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Rapport 17

2005

The Swedish Monitoring

of Pesticide Residues in Food

of Plant Origin: 2004

EC and National Report

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Produktion:

Livsmedelsverket, Box 622

SE-751 26 Uppsala, Sweden

Teknisk redaktör:

Merethe Andersen

Tryck:

Livsmedelsverkets repro

Uppsala 2005-06-28

Livsmedelsverkets rapportserie är avsedd för publicering

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Rapporter som utgivits 2004

1. Utvärdering av Livsmedelsverkets Riksprojekt 2002

2003 av R Lindqvist och E Hay.

2. Interkalibrering av laboratorier. Mikrobiologi

Livsmedel, januari 2004 av C Normark.

3. Proficiency Testing

Food Chemistry, Nutritional Components, Round 33,

March-April 2004 by L Merino.

4. Examination of Residues in Live Animals Products

Results of the Control 2003

by I Nordlander.

5. Proficiency Testing

Food Chemistry, Trace Elements in Food, Round T

−9

by C Åstrand and L Jorhem.

6. Riksprojekt 2002. Salmonella i frukt och grönsaker.

7. Projektinriktad kontroll 2003

2004. Granskning av salmonellaförekomst i köttberedningar

införda till Sverige från annat EU-land av A Brådenmark.

8. Proficiency testing. Food microbiology

April 2004

by Å Rosengren and C Normark.

9. Proficiency Testing. Drinking water microbiology

2004:1, March

by T Šlapokas

and M Ljunge.

10. Rapportering om livsmedelstillsyn 2003

Kommunernas rapportering om livsmedelstillsyn

av D Rosling.

11. Rapportering av dricksvattentillsyn 2003

Kommunernas rapportering om

dricksvatten-tillsyn av D Rosling.

12. The Swedish Monitoring of Pesticide Residues in Food of Plant Origin: 2003,

EC and National Report by A Andersson, A Jansson and G A Eskhult.

13. Mat och hälsa i undervisningen

skolan och lärarutbildningen av M Rosén.

14. Riksprojekt 2003

Temperaturer i storhushåll och butik av M Lindblad och M Boysen.

15. Synen på tillsyn

utvärdering av tillsyn vid anläggningar med Livsmedelsverkets som

tillsynsmyndighet av M Ljung.

16. Dioxins and PCBs in fish oil

a survey of fish oils and fish liver oils sold on the Swedish

market in February 2003 by S Wallin, P O Darnerud, R Bjerselius, A Glynn, M Aune

and A Andersson.

17.

Proficiency Testing

Food Chemistry, Nutritional Components, Round 34,

September

October 2004 by L Merino.

18. Nationella mål och strategier för nutrition 1999

2004

utvärdering av P Hagling

och M Ljung.

19. Du blir var du äter

studie om hur den socioekonomiska vardagsmiljön påverkar barns

förhållningssätt till mat av M Jansson.

20. Proficiency Testing

Food Chemistry, Vitamins in Foods, Round V-2 by H S Strandler

and A Staffas.

21. Validitet av enkätfrågor om kost och fysisk aktivitet bland vuxna

underlag till urval av

frågor i befolkningsinriktade enkäter av H Sepp, U Ekelund och W Becker.

22. Risk profile. Virus in food and drinking water in Sweden

Norovirus and Hepatitis A virus

by F Lund and R Lindqvist.

23. Interkalibrering av laboratorier. Mikrobiologi

Dricksvatten 2004:2, september

av T Šlapokas, C Gunnarsson och A Gidlund.

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Rapporter som utgivits 2005

ISSN 1104-7089

1. Verksamhetsplan 2005.

2. Collaborative study of method for detection of Escherichia coli O157 in food

NMKL no 164,

1999, by C Normark.

3. Proficiency Testing

Food Chemistry, Trace Elements in Food, Round T

−10

by C Åstrand and L Jorhem.

4. Utvärdering av första etappen av projektet God livsmedelskvalitet i Västernorrland

av H Nordenfors och U Fäger.

5. Lunchmat i Uppsala 2001

Undersökning av matens energi- och fettinnehåll av H Karlén Nilsson,

M Arnemo och W Becker.

6. Projektinriktad kontroll 2004. Ursprung och identitet av kött infört från annat EU-land

av U Evans Cederlund.

7. Interkalibrering av laboratorier. Mikrobiologi

Livsmedel, januari 2005 av C Normark

och C Gunnarsson.

8. Proficiency Testing

Food Chemistry, Nutritional Components in Food, Round N-35, by L Merino.

9. Normerande inspektioner av storhushåll 2002

2003. Resultat från normerande inspektioner av

stor-hushåll i samband med kommuninspektion av U Lantz och D Rosling.

10. A Risk Assessment of Uranium in Drinking Water by K Svensson, P O Darnerud and S Skerfving.

11. The Component Aspect Identifier

A Tool for Handling Food Component Information in a Food

Database Management System by I Unwin and W Becker.

12. Rapportering om livsmedelstillsyn 2004

Tillsynsmyndigheternas rapportering om livsmedelstillsyn

av D Rosling.

13. Interkalibrering av laboratorier. Mikrobiologi

Dricksvatten 2005:1, mars av T Šlapokas

och C Gunnarsson.

14. Interkalibrering av laboratorier. Mikrobiologi

Livsmedel, april 2005 av C Normark, K Mykkänen

och C Gunnarsson.

15. Campy-SET, Campylobacter: Smittspårning, epidemiologi och typning.

16. Examination of Residues in Live Animals Products

Results of the Control 2004 by I Nordlander.

17. The Swedish Monitoring of Pesticide Residues in Food of Plant Origin: 2004, EC and National

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The Swedish Monitoring

of Pesticide Residues

in Food of Plant Origin: 2004

Report concerning Directives 90/642/EEC, 86/362/EEC and

Commission Recommendation 2004/74/EC

By Arne Andersson and Anders Jansson

Further information

Information about the Swedish monitoring of pesticide residues in food

of plant origin is available from:

Arne Andersson

National Food Administration

Box 622, SE-751 26 Uppsala, Sweden

Fax: +46 18 17 53 53

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

3

CONTENTS

Summary

5

Introduction

6

Monitoring programme

7

Sampling procedures

8

Analytical procedures

9

Reporting levels

11

Maximum Residue Limits

11

Results and discussion

11

Dietary Exposure Assessment: Short-term intake

20

References

26

Appendix 1

Analytical method codes and their sources

28

Appendix 2

Pesticides, isomers and breakdown products sought and detected

31

Appendix 3

Number of surveillance samples grouped by methods used

35

Appendix 4

Number of surveillance samples analysed and residues found in per cent of

MRLs

36

Appendix 5

Number of enforcement samples analysed and residues found in per cent of

MRLs

46

Tables according to EU reporting format:

Table A1- Part I

Summary of numbers of samples analysed, sample origins and results,

surveillance sampling, national and co-ordinated programme

48

Table A1-Part II Summary of numbers of samples analysed, sample origins and results,

enforcement sampling, national and co-ordinated programme

49

Table A2-Part I

Fruits & vegetables: Summary table of pesticides sought and found,

surveillance sampling, national and co-ordinated programme

50

Table A2-Part II Cereals: Summary table of pesticides sought and found, surveillance

sampling, national and co-ordinated programme

55

Table B

Notifications of the co-ordinated programme (specific exercise) to the

European Commission

57

Table C

Notifications of the results of Check sampling (Surveillance sampling) of

the National programme to the European Commission. The results include

the samples in the co-ordinated programme

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

CONTENTS

Continue

Table D1

Details of residues exceeding EC-MRLs, surveillance sampling of fruits,

vegetables and cereals, national and co-ordinated programme

173

Table D2

Details of residues exceeding non-harmonised MRLs including national

MRLs, surveillance sampling of fruits, vegetables and cereals, national and

co-ordinated programme

175

Table D3

Details of residues exceeding EC-MRLs, follow-up enforcement sampling of

fruits, vegetables and cereals, national and co-ordinated programme

176

Table D4

Details of residues exceeding non-harmonised MRLs, including national

MRLs, follow-up enforcement sampling of fruits, vegetables and cereals,

national and co-ordinated programme

177

Table E

Details of samples with multiple residues (>2) in single samples, surveillance

and follow-up enforcement sampling of fruits, vegetables and cereals,

national and co-ordinated programme

178

Table F

Details of the homogeneity exercise

197

Table G

Laboratories: Information about laboratories involved in the monitoring

exercise

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

5

The Swedish Monitoring of Pesticide

Residues in Food of Plant Origin: 2004

EC and National Report

Summary

In 2004, a total of 2 280 surveillance samples of fresh, frozen or processed fruits and

vegetables, cereal grains and cereal products were analysed for residues of 239

pesti-cides (290 analytes). National or EU harmonised Maximum Residue Limits were

exceeded by 80 samples (3.5 %).

The violation rate has decreased compared with 2003 and amounted to 6.7 % in

fresh or frozen fruits and vegetables from third countries and 4.0 % in the samples

from EU countries except Sweden. None of the samples of domestic grown fruits and

vegetables contained residues above the MRLs.

Residues were found in two out of 45 samples from organic production. In

general, samples from domestic Integrated Production (IP) contained less residues

compared with samples from conventional production. The plant growth regulator

chlormequat was found in 3 out of 62 samples of domestic conventional grown

wheat. Although the levels were very low, chlormequat is not authorised for use in

wheat.

Apples, tomatoes, lettuce, strawberries, leek, orange juice, head cabbage, rye and

oats, in all 513 samples,

were analysed in the 2004 EU co-ordinated programme. Eleven of

these samples exceeded any of the EC-MRLs for the pesticides concerned.

In eleven commodities (17 samples) pesticide residues were found at levels

more than 10 times the MRLs. The highest violation rate, 37 times the MRL, was

found in strawberries from Egypt containing methomyl.

No residues were found in the 92 samples of foods for infants and young

children.

A total of 232 samples of cereal grains were analysed. Most of the samples

(80 %) contained no residues and only one sample of rice exceeded any MRLs.

In the enforcement sampling of fruits and vegetables 75 samples were collected

and 14 lots (35.8 tons) were prohibited from being sold.

The homogeneity factor, calculated as the highest value found in an individual

unit divided by the mean residue of individual units in a single sample, was

determined for

Chinese broccoli and potatoes.

The stability after wok cooking was investigated for certain pesticides found in

Chinese broccoli.

The short-term intake was estimated for the acute toxic pesticides based on the

highest residue found in a surveillance (composite) sample. The ARfDs were

exceeded for toddlers in eight cases.

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Introduction

The Swedish National Food Administration (NFA) checks foods of plant origin for

pesticide residues. Annual reports have been published in English since 1986. The

present report is our sixth combined European Commission (EC) and national report.

It is aimed for the Commission, the Member States in the European Union (EU) and

all other interested parties. The report contains general information about the

monitoring programme, sampling procedures and analytical methods as well as

detailed information about residues found using a format requested by the European

Commission (Table A–G). Certain results are also presented in percent of the MRL

according to our general format for reporting residues found (Appendices 4–5). An

assessment of the short-term intake, based on the 2004 monitoring data, has also

been carried out.

This report is available on NFA’s web site (www.slv.se) together with a separate

comprehensive summary report in Swedish. Since 2001 quarterly and from 2004

tertiary summary reports from the pesticide residues monitoring are also available in

Swedish on NFA’s web site.

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

7

Monitoring programme

The target number of samples to be collected of each food takes into account the

food's consumption rate, but fewer samples are taken of commodities causing few

exceedances of the MRLs. The number is also based on the importance of the

foodstuff in the diets of infants and young children and if the food is consumed with

or without the peel. In some cases, the number of samples of a specific food or a food

from a particular country was increased based on residues found in prior samples.

By analysis of 100 samples it can with 95 % confidence be predicted that the actual

percentage of exceedances is less than 3 % provided that no exceedances was discerned.

About 80 different commodities

were included in the sampling plan for year

2004 (Table 1).

Table 1. Number of samples and commodities to be collected according to the

monitoring programme 2004 and the outcome of the sampling.

COMMODITY

COMMODITY

planned

outcome

planned

outcome

Fruits (fresh or frozen)

970

970

Apples

195

198

Peppers

55

60

Bananas

80

80

Potatoes

95

96

Mandarins and similar

70

71

Others

320

299

Oranges

70

72

Peaches and nectarines

60

59

Cereal grains

250

232

Pears

130

130

Rice

50

56

Strawberries

50

55

Wheat

150

120

Table grapes

110

112

Others

50

56

Others

205

193

Processed or dried foods

285

288

Vegetables (fresh or frozen)

795

790

Baby foods

90

92

Carrots

60

61

Cereal products

45

44

Cucumbers

70

71

Juice, fruit drinks

40

41

Lettuce

65

71

Potatoe products

50

46

Melons

50

51

Others

60

65

Tomatoes

80

81

Total:

2 300

2 280

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Sampling procedures

Surveillance monitoring

Samples collected in accordance with the monitoring programme are defined as

surveillance samples, i.e. there are no suspicions about excessive amounts of pesticide

residues in the lots prior to sampling.

Enforcement sampling

When a surveillance sample contained a pesticide residue above the national or EC

maximum residue limit (1-3), the NFA prescribed a condition for the offering for

sale or other handling of the food or lot to which the food belonged. As a follow-up,

next lots of the commodity from the grower/exporter were detained and enforcement

samples were collected. The condition was cancelled either when a certain number

of lots contained pesticide residues below the MRLs, or when other information

showed that the residue problem did not exist any longer. Surveillance sampling was

then once more resumed.

Sample collection

Fresh fruit and vegetables were sampled at wholesalers' warehouses in the first trade

channel. The sampling was done according to the new EC sampling method

described in Commission Directive 2002/63/EC (4). The sample was sealed and

labelled with a unique sample identity.

Most of the samples of processed or frozen fruit and vegetables, juices, fruit

drinks, rice, cereal products and vegetable oils were collected in retail shops or

department stores.

Samples of domestic produced cereal grains were collected at the milling plants.

The “imported” cereal grains were sampled at the port where the shipment was

dis-charged. Usually, one bulk sample of about 3–5 kg was collected by stream sampling

technique.

Plant inspectors from the National Board of Agriculture collected most of the

samples,

but inspectors from the Municipal Environmental and Health Protection

Committees were to some extent also involved.

Quality assurance measures

Trained inspectors belonging to the National Board of Agriculture collected the

samples according to written instructions from the National Food Administration.

The bags with the samples were sealed and a photo was taken of the box that had

been sampled.

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

9

Analytical procedures

Methods and pesticide coverage

In all, by using both multi-residue methods and single residue methods, it was

pos-sible to determine 239 pesticides corresponding to 290 analytes (Appendices 2–3).

This is an increase with one pesticide compared with 2003 (5). By using LC-MS/MS

it has been possible to lower the limit of quantification (LOQ) to 0.01 mg/kg for a

large number of pesticides. The analytical method codes and their sources are listed

in Appendix 1.

A total of about 376 000 residues (pesticide/commodity combinations) were

sought (Table A2-Part I and II).

Fruit and vegetables

Practically all samples

of fruit and vegetables were analysed by the multi-residue

method (MRM) code 001. By this method, the samples were extracted with ethyl

acetate, cleaned up on an S-X3 gel permeation column and determined by capillary

gas chromatography. A total of 184 pesticides (213 analytes) were covered by using

this method.

Depending on commodity/country combination, the unclean extract was

determined by LC-MS/MS (method code 111). For acidic commodities sodium

hydroxide was added in the extraction step to enable quantitative determination

of 3,5-dichloroaniline, the benomyl group, thiabendazole and imazalil (method

code 002 and 112).

In addition to three MRMs also ten single residue methods were used, and in all

233 pesticides (282 analytes) were sought in fruits and vegetables. Of these

pesticides 97 were actually found. Figure 1 shows number of samples analysed and

pesticides sought and detected during the last six years.

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Figure 1. Number of pesticides (active substances) sought and detected, and number

of samples of fruit and vegetables analysed, surveillance sampling 1999-2004.

Vegetable oils

The samples were extracted using hexane and acetonitrile. After clean-up on an

S-X3 gel permeation column the residues were determined by GC equipped with

ECD, FPD or N/P-detector. A total of 32 pesticides (37 analytes) were covered

by the method used (code 018).

Cereal grains and cereal products

All samples of cereal grains and cereal products were analysed using MRM code

901. This method is similar to the multi-residue method (code 001) used for analysis

of fruit and vegetables. Single residue methods were used for analyses of

chlorme-quat, mepichlorme-quat, inorganic bromide, hydrogen phosphide, glyfosate and AMPA. In

all, 43 pesticides (52 analytes) were included in the control of cereals.

Quality control

Among other procedures, the quality control included daily checks of the

instru-ments' sensitivity by injection of test solutions. GC-determinations were in most

cases carried out using standards in matrix extracts.

The EC guidelines ”Quality Control Procedures for Pesticide Residue Analysis”

(6) have been implemented as far as possible (Table G). The laboratory has

parti-cipated in 16 proficiency tests. These were organised by the European Commission

and FAPAS (Table G).

0

1000

2000

3000

4000

5000

1999

2000

2001

2002

2003

2004

N

o

. o

f

sa

m

p

le

s

0

50

100

150

200

250

N

o

. o

f

p

e

st

ic

id

e

s

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

11

Laboratory used and accreditation

The analyses were carried out on a contract basis at AnalyCen Nordic AB,

Lidköping. This laboratory is accredited by the Swedish accreditation authority

SWEDAC for all analytical methods used for the NFA’s official control of pesticide

residues in food of plant origin.

Reporting levels

The majority of the pesticide residues were measured and reported from the limit

of quantitation (determination), generally in the range of 0.01–0.1 mg/kg. Reporting

levels for each of the pesticides are given in Table A2-Part I-II. For certain pesticides

the EC-MRLs set at the LODs (Limit of Determination) were not achievable in our

routine monitoring.

Maximum Residue Limits

The National Food Administration's Regulations on Pesticide Residues in Food, sets

MRLs for about 200 individual substances or group of substances (according to the

residue definition in the regulation). Fresh, frozen and dried fruits and vegetables,

cereal grains, some cereal products as well as baby foods are covered by the

regulations (1-3).

The MRLs, national and EC-MRLs, apply equally to domestic, EU and third

country commodities, whether or not the pesticide is authorised in Sweden. When

regulations concerning a certain pesticide or a certain group of food products are not

given in the regulations, the NFA can decide the maximum level to be applied in

each individual case.

Results and discussion

Surveillance monitoring

In 2004, a total of 2 280 surveillance samples of fresh, frozen or processed fruit and

vegetables, cereal grains and cereal products were analysed for pesticide residues.

Table 2 shows the number of surveillance samples analysed by country of origin.

About 70 % of the samples originated from foods from 61 foreign countries. Most

of the samples with unknown origin came from processed products. In 2003, the

number of samples amounted to 2 352 originating from 61 countries (5).

National and EU harmonised Maximum Residue Limits (EC-MRLs) were

exceeded by 80 (3.5 %) of the 2 280 samples analysed.

Out of 1 760 samples of fresh or frozen fruits and vegetables 806 samples

(45.8 %) contained residues at or below national and EC-MRLs and 77 samples

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

(4.4 %) exceeded these limits. One of the 232 samples of cereal grains exceeded the

MRLs and 79.7 % contained no residues at all (Tables A1-Part I and D1–2).

In all, 5 844 analyses were carried out using 16 analytical methods. The number of

surveillance samples analysed by the different analytical methods and arranged by

food-groups is shown in Appendix 3. Out of the 239 pesticides (active substances)

sought in all foodstuffs 100 were actually detected. The total numbers of findings of

each pesticide in fruits, vegetables and cereal grains are shown in Table A2-Part I-II.

Table 2. Total number of surveillance samples by country analysed in 2004.

Country

No. of

samples

Country

No. of

samples

Country

No. of

samples

Argentina

64

Honduras

2

Panama

8

Australia

2

Hungary

17

Peru

15

Belgium

40

India

18

Poland

24

Brazil

107 Iran

7

Portugal

1

Canada

1

Israel

32

Republic of Korea 1

Chile

32

Italy

195

Romania

2

China

30

Ivory Coast

4

Senegal

1

Colombia

42

Jordan

1

South

Africa

87

Costa Rica

45

Kazakhstan

2

Spain

185

Cyprus

26

Kenya

8

Sweden

618

Czech Republic

2

Latvia

1

Taiwan

1

Denmark

8 Lebanon

5

Thailand

61

Dominica

Rep. 2 Lithuania 1

Turkey

83

Ecuador

11

Makedonia

1

Ukraine

2

Egypt

19

Mauritius

2

United

Kingdom 19

Finland

3

Morocco

44

United

States

91

France

36

Namibia

2

Unknown

country 56

German Fed.Rep.

39

Netherlands

113

Uruguay

9

Ghana

1

New Zealand

27

Venezuela

1

Greece

13

Norway

3

Vietnam

1

Guatemala

1

Pakistan

2

Zimbabwe

3

Totalt

2280

The most commonly found pesticides in fresh or frozen fruit, vegetables and cereal

grains are presented in Table 3. The fungicides imazalil and thiabendazole were

among those most often found in fruits, while imidacloprid and carbendazim were

most often found in the vegetable samples. Out of the eight different pesticides

detected in cereal grain, the growth regulators chlormequat and mepiquat were most

often found.

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

13

Table 3. Pesticides most commonly found in fruits, vegetables and cereal grains,

surveillance sampling in 2004.

Comparison of residues from different types of production system

The total number of samples analysed from organic, integrated and conventional

production was 45, 175 and 2 060, respectively (Table 4). Two of the samples from

organic growing contained residues. Seventeen samples from Integrated Production

(IP) contained residues but none exceeded the MRLs. All the 80 exceedances came

from samples of “imported” food from conventional production. In general, fewer

residues were found in samples from Integrated Production compared with samples

from the conventional production.

The plant growth regulator chlormequat was found in 3 out of 62 domestic

samples of wheat. The levels were very low, however, the use of chlormequat in

wheat is not authorised in Sweden.

Table 4.

Comparison of residues found grouped by type of farming, surveillance

sampling in 2004.

Type of

production

Origin

Total no. of

samples

No of samples containing

No residues

Residues<

MRL

Residues >

MRL

Organic

Domestic

19

18

1

0

Import

26

25

1

0

IP

Domestic

171

156

15

0

Import

4

2

2

0

Conventional

Domestic

428

356

72

0

Import

1 632

75

796

80

Fruits

(970 samples)

Vegetables

(790 samples)

Cereal grains

(232 samples)

No. of

No. of

No. of

Pesticide findings

Pesticide findings

Pesticide findings

Imazalil

157

Imidacloprid

51

Chlormequat

32

Thiabendazole

128

Carbendazim

41

Mepiquat

25

Carbendazim

84

Dithiocarbamates

33

Hydrogen

phosphide 5

Dithiocarbamates

71

Endosulfan

30

Glyphosate

4

Carbaryl

62

Oxamyl

29

Pirimiphos-methyl

4

Chlorpyrifos

60

Chlorothalonil

28

Chlopyrifos-methyl 3

Orthophenylphenol 55

Procymidone

26

Bromide

(inorganic) 1

Captan

50

Iprodione

20

Deltamethrin

1

Iprodion

50

Methomyl

20

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Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Fruits and vegetables - fresh or frozen

A total of 1 760 samples of fresh or frozen fruit and vegetables including potatoes

were analysed for residues of 233 pesticides (282 analytes). About 50 % of the

samples contained no residues. National or EC-MRLs were exceeded in 77 (4.4 %)

of the samples (Figure 2). The number of exceedances in 2003 was 113 (6.3 %).

Figure 2. Summary of results for fruit and vegetables, surveillance sampling 2004.

Sweden 369 samples 85,6% 14,4% Total 1760 samples 49,8% 45,8% 4,4% EU except Sweden 599 samples 44,9% 51,1% 4,0% Third countries 792 samples 36,9% 56,4% 6,7%

Residues above national or EC-MRL:s Residues at or below national or EC-MRL:s Without residues

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National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

15

In general, the “imported” commodities contained considerably more often residues

than the domestic. Most samples (86 %) of domestic grown fruit and vegetables

con-tained no residues. The corresponding figures for EU-countries (except Sweden) and

third countries were 45 % and 37 %, respectively. None of the domestic grown fruits

and vegetables exceeded national or EC-MRLs compared with 4.0 % of the samples

from EU countries (except Sweden) and 6.7 % from third countries.

Number of surveillance samples of each fruit and vegetable and the pesticide

residues found (in per cent of the MRL) are presented in Appendix 4.

Commodities containing pesticide residues greater than 10 times the MRL are

shown in Table 5. The ratio between the highest level found in the surveillance

sampling and the MRL is given. Residues of methomyl in a sample of strawberries

from Egypt amounted to 37 times the MRL. However, the high figures are partly due

to cases where the MRLs are set at the limit of determination.

Table 5. Commodities containing pesticide residues greater than 10 times the MRL,

surveillance sampling in 2004.

Table grapes

A total of 112 samples of table grapes from 12 countries have been analysed. Five

samples (4.5 %) contained residues above EC or national MRLs. One sample of table

grapes originating from Spain contained 0.14 mg/kg of monocroophos. The

short-term

intake, calculated on this level, resulted in an exceedance of the acute reference

dose with 381 % for a child (Table 10).

Country

Max.

MRL

Ratio

of origin

residue

found

max.

residue/

MRL

mg/kg

mg/kg

Strawberries

Methomyl

Egypt

2

1,87

0,05

37

Papayas

Chlorothalonil

Brazil

4

0,36

0,01

36

Kumquats

Imazalil

Argentina

1

0,59

0,02

29

Litchis

Prochloraz

Israel

2

1,04

0,05

21

Kumquats

Dicofol

Morocco

1

0,34

0,02

17

Mandarins

Bromopropylate

Cyprus

1

0,84

0,05

17

Persimmons

Imazalil

South Africa

1

0,32

0,02

16

Spinach

Dithiocarbamates

Italy

1

0,80

0,05

16

Passion Fruits

Chlorothalonil

Kenya

1

0,14

0,01

14

Kumquats

Carbendazim

Morocco

1

1,31

0,10

13

Litchis

Thiabendazole

Mauritius

1

0,63

0,05

13

Beans, with pods

Dimethoate

Thailand

1

0,23

0.02

11

Passion Fruits

Dithiocarbamates

Kenya

1

0,55

0,05

11

Parsley

Dimethoate

Italy

1

0,22

0,02

11

Kumquats

Thiabendazole

Argentina

1

0,53

0,05

11

Lemons

Bromopropylate

Cyprus

1

0,53

0,05

11

Papayas

Dithiocarbamates

Brazil

1

0,51

0,05

10

Commodity

Pesticide

No. of

samples

with

residues >10

(20)

16

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

The EU co-ordinated programme

The EU co-ordinated programme for 2004 consisted of nine commodities and 47

pesticides (7). The minimum number of samples per commodity to be analysed by

each of the member states was 12 to 93 depending on the population size in the MS.

In Sweden the EU co-ordinated programme is included in the national monitoring

programme. In all, 513 samples of apples, tomatoes, lettuce, strawberries, leek,

orange juice, head cabbage, rye and oats were analysed (Table B). Residues above

the EC-MRLs for the pesticides listed in Table B were found in five out of the 198

samples of apples, one out of the 45 samples of lettuce, two out of the 55 samples of

strawberries, two out of the 30 samples of leek and in one out of the 30 samples of

head cabbage. None of the samples of tomatoes, orange juice, rye and oats contained

residues above the EC-MRLs (Figure 3).

The EU co-ordinated programme included also analysis of individual units

of apples, tomatoes, lettuce, leek and head cabbage for pesticides posing an acute

risk. The homogeneity factor has to be calculated based on the residues in the

individual units. No investigations were possible to carry out as none of the samples

taken contained residues for those combinations. However, the homogeneity factor

has been determined for chlorpropham in potatoes and eight pesticides in Chinese

broccoli. The

result is shown in Table 7.

Figure 3. Summary of results for the EU co-ordinated programme, only EC-MRLs

and pesticides included in Table B, surveillance sampling in 2004.

0%

20%

40%

60%

80%

100%

Ap

pl

es

He

ad

C

ab

bag

e

Le

eks

Le

ttu

ce

O

ats

O

ra

ng

e Ju

ice Ry

e

St

ra

be

rri

es

Tom

at

oes

Commodity

P

e

rc

e

n

ta

ge

of

num

be

r of

sam

p

le

s

No residues

Residues below MRLs

Residues above MRLs

(21)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

17

Table D1 gives detailed information about pesticide residues found and action taken

for those 78 surveillance samples of fruits, vegetables and cereal grains that exceeded

EU harmonised MRLs. In 21 of the samples, two or more pesticides exceeded the

EC-MRLs in the same sample. Three of those samples contained even three

pesticides above the limits.

A total of 23 samples in the follow-up enforcement sampling of fruits, vegetables

and cereals contained residues above the EC-MRLs (Table D3).

Out of 2 067 samples of fruit, vegetables and cereal grains (surveillance and

compliance) 492 contained residues of two or more pesticides in a single sample.

The highest number of pesticides found was eight and this was found in one sample

of Chinese broccoli from Thailand and one sample of pears from Italy. None of the

samples contained seven pesticides. Six pesticides were found in five samples.

Detailed information is given in Table E for all samples with two or more pesticide

residues in a single sample.

Violation rates of pesticide residues

The frequency of samples of fresh or frozen fruits and vegetables with pesticide

resi-dues above national or EC-MRLs is shown in Figure 4. The violation rate has

decreased and amounted to 6.7 % in fresh or frozen fruits and vegetables from third

countries and 4.0 % in the samples from EU countries except Sweden. None of the

samples of domestic grown fruits and vegetables contained residues above the

MRLs.

Figure 4. Violation rate of pesticide residues in samples of fresh or frozen fruits and

vegetables, national or EC-MRLs, surveillance sampling during 1995–2004.

0%

1%

2%

3%

4%

5%

6%

7 %

8%

9%

10%

11%

12%

95

96

97

98

99

00

01

02

03

04

E

x

ceed

a

n

ces

Sweden

EU (excl. Sweden)

Third countries

(22)

18

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Foods intended for infants and young children

In total, 92 samples of baby foods e.g. cereal

based product, juices, fruit drinks, canned fruits

and vegetables were analysed. No detectable

residues were found in any of the samples.

Photo: Harriet Böckman-Superti

Juices and fruit drinks (excluding “baby food”)

A total of 41 samples of juices and fruit drinks were analysed. Three out of six

samples of grape juice contained residues. The pesticides found were: carbaryl

(0.04 mg/kg), carbendazim (0.01 mg/kg) and pyrimethanil (0.08 mg/kg).

Fruits and vegetables – processed or dried (excluding “baby food”)

43 samples of dried fruits and canned or processed vegetables were analysed. Ten

out of the 16 samples of dried grapes contained pesticide residues. The highest

residue found was 0.31 mg/kg of carbendazim. The sprout inhibitor chlorpropham

was found in 8 out of 35 samples of fried potato products. Two samples exceeded the

national MRL and the highest residue was 2.7 mg/kg. Detailed information is given

in Table C.

Vegetable oils

Olive oil, 22 samples in all, were analysed for residues of 32 pesticides (method code

018). Endosulfan was detected in 14 of the samples and the highest residue found

was 0.07 mg/kg (Table C).

Cereal products

A total of 44 samples of pasta, were analysed. None of the samples contained

residues (Table C).

Cereal grains

A total of 232 samples of cereal grains, mainly wheat, rice and rye, were analysed.

Most of the samples (80 %) contained no residues at all (Figure 5). One sample of

rice contained 0.15 mg/kg of hydrogen phosphide, which is above the limit of 0.1

mg/kg.

The growth regulators chlormequat and mepiquat were most frequently found

(Table 3). Chlormequat was found in 3 out of 62 samples of domestic wheat. The use

of chlormequat in Sweden is authorised for rye but not for wheat (Table C).

(23)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

19

Figure 5. Summary of results for cereal grains, national or EC-MRLs, surveillance

sampling in 2004.

Enforcement

Enforcement samples were collected as a follow-up, when excessive amounts of

pesti-cide residues were found in surveillance samples. EC-MRLs were exceeded in 23 out

of 75 enforcement samples (Tables A1-Part II, Tables D3-4).

A total of 14 lots (35.8 tons) of foods were prohibited for sale in 2004 (Table 6),

compared with 23 lots (42.3 tons) in 2003 (5). These lots had either to be destroyed

or returned to the supplier. A re-export is accepted only when the competent author-

ity in the receiving country gives its approval. The number of samples analysed,

grouped by food commodity, country of origin and residues found, expressed in per

cent of the MRL, are shown in Appendix 5.

Table 6. Lots prohibited for sale in 2004

Food

Country

No. of lots

Weight, ton

Carambole Malaysia

1

0.02

Kumquats Argentina

1

0.04

Papayas Brazil

2

1.39

Parsley Italy

4 6.68

Passion fruits

Kenya

3

1.68

Pepper, white

Hungary

1

7.92

Spinach Italy

1

0.02

Table grapes

Turkey

2

18.0

Total

14

35.75

Sweden 153 samples 79,7% 20,3%

Total

232 samples

79,7% 19,8% 0,4% EU except Sweden 12 samples 75,0% 25,0% Third countries 67 samples 80,6% 17,9% 1,5%

Residues above national or EC-MRL:s Residues at or below national or EC-MRL:s Without residues

(24)

20

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Rapid Alert System

The Rapid Alert System for Foodstuffs (RASFF) was established by Council

Directive 92/59/ECC on General Product Safety. Products entailing a serious health

risk to the consumer are classified as Alert notifications. The notifying Member State

(MS) informs the Commission, which then notifies the other Member States.

Sweden has during 2004 sent three food-alarms concerning high pesticide

residues to the Commission. The notifications were for one consignment of table

grapes from Spain containing monocrotophos and two consignments of Chinese

broccoli from Thailand containing dicrototophos and methamidophos, chlorpyrifos

and dicrotophos, respectively.

Dietary Exposure Assessment

Homogeneity (variability) factor

The homogeneity (variability) factor is defined as the quotient between the maximum

and the mean residue of individual units in a sample. This factor was determined for

chlorpropham in potatoes and for eight different pesticides in Chinese broccoli. In

the calculations, units containing no residues were assigned a figure corresponding to

half of the limit of determination. The homogeneity factor varied from 1.6 to 4.9

(Table 7).

Table 7. Homogeneity factors for pesticides/commodities investigated in 2004.

Pesticide

Commodity

No. of

units

Homoge-neity

M ax

residue,

M ean

residue,

Sample

Reference

factor

mg/kg

mg/kg

Chlorothalonil Chinese

broccoli 10

3.7 1.3

0.34 20041005S401

Chlorpyrifos -“-

10 2.8 0.75 0.27 -“-

Cypermethrin -“-

10 2.6 7.6

2.9 -“-

Dicrotophos -“-

10 2.2 1.6 0.75

-“-

Iprodione -“-

10

2.7

0.20

0.07

-“-

Metalaxyl -“-

10

2.3

1.4

0.59

-“-

Metamidophos -“-

10

2.1 9.2

4.4

-“-

Chlorothalonil Chinese

broccoli 5

1)

4.9 0.37 0.08

20041007G201

Dicrotophos -“-

5

1)

2.9 10.4 3.6 -“-

M yclobutanil -“-

5

1)

2.8 0.1 0.04

-“-

Chlorpropham Potatoes

10

1.6

4.9

3.2 20040906H507

1)

Plastic bags containing 5-6 units of small broccoli, plant weight about 15

gram.

(25)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

21

Study of stability of pesticides after wok cooking

Two studies have been done to investigate the stability after wok cooking of

pesticides found in Chinese broccoli. The broccoli with the incurred residues was

divided in two equal portions, one part was analysed as raw (unprepared) and the

second part was analysed after frying in a hot wok for about two minutes according

to recipe. Two spoons of vegetable oils were added in the pan before frying. No

significant reduction of the residues was obtained for the organophosphorous

pesticides

chlorpyriphos, dicrotophos and methamidophos. These pesticides are

classified as acute toxic compounds (Table 8).

Table 8. Studies of the stability after wok cooking of some pesticides found in

Chinese broccoli.

Short-term Intake

The acute dietary intake or short-term exposure has to be considered for those

pesticides that are classified as acute toxic. This area is relatively new and

approaches how to estimate the acute intake has been put forward by WHO (8-11)

and UK (12). The aim of the WHO and EU is to evaluate pesticides and establish

acute reference doses (ARfD) for pesticides that possibly impose an acute health risk

(13-14).

The acute reference dose of a chemical is an estimate of the amount a

consumer can ingest during one meal or during one day without any health risk.

In this study the national estimated short-term intake (NESTI) has been

calculated for each pesticide found and for which EU, JMPR, JECFA or US-EPA

(15) have established a reference dose.

The type of foodstuffs of most concern when estimating the acute exposure are

those where the entire commodity (including peel) is consumed at one occasion, i.e.

nectarines, apples or table grapes.

Pesticide

Study

Raw broccoli

After cooking

1)

Remaining

residues

%

Chlorpyriphos

1

0.27

0.42

156

Dicrotophos

1

0.75

0.98

131

Dicrotophos

2

3.6

2.9

81

Metahmidophos

1

4.4

4.1

93

Chlorothalonil

1

0.34

0.08

24

Chlorothalonil

2

0.08

< 0.01

-Cypermetrin

1

2.9

1.8

62

Iprodione

1

0.07

0.09

129

Metalaxyl

1

0.59

0.8

136

Myklobutanil

2

0.04

0.03

75

1)

The residues are re-calculated taking into account the lost of water due to the wook cooking

mg/kg

(26)

22

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Calculation of the national estimated short-term intake

The national estimated short-term intake was calculated using the formulae shown in

Figure 6. These formulae (case 2) are used when the meal-sized portion, as a single

fruit or piece of vegetable (unit weight of the whole portion is > 25 g) might have a

higher concentration of residue than the composite sample due to variability of

residues in individual units. When the residue data reflect residue levels in the food

as consumed (case 1), no variability factor is considered (i.e. cereals, juices).

The consumption figures used when calculating the national estimated short-term

intake (NESTI) are based on the 97.5

th

percentile consumption of eaters only, which

reflects the largest portion consumed during one meal or during one day. In this

study consumption data from United Kingdom have been used (Table 9).

Monitoring data reflect residue levels found in the products on the market. The

observed residue (OR

comp

) is the highest residue found in a composite sample. In

order to refine the intake estimates, correction factors (when available) were applied

to foodstuffs that normally are peeled or prepared, e.g. boiled or fried (12). OR

comp

is multiplied with a variability (homogeneity) factor (V). For commodities with unit

weights between 25−250 g a default factor of 7 (10 for leafy vegetables) is used.

A factor of 5 is used for unit weights above 250 g. Known variability factors or

resi-dues in individual units should be used for more refined estimates.

Table 9. Consumption figures and unit sizes for foods used in the short-term intake

calculations (UK data).

Commodity

Large portion size

Unit size

Toddlers

Adults

(kg)

(kg)

(kg)

Chinese Broccoli

1)

0.015

0.045

0.015

Cucumbers

0.072

0.084

0.084

2)

Lettuce

0.025

0.093

0.558

Melons

0.303

0.513

0.322

Potatoes

3)

0.241

0.473

0.216

Table grapes

0.158

0.19

0.500

Zucchini

0.06

0.222

0.114

1)

Consumption data not availably. One unit for toddlers and three units for

adults used in the intake calculation

2)

A slice of one inch

3)

(27)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

23

Figure 6. The formulae used for calculating the national estimated

short-term

intake.

V

National estimated short-term intake

Case 2b:

Case 1:

The composite residue data reflect residue levels in the food as

consumed

The unit weight of the whole commodity (U) is larger

than the large portion (LP)

Case 2a: The unit weight of the whole commodity (U) is smaller

than the large portion (LP)

NESTI

U

ORcomp

LP

bw

Median unit weight of the edible portion (kg)

Highest observed residue in a composite sample of edible

portion incorporation processing factors if available

(mg/kg)

Variability factor; 1 to 10 depending on unit weight and

commodity

Highest large portion provided (97.5th percentile of

eaters) in kg of food per day

Body weight (kg)

=

=

=

=

=

=

=

bw

=

bw

ORcomp

LP

NESTI

=

)

(

bw

ORcomp

U

LP

V

ORcomp

U

NESTI

=

+

bw

V

ORcomp

LP

NESTI

=

(28)

24

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Results of the assessment of the national estimated short-term intake

Children, with low body weight relative to their consumption of fruits and

vege-tables, compose a risk group of approaching the acute reference dose when the

products contain high levels of acute toxic pesticides. In this study the estimated

short-term intake has been calculated for a large number of pesticides/commodity

combinations but the results are shown only when the intake for a child is above 50

% of the acute reference dose (Table 10 and Figure 7).

The estimated short-term intake for a child (body weight 14.5 kg) exceeded the

ARfD for aldicarb in potatoes, dicrotophos in Chinese broccoli, endosulfan in

melons, lambda-cyhalothrin in lettuce, monocrotophos in table grapes and oxamyl in

zucchini and cucumber (Figure 7).

The intake of dicrotophos from Chinese broccoli reached 18 times the acute

reference dose for a child and four times the ARfD for an adult (Table 10).

Figure 7. Estimated short-term intake for a child, surveillance sampling in 2004.

0%

50%

100%

150%

200%

C

hi

n

e

se

b

ro

cc

o

li

C

uc

u

m

b

er

L

e

tt

u

ce

M

e

lo

n

s

P

o

ta

to

e

s,

B

a

ke

d

T

a

b

le

g

ra

p

e

s

Z

u

cc

h

in

i

P

e

r c

e

nt

of

A

R

fD

Aldicarb

Deltamethrin

Dicrotophos

Endosulfan

Lambda-Cyhalothrin

Monocrotophos

Oxamyl

381% 1 763%

(29)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

25

Table 10. The estimated short-term intake of certain pesticides based on the highest

residue found in composite samples in 2004. Only intakes above 50 % of the ARfD

for a toddler are shown.

Pesticide Commodity ARfD mg/kg bw Highest residue Correction factor Homo-geneity factor (mg/kg) toddlers adults

Aldicarb Potatoes, Baked 0.003 0.035 1 7 122 25 Potatoes, Baked 0.003 0.034 1 7 118 24 Deltamethrin Table grapes 0.01 0.14 1 5 76 19 Dicrotophos Chinese broccoli 0.0017 4.14 1 7 1763 365 Endosulfan Melons 0.02 0.21 1 5 110 24

Melons 0.02 0.12 1 5 63 14

Lambda-Cyhalothrin Lettuce 0.0075 0.92 1 5 106 81 Monocrotophos Table grapes 0.002 0.14 1 5 381 95 Oxamyl Zucchini 0.009 0.42 1 7 135 53 Cucumber 0.009 0.28 1 7 108 28

Intake

(30)

26

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

References

1. The National Food Administration's regulations on pesticide residues in food,

SLVFS 2002:43, amendment 2003:27. National Food Administration,

Uppsala, Sweden.

2. The National Food Administration's regulations on pesticide residues in food,

SLVFS 2004:14, amendment 2004:24. National Food Administration,

Uppsala, Sweden.

3. Commission Directive 2003/13/EC amending Directive 96/5/EC on

processed cereal-based foods and baby foods for infants and young children.

4. Commission Directive 2002/63/EC of 11 July 2002 establishing Community

methods of sampling for the official control of pesticide residues in and on

products of plant and animal origin and repealing Directive 79/700/EEC. OJ

L187, 16.7.2002, 30-43.

5. Andersson A, Jansson A, Eskhult A G. The Swedish monitoring of pesticide

residues in food of plant origin: 2003. Rapport nr 12, 2004. National Food

Administration, Uppsala, Sweden.

6. Quality control procedures for pesticide residues analysis. Guidelines for

residues monitoring in the European Union, third edition, 2003. Document

no. SANCO/10476/2003.

7. Commission recommendation of 9 January 2004 concerning a co-ordinated

community monitoring programme for 2004 to ensure compliance with

maximum levels of pesticide residues in and on cereals and certain products

of plant origin. (2004/74/EC). OJ L16, 23.1.2004, 60-64.

8. Guidelines for predicting dietary intake of pesticide residues (revised).

GEMS/Food, WHO/FSF/FOS/97.7, World Health Organization, Geneva.

9. FAO/WHO. Pesticide Residues in food – 1999. Report of the joint meeting of the

FAO panel of experts on pesticide residues in food and the environment and the

WHO core assessment group on pesticide residues. Rome, Italy, 20-29 September

1999.

10. 10. FAO/WHO. Pesticide residues in food-2001. Report of the joint meeting

of the FAO panel of experts on pesticide residues in food and the

environment and the WHO core assessment group on pesticide residues.

Geneva, Switzerland, 17-26 September 2001.

11. FAO/WHO. Pesticide Residue in food – 2004. Report of the joint meeting of

the FAO panel of experts on pesticide residues in food and the environment

and the WHO core assessment group on pesticide residues. Rome, Italy,

20-29 September 2004.

12. New UK technical policy on the estimation of acute dietary intakes of

pesticides. PSD, York, UK, 13 January 1998.

(31)

National Food Administration, Sweden Livsmedelsverkets rapport nr 17/2005

27

13. Inventory of IPCS and other WHO pesticide evaluations and summary of

toxicological evaluations performed by the Joint Meeting on Pesticide

Residues (JMPR) through 2002. WHO/PCS/02.3. World Health

Organization, Geneva.

14. Legislation, the status of active substances under EU review (document 3010,

updated 04/11/2004).

15. US-EPA interim registration eligibility decision for dicrotophos. Case No

0145, April 3, 2002.

(32)

28

Livsmedelsverkets rapport nr 17/2005

National Food Administration, Sweden

Appendix 1. Analytical method codes and their sources

Code 001: GC-Multimethod

Andersson A, Pålsheden H. Multi-residue method for analysis of pesticides in fruit and

vegetables using ethyl acetate extraction, GPC clean-up and GC determination. In: Pesticide

analytical methods in Sweden, part 1. Uppsala, Sweden: National Food Administration,

Rapport 1998;17:9–41.

Code 002: GC-Multimethod (alkaline extraction)

Wåglund T, Elgerud C. A multi-residue procedure applied to the analysis of

3,5-dichloroaniline in some vegetables by use of gas chromatography. In: Pesticide analytical

methods in Sweden, part 1. Uppsala, Sweden: National Food Administration, Rapport

1998;17:58–62.

Ohlin B, Jansson C. Determination of benzimidazoles and some other pesticides in

agricultural crops with HPLC. In: Pesticide analytical methods in Sweden, part 1. Uppsala,

Sweden: National Food Administration, Rapport 1998;17:63–74.

Code 008: Dithiocarbamates

Pihlström T. Determination of dithiocarbamates in fruits and vegetables using GC/FPD. Not

published, National Food Administration, Uppsala, Sweden.

Harrington P. Analysis of dithiocarbamates by quantification of CS

2

using 2,2,4-trimethyl

pentane method. Central Science Laboratory, York, UK.

Keppel G E. Collaborative study of the determination of dithiocarbamate residues by a

modified carbon disulphide evolution method. J. Ass. Offic. Anal. Chem. 1971;54:528–532.

Winell B. Residues of dithiocarbamates in fruit, berries, vegetables and potatoes (in

Swedish). Vår Föda 1975;27:94–102.

Code 009: Diquat

Kirsten W J. The determination of diquat residues in potato tubers. Analyst 1966;91:732–

738.

Åkerblom M. Second derivative scanning in spectrophotometric determination of pesticide

residues. Fourth International Congress of Pesticide Chemistry (IUPAC), Zürich, 1978.

Ab-stract volume VI–701.

Code 010: Bromide, inorganic

Rocklin R D, Johnsson E L. Determination of cyanide, sulfide, iodide, and bromide by ion

chromatography with electrochemical detection. Analytical Chemistry 1983;55:4–7.

Modified by the Swedish University of Agricultural Sciences, Department of Environmental

Assessment, Uppsala, Sweden.

Lindgren B, Berglöf T, Ramberg Å, Stepinska A, and Åkerblom M. Liquid chromatographic

determination of bromide ion in cereals, fruit, vegetables, and blood with a Silver electrode

in an electrochemical detector system. JAOAC International 1995,78:841–845.

Figur

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