Rapport 17
−
2005
The Swedish Monitoring
of Pesticide Residues in Food
of Plant Origin: 2004
EC and National Report
Produktion:
Livsmedelsverket, Box 622
SE-751 26 Uppsala, Sweden
Teknisk redaktör:
Merethe Andersen
Tryck:
Livsmedelsverkets repro
Uppsala 2005-06-28
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av projektrapporter, metodprövningar, utredningar m m.
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Rapporterna utges i varierande upplagor och
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Livsmedelsverkets kundtjänst (tel 018-17 55 06) till
själv-kostnadspris (kopieringskostnad + expeditionsavgift).
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.
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
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
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
4
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
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.
6
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.
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
8
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.
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.
10
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
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
12
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.
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
14
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
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
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
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
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).
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
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.
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
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
thpercentile 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
compis 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)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
=
∗
∗
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%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
