lab045

Lab046*

Lab047

Lab048

Lab049*

Lab050

Lab051*

Lab052

Lab053

Lab054

Lab055

Lab056

Lab057*

Lab058

Lab059

Lab060

Lab061

Lab062

Lab063

Lab064

Lab065

Lab066

Lab067

Lab068

To

tal

Dete

ctio

ns

18 6 19171820191817351229142121 5 16 5 1310 5 6 211520191520161618 9 9 201832221616171912251020161815171615201218122119 9 19 3 13 3 15151315 9

GC

Dete

ctio

ns

12 0 4 9 16 3 8 4 7 6 7 18 0 1612 5 1 3 12 0 5 6 8 6 4 7 11 7 11 8 5 5 3 3 8 14 4 5 2 2 6 5 19 7 1 12 6 4 3 11 8 5 4 1 12 9 14 4 6 2 13 0 1211 3 10 4

LC

Dete

ctio

ns

6 6 15 8 2 1711141029 5 1114 5 9 0 15 2 1 10 0 0 13 9 1612 4 13 5 8 13 4 6 1710181811141513 7 6 3 19 4 121114 5 7 15 8 17 0 12 5 5 13 1 0 3 3 4 10 5 5

To

tal

Fu

ll S

can

0 0 0 7 0 18 0 15 0 20 5 0 1420 0 5 0 0 1 0 5 6 14 0 16 0 0 7 11 8 0 1 0 0 0 32 0 2 1117 0 0 19 0 14 3 18 0 3 2 152016 1 12 5 19 0 6 0 13 0 1511 0 0 4

GC

Fu

ll S

can

0 0 0 0 0 2 0 2 0 4 4 0 0 16 0 5 0 0 0 0 5 6 8 0 0 0 0 7 11 8 0 1 0 0 0 14 0 2 0 2 0 0 19 0 0 3 6 0 3 2 8 5 4 1 12 4 14 0 6 0 13 0 1211 0 0 4

LC

Fu

ll S

can

0 0 0 7 0 16 0 13 0 16 1 0 14 4 0 0 0 0 1 0 0 0 6 0 16 0 0 0 0 0 0 0 0 0 0 18 0 0 1115 0 0 0 0 14 0 12 0 0 0 7 1512 0 0 1 5 0 0 0 0 0 3 0 0 0 0

Total Detections: 1062 GC Detections: 459 LC Detections: 603

Total Full Scan: 427 GC Full Scan: 224 LC Full Scan: 203

(40% of the Total) (49% of the FS detections) (34% of the FS detections)

Total Detections: 1001 GC Detections: 313 LC Detections: 688

Total Full Scan: 318 GC Full Scan: 157 LC Full Scan: 161

(32% of the Total) (50% of the FS detections) (23% of the FS detections)

Analytical Techniques

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Full

Scan

Full

Scan

Full

Scan

Full

Scan

Analytical Techniques

European Union Proficiency Test in Fruits and Vegetables - Screening Methods 06

Thank you for

your attention