annex to monitoring of pesticide residues in products of...
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EUROPEAN COMMISSIONHEALTH & CONSUMER PROTECTION DIRECTORATE-GENERALDirectorate F - Food and Veterinary OfficeUnit 4 - Food of plant origin, plant health; processing and distributionIn cooperation with JRC IRMM, Food & Feed Unit and DG SANCO E1
Annex to SANCO/20/03 final
ANNEX
to
Monitoring of Pesticide Residues
in Products of Plant Origin
in the European Union, Norway, Iceland andLiechtenstein
2001 Report
March 2003
2
TABLE OF CONTENTS
1. NATIONAL AUTHORITIES AND CONTACT POINTS FOR PESTICIDE RESIDUEMONITORING ........................................................................................................... 3
2. COUNTRY COMMENTS.......................................................................................... 7
Belgium ....................................................................................................................... 7
Denmark .................................................................................................................... 11
germany..................................................................................................................... 16
Greece........................................................................................................................ 17
Spain 21
France ........................................................................................................................ 23
Ireland........................................................................................................................30
Italy 32
Luxembourg .............................................................................................................. 33
Netherlands................................................................................................................ 34
Austria ....................................................................................................................... 39
Portugal ..................................................................................................................... 43
Finland....................................................................................................................... 46
Sweden ...................................................................................................................... 47
United Kingdom........................................................................................................ 49
Norway...................................................................................................................... 51
Iceland ....................................................................................................................... 52
Liechtenstein ............................................................................................................. 53
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1. NATIONAL AUTHORITIES AND CONTACT POINTS FOR PESTICIDE RESIDUE MONITORING
Authority Contact person Contact point
Belgium:
Federal Agency for the Safety of the FoodChainWTC IIISimon Bolivarlaan 301000 Brussel
Alain Lacroix Tel.: +32 2 208.38.75Fax: +32 2 208.38.66e-mail :mailto:[email protected]
Denmark
The Danish Veterinary and FoodAdministrationInstitute of Food Safety and NutritionDiv. of Chemical ContaminantsMørkhøj Bygade 19DK2860 SøborgDenmark
A. Büchert Tel.: +45 33 95 64 61Fax: +45 33 95 60 01e-mail:[email protected]
Germany:
Bundesministerium für Verbraucherschutz,Ernährung und Landwirtschaft (BMVEL)Rochusstraße 1D-53123 Bonn
Dr. W. Töpner Tel.: +49 1888-529-4659Or: +49 1888-529-4661Fax: +49 1888-529-4943e-mail:[email protected]
Greece:
Ministry of Agriculture, Plant ProtectionDirectorate3-5 Hippokratous str.EL-10164, Athens, Greece
Pesticide Residue Laboratory1, S. Venizelou str.EL-14123, LycovrissiGreece
Director Mr.Ev. Arvanitakis
Dr. Ch. Lentza-Rizos
Tel.: +30 21 0361 5394Fax: +30 21 0361 7103
Tel.: + 30 21 02819019Fax: +30 21 02818735e-mail:[email protected]
Spain:Ministerio de Agricultura, Pesca yAlimentaciónDirección General de AgriculturaSubdirección General de Medios deProducciónAgricolasAvda. Ciudad de Barcelona, 118-12028007 Madrid
Mr. A. Yague Tel.: +34 91 3478273/75Fax: +34 91 3478316e-mail:[email protected]
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France:
Laboratoire Interregional de la Repressiondes Fraudes de Paris-Massy25 Avenue de la RepubliqueF-91744 Massy Cedex
and:DGCCRF-bureau C2 télédoc 05159, boulevard Vincent Auriol75703 Paris Cedex 13
Mr B. Declercq Tel.: +33 1 6953 8750Fax: +33 1 6953 8725Fax: +33 1 6953 8766e-mail: [email protected]@dgccrf.finances.gouv.fr
Tel: +33 1 4497 2379Fax: +33 1 4497 2486e-mail:mailto:[email protected]
Ireland:
The Pesticide Control ServiceDepartment of Agriculture, Food and RuralDevelopmentAbbotstownCastleknockDublin 15
Dr. D. O'Sullivan Tel.: +353 1 6072614Fax: +353 1 8204260e-mail:[email protected]
Italy:
Ministero della saluteD.G.S.P.V.A.N. Ufficio XIVPiazza Marconi 2500144 Roma
E. Cecere Tel.: +39 06 5994 6566Fax.: +39 36 5994 6627e-mail:[email protected]
Luxembourg:
Laboratoire National de SantéBP. 1102, L-1011 Luxembourg
Dr. CaroleDauberschmidt
Tel. :+352 491191-394Fax: +352 494 258e-mail:[email protected]
Netherlands:
Keuringsdienst van Waren(Inspectorate for Health Protection)Hoogte Kadijk 401NL-1018 BK Amsterdam
H. A. van der Schee Tel.: + 31205244600Fax: +31 20 5244700e-mail:[email protected]
Austria:
Bundesministerium für Soziale Sicherheitund Generationen, Abteilung VII/13Radetzkystraße 2A-1031 Wien
Dr. SylviaFrischenschlager
Dr. RolandGrossgut,Risikobewertung,ÖsterreichischeAgentur fürGesundheit undErährungssicherheitGmbH, Spargelfeld-strasse 191,
Tel.: +43/1/71100-4628Fax.: +43/1/71100-4681e-mail:[email protected]
Tel.: +43 1 73216 4150Fax.: +43 1 73216 2108e-mail: [email protected]
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A-1226 WienPortugal:
Direcςãao-Geral de Protecςão das CulturasQuinta do MarquesPT-2780 Oeiras
J. R. Santos Tel: +351 1 44 64000Or +351 1 44 64078
Fax: +351 1 44 20616e-mail:[email protected]
Finland :
Senior InspectorNational Food AgencyP.O. Box 28, FIN-00581 Helsinki
Arja Kaiponen Tel. +358 9 3931 529Fax: +358 9 3931 592e-mail:[email protected]
Sweden:
National Food AdministrationBox 622, S-751 26, Uppsala
A. Andersson Tel.: +46 18 17 56 41Fax: +46 18 17 53 53E-mail:[email protected]
United Kingdom:
Pesticides Safety DirectorateMallard House, Kings Pool3 Peaseholme GreenYork YO1 7PX
Jane Simcock Tel.: +44 1904 455 756Fax: +44 1904 455 733e-mail:
mailto:[email protected]
Norway:
Statens naeringsmiddeltilsynPostboks 8187 Dep0034 OsloNorway
M. Tomtum Tel.:+47 23 21 70 00Fax: +47 23 21 70 01e-mail:[email protected]
Iceland:
The Environment and Food Agency ofIcelandSuðurlandsbraut 24,108 ReykjavíkIceland
Sesselja MaríaSveinsdóttir
Tel.: +354 591 2000Fax: +354 591 2020e-mail:[email protected]
Liechtenstein:
Amt für Lebensmittelkontrolle undVeterinärwesenPostplatz 2Postfach 37FL- 9494 Schaan
Dr. P. Malin Tel.: +423 236 7311Fax: + 423 236 7310e-mail:[email protected]
European CommissionDG SANCO, FVO/F4Grange, DunsanyCounty MeathIreland
A. Bitterhof Tel.: +353 46 61 856Fax: +353 46 61 864e-mail:[email protected]
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European Commission
DG SANCO/ E1200, rue de la Loi (L86/1/8)B-1049 Bruxelles
B. Drukker Tel.: +32 2 2965779Fax: +32 2 2965963e-mail:[email protected]
European Commission
DG Joint Research CentreInstitute for Reference Materials andMeasurementsFood & Feed UnitTP 260I-21020 Ispra, Italy
Dr. Christoph vonHolst
Tel.: ++ 39 0332 785288Fax: ++39 0332 786267e-mail:[email protected]
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2. COUNTRY COMMENTS
BELGIUM
Pesticide Residue Monitoring in Fruit, Vegetables and Cereals in Belgium - 2001
SummaryThis report shows the results of pesticide residue monitoring on fresh and frozen fruits andvegetables, cereals, and processed foods on the Belgian market in 2001. These are domestic as wellas imported foods. Foodstuffs of animal origin are not included in this report.
The samples were taken by trained officials from the Food Inspection Service from the Ministry ofSocial Affairs, Public Health and the Environment (955 samples), or from the Service for PlantQuality and Plant Protection from the Ministry of Middle Class and Agriculture (74 samples). Bothservices are now part of the Federal Agency for the Safety of the Food Chain, under theresponsability of the Minister of Health. Sampling was done mostly according to directive79/700/EEC, at auctions, importers, wholesalers, processors and exceptionally in retail.
In selecting the commodities, the methods of analysis and the number of samples, several factorswere taken into account : the average consumption, the Belgian production, the rate of exceedancesand findings of previous years, the analytical and budgetary possibilities and all other usefulinformation. For less important commodities, a rolling programme is preferred. The differentgroups of fruits and vegetables were included as much as possible. The co-ordinated programme ofthe European Commission was of course included in the national programme. In total 11 differentsorts of fruit, 16 different sorts of vegetables (not including the different fresh herbs), potatoes,wheat, and processed foodstuffs (babyfood, concentrated tomato products, cereal products andpotato products) were analysed. It needs to be stressed that the programme is meant to enforce thelegislation and does not provide for a total random analysis, as more samples are taken of fooditems expected to contain pesticides or to exceed MRLs. For example, pears were still followedclosely, due to chlormequat problems in the past. Similarly, lettuce continues to be surveilledclosely, although less than in the past as the situation has improved, probably due to preharvestmonitoring, which is not included in this report.
A GC-multiresidue method was performed on most samples, except for almonds (in which onlybromide ion was sought), potatoes and potato products (in which only chlorpropham was sought),and for those samples for which only chlormequat was sought (concentrated tomato products andbabyfood with fruit). In cereal products, only chlormequat and mepiquat were sought. Chlormequatwas also sought in apples, pears and carrots. Chlorpropham was also sought in babyfood withvegetables. Dithiocarbamates analysis was carried out on apples, peaches, nectarines, table grapes,strawberries, tomatoes, sweet peppers, eggplant, cucumber, broccoli, head cabbage, lamb’s lettuce,lettuce, fresh herbs, spinach, peas, beans, celery and leek. It should be mentioned that it can not beexcluded that ‘dithiocarbamates’ found in head cabbage or broccoli up to a certain level can resultfrom natural levels of sulphur containing compounds, but this possibility has been taken intoaccount when setting the MRL, so that exceedances of this MRL cannot be explained by thepresence of natural compounds. Propamocarb analysis was performed on lettuce, lamb’s lettuce,fresh herbs, celery and babyfood with vegetables. GC-analysis after extraction for the more polarpesticide residues such as methamidophos, was carried out on the foodstuffs for the EU coordinatedprogramme (apples, strawberries, lettuce, tables grapes, and tomatoes) as well as on peaches andnectarines, sweet peppers, eggplant, and babyfood with vegetables. Benzimidazoles (carbendazimand thiabendazole) were sought in the foodstuffs of the EU coordinated programme and also ingrapefruit, pears, bananas, avocados, mangos, broccoli, head cabbage, celery, and babyfood with
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vegetables. Imazalil (typically used postharvest to prevent rotting of fruit) was analysed for ingrapefruit, apples, table grapes, strawberries, bananas, avocados, mangos and also in tomatoes andlettuce because of the coordinated EU programme. Bromide ion was sought in commodities that arefrequently grown in greenhouses (radish, tomatoes, sweet peppers, eggplant, cucumber, lettuce,lamb’s lettuce, and celery) and in dry products which could have been desinfected withmethylbromide (almonds, wheat) and babyfood with vegetables. A separate analysis for pyrethroidswas carried out on some of the samples of apples, strawberries and lettuce. N-methylcarbamateswere looked for in lettuce, leek, and fresh herbs. Ethephon analysis was carried out on apples andprochloraz analysis on avocados and mangos.
Samples were refrigerated and analysed within 2-10 days. Three officially recognized laboratorieswere involved. The two major officially recognized laboratories involved in the monitoringprogramme were accredited for the most important analytical methods and commodities, andaccreditation was gradually extended. The certificates of accreditation of the « WetenschappelijkInstituut Volksgezondheid-Louis Pasteur (Afdeling Voedingswaren)» and the « Fytolab » can befound on the website of the accreditation body BELTEST (http://beltest.fgov.be/). Both laboratorieshad participated in the European Commission’s Proficiency Tests and in the Workshops on Co-ordinated Analytical Quality Control. The laboratories to a large extent take into account annex II ofCommission Recommendation 1999/333/EC. The Dr. L. Willems-Institute is only accredited forchlormequat and has, as to be expected, not taken part in an EU proficiency test.
Out of a list of 150 different pesticide residues sought in fruit and vegetables, a total of 43 werefound at least once during this random monitoring programme. This means that, compared toprevious years, again more pesticide residues were sought but again less were found. For fruits andvegetables, the ten most frequently found pesticide residues, in decreasing order of frequency(found/sought) are: chlormequat, propamocarb, bromide ion, imazalil, prochloraz, chlorpropham,dithiocarbamates, iprodione, thiabendazole carbendazim. Most of these are found by single residuemethods, which are only executed when the presence of residues is expected. When counted onabsolute number of findings, the ten most frequently found pesticide residues, in decreasing order ofnumber of findings, are: chlormequat, iprodione, dithiocarbamates, bromide ion, tolylfluanid,imazalil, propamocarb, thiabendazole, carbendazim, tolclofosmethyl.In cereals, out of 11 pesticide residues sought, the following pesticide residues were found at leastonce : bromide ion, dichlorvos, malathion and pirimiphos-methyl.In processed products, only chlormequat and chlorpropham were detected.
A total of 1029 samples were analysed : 352 fresh fruit, 502 fresh or frozen vegetable, 38 potato, 35raw cereal and 102 processed food samples were counted. Fruit and vegetables were fresh exceptfor peas for which frozen products were sampled and for broccoli and beans for which fresh andfrozen samples were included.
In 54% of the samples of fruit and vegetables, no residues were found, similar to the result ofprevious years. No residues were found in 40% of the fruit samples, 64% of the vegetable samples,37% of the potato samples, 14% of the cereal samples and 91% of the samples of processed food.All these samples were from conventional produce (not organic), except some of the samples ofbabyfood. No samples with pesticides were found for avocado, radish, spinach, several fresh herbs,cereal products and babyfood. Pesticides were found most often in grapefruit (96%), lettuce grownin greenhouses (89%), bananas (86%), lamb’s lettuce (73%), and pears (72%). It should be notedthat these grapefruits and bananas are analysed including the peel, and that removing the peel canremove most of the pesticide residues. A maximum of 6 different pesticide residues could be foundin one sample (lettuce).
Significantly less exceedances of MRLs (MRL= maximum residue level) were counted than inprevious years. No exceedances at all were found for babyfood, cereals and cereal products,
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potatoes and potato products, grapefruit, almond, apple, tablegrapes, strawberries, avocado, banana,radish, tomato, egg plant, cucumber, broccoli, spinach, peas, beans, leek.In 38 samples or 3.7% of the total number of samples, the MRL was exceeded : in 4.2% of the fruitsamples, 4.4% of the vegetable samples, and in one sample of processed food. Note thatexceedances were counted in this reportnot taking into account the uncertainty on the analyticalresult. More exceedances related to EC MRLs than to national MRLs, reflecting the progress inharmonisation compared to previous years. A lot of exceedances are related to MRLs at the limit ofdetermination. Relatively high percentages (>10%) of exceedances were found for peach, mango,lamb’s lettuce, fresh herbs as a group and celery. Two exceedances related to the EU coordinatedprogramme (both samples were lettuce). A remarkable decrease in exceedances compared to theyear 2000 was noted for concentrated tomato products, apples, table grapes, cucumbers, headcabbage, spinach, peas and babyfood. The situation for carrots, lamb’s lettuce, lettuce grown ingreenhouses, and celery was also better in 2001 than in 2000. On the other hand, for pears, moreexceedances were found in 2001 compared to 2000, which can be related to the lowering of themaximum residue level for chlormequat on 1 July 2001.For a good understanding, it is important to know that exceedances are only exceptionally apossible health threat. MRLs are based on good agricultural practices and checked to be sure thatthe acceptable daily intake or acute reference dose are not exceeded. A big survey in the past hasdemonstrated that acceptable daily intakes or not exceeded in practice, as chronic exposure is to belooked at. On the other hand, one exceedance found this year for chlormequat in pears could haveresulted in an exceedance of the acute reference dose in toddlers if eaten fresh in a large quantity onone day and without pealing. A similar conclusion can be raised for one exceedance formethamidophos in peaches using the temporary acute reference dose. Although no final conclusionon the acute reference dose of omethoate is reached, the current knowledge in 2002 indicates thatthe one exceedance found for omethoate in lettuce might also have resulted in a possible health risk,for all age groups.
No methidathion was found in apples, so that we could not participate in this special excercice forhomogeneity factors of recommendation 2001/42/EC.
Contact :E-mail : [email protected] : +32 2 210 48 43; Fax : +32 2 210 48 16Mail-address : Pachecolaan 19/5, B-1010 Brussels
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Presentation of the results
The results are presented in Tables A to G, in the format recommended by the Commission. Thefollowing tables of the format are not included in this report, as they remained empty : table A1-PartII, table D3 and D4, table F. Table A1 gives data on the number and origin of samples, and resultsrelated to the MRL. For the results of this year 2001, unfortunately some information on country oforigin was lost from the database. Table A2 is a list of pesticides which were included in analyticalmethods used during this monitoring programme. It gives the number of samples in which thepesticide is sought, the number of findings and the reporting level. Not only the pesticidesmentioned in EC-directives are included, but all pesticides. The reporting level is the limit ofdetermination of the laboratory, even in those cases where this limit is lower than the legallyrequired limit of determination. This results for some samples in the reporting of levels which arelegally absent. This is a change of the way of reporting compared to previous years and is due to anagreement on the EU level. When laboratories had a higher limit of determination than that in thelegislation, this higher level is the reporting level. For instance the reporting levels are higher fordithiocarbamates, iprodione, and imazalil. Table B gives the detailed results of the co-ordinatedprogramme. Table C contains the detailed results of the national programme, including the co-ordinated programme. Only pesticides which were found at least once, are listed, although muchmore were sought. In tables C, fruits and vegetables are listed according to their listing in annex I ofdirective 90/642/EEC, starting with citrus fruits. Please note that the exceedances counted in TableB and C are mathematical exceedances, not taking into account the uncertainty of the analyticalresult. Table D1 gives a list of exceedances of EC harmonised MRLs, which were higher than 1.5 xMRL. Similarly, table D2 lists exceedances of national MRLs. Table E gives information onmultiple residues in single samples. Table G comments on laboratories.Please note that processed products are not included in tables D and A2, in accordance with the EUguidelines. You can find the details on those products at the end of tables C.
Background of MRL legislation
Pesticide residue levels in foodstuffs cannot be higher than the analytical limit of determinationunless another maximum residue level (MRL) is fixed after an evaluation of the safety andnecessity of the use.Pesticides or plant protection products are applied in order to protect plants against diseases such asthose caused by fungi (fungicides are used then), against attacks by insects (protection withinsecticides), etc. Also growth regulators are covered by the same legislation on plant protectionproducts. Plant protection products are not only used before harvest, but in some cases also postharvest to prevent rotting (e.g. citrus fruit), to prevent sprouting of potatoes, or to protect againstinsects (e.g. raw cereals).MRLs are set as low as possible, in accordance with the good agricultural practice (not higher thannecessary for plant protection), but never higher than what is safe (an authorisation for use will notbe given if the proposed MRL is evaluated as unsafe). As a consequence, most exceedances ofMRLs do not result in a safety problem.Not all MRLs higher than the limit of determination should be interpreted as an authorisation foruse in Belgium, as MRLs might also be based on authorised uses in other European countries orthird countries : MRLs are harmonised to ensure free trade after a safety evaluation. Theharmonisation process is still ongoing, explaining differences in legislation in different countries.On the other hand, an MRL at the limit of determination can be linked to an authorised use whichdoes not normally result in residues on the food after harvest.
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DENMARK
Pesticide Residue Monitoring of Fruits, Vegetables and Cereals in Denmark – 2001
IntroductionThis report to the Commission of the European Communities includes national and co-ordinatedmonitoring results from the Danish pesticide monitoring programme 2001 of fruit, vegetables andcereals (including samples of processed food and infant food).Results from the monitoring of samples of animal origin are reported elsewhere.
SummaryA total of 3481 samples were analysed at two laboratories, both accredited to pesticide analysis.The number of samples has increased considerable compared to 2000 where the pesticidemonitoring system had a reduced capacity due to restructuring of the laboratory organisation.Danish grown as well as commodities grown in other EU member states and in third countries wereincluded in the monitoring.Pesticide residues were found in 68% of the fruit samples, 21% of the vegetable samples and in 9%of the cereal samples. Residues exceeding the maximum residue limits (MRLs) were found in 4%of the conventionally grown samples.The toxicological evaluation concluded that in general the detected residues did not constitute ahealth hazard to the consumer although for a few samples residues were toxicologicallyproblematic.
OrganisationThe Danish pesticide monitoring system is organised by the Institute of Food Safety and Nutrition,the Danish Veterinary and Food Administration under the Ministry of Food, Agriculture andFisheries with participation of regional food control authorities and the Food Control Laboratory inCopenhagen.
SamplingThe Institute of Food Safety and Nutrition designed the sampling plans. They were based on thedietary consumption pattern, production and import data, and monitoring results from previousyears.Samples where taken by authorised personnel from the 11 Danish Regional Veterinary and FoodControl Authorities mainly at wholesalers and importers. 11% of the Danish grown samples weretaken at primary producers and 4% at shops. Samples of processed food (including infant food)were taken at shops.44% of the samples were fresh or frozen fruit, 43% were fresh or frozen vegetables, 6% werecereals and 7% were processed products. 34% were of domestic origin, 41% were grown in otherEU member states and 25% from third countries. Sampling included 4% commercially frozenproduce and 5% organically grown samples.Analysis and quality assuranceThe analytical methods are developed and validated by the Institute of Food Safety and Nutrition.The laboratory at the Regional Food Control Authority in Copenhagen performed the majority ofthe analyses. The Institute of Food Safety and Nutrition performed confirmational analysis forresidues exceeding 75% of the MRL. Both laboratories are accredited for pesticide analysis incompliance with EN45001 by the Danish body of accreditation, DANAK (certificate numbers 315and 350). Thelaboratories participate in the relevant FAPAS performance verification scheme."Guidelines concerning Quality Control Procedures for Pesticide Residue Analysis" has beenapplied for all methods. Mass selective confirmation was performed for part of the GCmultimethods and for the LC/MS methods for cereals.
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The fruit and vegetables were analysed for 130 pesticides using a GC multi method based onextraction with acetone/cyclohexane/ethyl acetate, a HPLC method for fungicides (benomyl-group,thiabendazole, biphenyl and orto-phenylphenol) and a spectrophotometric method for the sum ofdithiocarbamates (maneb-group). The cereals were analysed for 80 pesticides using a GC multimethod and two LC-MS/MS methods (glyphosate, chlormequat and mepiquat).In 2001, no authorisation for the use of disulfotone, oxydemeton-methyl, phorate and thiometonexisted in Denmark. Oxydemeton-methyl, phorate and thiometon were included in the monitoringprogramme.In the analytical methods 1-2 spiked samples were included in each analytical batch. The GC multimethods included spiked samples containing 8-50 pesticides at 2 concentration levels alternatingbetween all pesticides. Bracketed calibration was performed with matrix-matched standards or puresolvent standards. The reporting levels entered in Table A are the lowest calibration levels (LCL)achieved in at least 90% of the analytical series. Results below the general LCL have only beenreported, if they exceeded the LCL of that specific analytical series. Samples with pesticide residuesexceeding the MRL were confirmed by analyses at the Institute of Food Safety and Nutrition exceptfindings of dithiocarbamates. Due to the methodology applied it is not possible to distinguishbetween dithiocarbamates included in the MRL definition and other dithiocarbamates for which noMRL has been fixed. Thus it is not possible to report confirmed exceedances for the maneb-group.
ResultsPesticide residues were found in 68% of the fruit samples, 21% of the vegetable samples and in 9%of the cereal samples (excluding organically grown samples and findings of glyphosate,chlormequat and mepiquat).Fiftyone samples of cereal samples were analysed for glyphosate, chlormequat and mepiquat.Residues were found in 51% of the 41 conventional grown samples.Samples of organically grown fruit, vegetables and cereals were analysed (148 samples of fruit andvegetables, 41 samples of cereals). Pesticide residues found are shown below.
Residues found in samples declared as organically grownCommodity Residue found Country of origin
Apple Diphenylamin 0.05 mg/kg ItalyCarrot Hexachlorobenzene
Quinotozene0.01 mg/kg0.01 mg/kg
Denmark
Carrot Quinotozene 0.01 mg/kg DenmarkOrange Dicofol 0.35 mg/kg Italy
Strawberry jam Procymidon 0.04 mg/kg DenmarkMaize, dried Pirimiphos-methyl 0.34 mg/kg Italy
Rye Pirimiphos-methyl 0.01 mg/kg DenmarkRye Chlorpyrifos 0.01 mg/kg Denmark
Wheat Chlorpyrifos 0.03 mg/kg Denmark
Residues exceeding the maximum residue limits (MRLs) were found in 118 samples correspondingto 4% of the conventionally grown samples.More that one pesticide was found in 22% of the conventionally grown samples.Substances have been reported according to their residue definition. Due to the methodologyapplied results for the maneb-group may include dithiocarbamates not included in the MRL-definition.
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ND70%
> MRL1%
? MRL29%
ND21%
> MRL8%
? MRL71%
ND31%
> MRL8%
? MRL61%
Danish grownGrown in other
EU member statesGrown in countries
outside the EU
For processed foods MRLs were calculated using estimated factors for concentration or dilutionduring processing.Some of the MRLs changed during 2001. Tables B, C and D do not reflect this fact as only oneMRL are shown in the tables. The table below lists the combinations of commodity and pesticidewhere more than one MRL were used when evaluating detected residues. Detected residues were inevery case compared to the MRL that were in use at the time of sampling.
ND93% > MRL
1%
? MRL6%
ND65%
> MRL3%
? MRL32%
ND70%
> MRL3%
? MRL27%
Danish grownGrown in other
EU membe r statesGrown in countries
outside the EU
Figure 1: Residues in conventionally grown fruits (Danish Pesticide Monitoringprogramme 2001). ND: Not detected
Figure 2: Residues in conventionally grown vegetables (Danish Pesticide Monitoringprogramme 2001). ND: Not detected
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Commodity/pesticide combinations where more than one MRL were used whenevaluating detected residues in samples from 2001
Commodity Pesticide MRL (old) 1)
(mg/kg)MRL (new) 1)
(mg/kg)Banana Thiabendazole 3 E 5 E
Cherry Diazinon 0.02 N 1 E
Cucumber Carbendazim 0.5 E 1 E
Cucumber Metalaxyl W 0.5 E
Grape Diazinon 0.5 N 0.02 E
Grapefruit Dicofol 0.02 E 2 E
Kiwi Quinalphos W 0.05 E
Lemon Dicofol 0.02 E 2 E
Lemon Quinalphos W 0.05 E
Lettuce Metalaxyl W 1 E
Mandarin, clementine Dicofol 0.02 E 2 E
Mandarin, clementine Thiabendazole 6 E 5 E
Melon Endosulfan 0.05 N 0.3 E
Melon Pyrazophos 0.2 N 0.05 E
Orange Dicofol 0.02 E 2 E
Orange Endosulfan 0.05 N 0.5 E
Orange Thiabendazole 6 E 5 E
Pear Chlormequat 0.05 N 0.5 E
Pear Endosulfan 0.05 N 0.3 E
Pepper,sweet Pirimiphos-methyl W 1 E
Raspberry Metalaxyl W 0.05 E
Strawberry Benomyl-group W 0,1 E
Tomato Endosulfan 0.05 N 0.5 E
1) E: EU-MRL; N: National MRL; W: No MRL
Toxicological evaluationA toxicological evaluation was performed for samples with residues exceeding the MRL, multipleresidues and residues where no MRL was set. The evaluation concluded that in general the detectedresidues did not constitute a health hazard to the consumer. However, findings of chlorinatedpesticides such as hexachlorbenzene and dieldrin are undesirable, due to accumulation in theorganism. One sample of carrot with 0.11 mg dieldrin/kg wasestimated to constitute a toxicologicalproblem if consumed by small children. One sample of orange with multiple residues (chlorpyrifos,dicofol, fenitrothion, fenthion, imazalil, methidathion) and one sample of fresh ginger (HCH,lindane) could constitute toxicological problems. Twelve samples had residues that might exceedthe Acute Reference Dose. ARfD (dimethoate and omethoate in lettuce (0.68, resp. 0.09 mg/kg), ingrape (0.04, resp. 0.03 mg/kg) and in kaki/sharon (0.08, resp. 0.07 mg/kg); omethoat in kaki/sharon(0.04 mg/kg); methidathion in orange (0.21 mg/kg), in lemon (four samples) (0.33 – 0.62 mg/kg)and in kumquat (0.50 mg/kg); profenphos in grape (0.25 mg/kg); fenthion in clementine (0.40mg/kg). The residues were judged to be toxicologically acceptable.
Regulatory actionsFor reporting purpose the analytical result is compared directly with the MRL. The analyticaluncertainty is taken into consideration before regulatory actions are taken.The following up of violations lies with the Regional Veterinary and Food Control Authorities.Most frequently the action for confirmed exceedances was to order the companies to update theirown-check procedures in combination with warnings.
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Annexes:Table A 1 - Part I: Table A 1 - Part I: Summary of numbers of samples, sample origins
and results (surveillance sampling)
Table A 1 - PartII:
Table A 1 - Part I: Summary of numbers of samples, sample originsand results (follow-up enforcement sampling)
Table A 2 - Part I: Summary table of pesticides sought and found (surveillancesampling)
Table A 2 - PartII:
Summary table of pesticides sought and found (follow-upenforcement sampling)
Table B: Notifications of the co-ordinated programme (specific exercise) tothe European Commission
Table C: Notifications of the results of Check Sampling and Monitoring ofthe National Programme to the European Commission
Table D1: Details of Residues Exceeding EC-MRLs (surveillance sampling)
Table D2: Details of Residues Exceeding non-harmonised MRLs, includingnational MRLs in Open positions) (surveillance sampling)
Table E: Details of Samples with Multiple Residues (>=2) in Single Samples
Table G: Laboratories
Not included
(no data):
Table D3, D4, F
16
GERMANY
Summary of the Results from the Federal Republic of Germany
The report contains the results of the tests carried out in fresh and frozen fruit, vegetables andcereals during the 2001 survey period. It includes all of the data transmitted by 45 accreditedlaboratories of the official food control laboratories of the 16 Laender to the ‘Federal Institute forHealth Protection of Consumers and Veterinary Medicine, BgVV’.
In Germany there is a difference between Monitoring Programme and official food control. Parts ofthe data generated in both programmes correspond with the provisions of Directives 86/362/EEC ,90/642/EEC and the Commission Recommendation of 22 December 2000 (2001/42/EC)concerning a coordinated Community monitoring programme. Therefore, the report includes therespective data from both programmes:
- Monitoring programme 1414 samples- official food control 4926 samples.
Samples were taken on the level of producers, manufacturers, wholesalers and retailers, andrestaurants according to a national sampling protocol published as official legal regulations. Theactive ingredients tested for were ingredients which had already been included in the Annexes toDirectives 86/362/EEC or 90/642/EEC.
In the course of the 2001 survey period, a total of 6340 samples were tested for pesticide residuesin the Federal Republic of Germany. In 3442 (54.3 %) samples residues of pesticides were notdetected and in 2675 (42.2 %) samples, residues of pesticides were determineted in compliancewith official, national and EU MRLs. Only 223 (3.5 %) samples contained residues of pesticidesexceeding MRLs.
Table 1 shows the number of samples divided into domestic production and imports and takes intoaccount the three Directives. The overview given in this table indicates that residues of importedsamples exceeded MRLs more frequently than those of domestic foods. The reason could surely beseen in the fact that parts of the imported foods originated from countries with other climaticconditions which require an increased use of pesticides.
Table 1 Overview of the results of the tests performed on domestic and foreign produce.
Domestic samples Import samples
Food item totalamount
withoutresidue
s
residuesup toMRL
residuesaboveMRL
totalamoun
t
withoutresidues
residuesup toMRL
residuesaboveMRL
Cereals 282 195 83 4 16 6 10 0
Fruit/vegetable
2540 1667 796 77 3502 1574 1786 142
Total 2822 1862 879 81 3518 1580 1796 142
The food samples were analysed for a total of 95 different pesticides from which 60 were detectedat least in one sample. Residues of 44 individual pesticides exceeded MRLs.
17
GREECE
SUMMARY OF PESTICIDE RESIDUE MONITORING RESULTS OF HELLAS FOR
THE YEAR 2001
A total number of 1739 samples were examined by 6 laboratories, including 1369
samples of fresh and frozen fruit and vegetables, 5 samples of cereals and 365
samples of processed products.
� fresh and frozen fruit and vegetables
1043 were domestic samples (76.2% of the total number of samples), while 326
samples (23.8%) were imported ones:
• 926 samples (67.6%) contained not detectable residues of the pesticides sought.
• 394 samples (28.8%) contained detectable residues at or below the MRL.
• In 49 samples (3.6%) residues of one or more pesticides at concentrations
exceeding the EU or national MRLs were detected (46 exceeded the EU and 3 the
national MRL).
From the above 1369 samples analysed, 305 samples were also examined for the
pesticides specified in the 2001/42/EC Commission Recommendation. No authorised
uses of disulfutone, oxydemethon methyl, phorate and thiomethon in strawberries
and grapes exist in Hellas. There is also no authorised use of phorate in lettuce, or
phorate and disulfutone in apples.
� Cereals
5 samples of rice were analysed, all of them without detectable residues of the
pesticides sought.
� processed products
365 samples of virgin olive oil – all samples were domestic ones- were analysed:
• 110 samples (30.1%) contained not detectable residues of the pesticides sought.
• 249 samples (68.2%) contained detectable residues at or below the MRL.
• In 6 samples (1.6%) residues of one or more pesticides at concentrations exceeding
the national MRLs were detected.
Samples were randomly taken from points of entry, wholesalers, retailers and
farmgates.
The total number of pesticides analyzed for was 207. The 10 most frequently
pesticides found were: maneb group (53.4% of samples analysed), benomyl group
(23%), chlorpyrifos (8.9%), phosalone (8.7%), endosulfan (5.7%), myclobutanil (4.8%),
bifenthrin (4.4%), bromopropylate (4.3%), procymidone (4.1%), tetradifon (3.2%).
The reporting levels are generally those routinely achieved in the laboratories.
18
In Table F, no results of the homogeneity exercise 2001 are reported, since all
samples analysed, contained not detectable residues of phorate in potatoes and/or
methidathion in apples.
QUALITY ASSURANCE
The EU guidelines are followed as close as possible. The screening of samples by GLC
involves the use of matrix-matched standard mixtures containing the most commonly
encountered pesticides, including at least two pesticides with a poor or variable GC
response or recovery. Bracketing calibration is used. Although most quantitations are
carried out using calibration curves with 3-5 levels covering a limited concentration
range, a single calibration point is sometimes used, for example for confirmation of a
residue, which has already been quantified on a different GC system.
Routine recovery checks and blanks are carried out approximately every 20 samples
rather than on the basis of batches, because of the uneven flow of samples to the
laboratory.
None of the laboratories is yet accredited.
Results are summarised in the following tables and figures.
19
Table 1. Overview of the results from the Hellenic pesticide monitoring programme
2001.fresh and frozen
fruit and
vegetablesCereals Processed foods
Number%
TotalNumber
%
TotalNumber
%
Total
Total samples
analysed1369 100 5 100 365 100
Samples with
non detectable
residues
926 67.6 5 100 110 30.1
Samples with
detectable
residues at or
below the MRL
414 28.8 0 0 249 68.2
49 0 6
EU
MRLs
National
MRLsEU
MRLs
National
MRLs
EU
MRLs
National
MRLs
Samples with
detectable
residues of one
or more
pesticides
exceeding the
EU or national
MRLs
46 3
3.60 0
0
0 6
1.6
20
Figure 1. Results from the Hellenic National monitoring programme 2001 – fresh and
frozen fruits and vegetables.
Total number of samples: 1369 Fig. 1
ND67,6
>3,6
<28,8
Figure 2. Results from the Hellenic National monitoring programme 2000 – cereals.
Total number of samples: 5 Fig. 2
ND100,0%
Figure 3. Results from the Hellenic National monitoring programme 2000 – processed
products.
Total number of samples: 365 Fig. 3
ND30,1%
> MRL1,6%
< MRL68,2%
21
SPAIN
SPANISH PESTICIDE MONITORIN Results –2001
The Spanish pesticide monitoring programme for pesticide residues in food was carried out by theAutonomies Communities coordinated by the Spanish Ministry ofAgriculture, Fish and Food.
The objectives of the programme were to assume that:
The pesticide was used accordingly with the Good Agriculture Practice.The health of consumer was protected.
The vegetables were collected by the inspectors following the requirements of the directive 79/700at the productions and wholesalers level because more that 95% of the Spanish food is produced inSpain a very few are imported food. Then they are sent to the laboratories. The monitoringprogramme has been coordinated by Ministry of Agriculture Fisheries and Food and included theEuropean and national action.
This programme takes into account:
Proportion of the crops accordingly with the production.Requirements from EU coordinated programmeSome special actions concerning problems with certain crop.
Laboratories
14 laboratories carried out the monitory programme but until now their report is not yetaccordingly with the European format that was make at Central Service.
All samples were analysed by multiresidues method and same of their by simple method.
For multiresidues methods the samples were extracted by solvent (acetone or ethil acetate)then partitioned by liquid-liquid. The purification for organo-halogenated and organo phosphatemolecules were performed by cartridge set-pack, florisil or GPC. The determination is conducted byECD, NPD, FPD or hall detector GC/MS is used as confirmation for samples above MRL's whenthe techniques is applicable.
Additional methods were used for determination of methyl carbamate, maneb groups,inorganic bromides, benomyl group and so on.
175 pesticides can be research and we have found 78. (approximatly 44%)
Four laboratories, Madrid, Valencia, Zaragoza and Barcelona were accredited by ENACand others are in very advance fase to obtain the accreditation. The accreditation can be occurredonly if methods was validated by collaborative study. The validation "in house" required a lot ofinvestigation. For the new molecules the accreditation seems difficult to obtained. The threelaboratories were assuming approximately 40% of the samples.
All laboratories were involved in some proficiency test with Almeria university and EUproficiency text.
22
Results
The total number of samples analysed in coordinated EC programme and Spanishprogramme were3.341, the 3.098 and the repartion were 1.362 (43,9%) fruits, 1.519 (49,03%)vegetables, and 217 (4,09%) other vegetables, the 243 (7,84%) cereals.
For cereals only 2 sample (0,8%), was above the MRL's. For vegetables and fruits and otersvegetables the samples that exceeded the MRL's were about 4,4%.
The pesticides that were found the most frequently were accordingly with the crop.
Citrus fruits / chlorpiryphos, dicofol, imazalil, methidathion, ortophenil-phenol, thiabendazol.Pomes fruits/ captan, chlortalonil, folpet, imazalil, phosalone.Stone fruit/ captan, chlorpiryphos, maneb-groupGrapes/chlorpiryphos, dicofol, maneb-group, procymidone.Banana /dimethoate, procymidoneTomato/ chlortalonil, endosulfan, maneb-group, procymidone.Pepper/ endosulfan, metamidophos, pirimiphos-methil, procynidone.Lettuce / cypermetrine, maneb-group, metalaxil, procymidone.
Productos Analizados SINRESIDUOS
CONRESIDUOS
< LMR > LMR > LMR EC > LMR N
Frutas 1362 542 820 762 58 53 5Hortalizas 1519 1080 439 362 77 76 1Cereales 243 223 20 18 2 2Otros p.vegetales
217 205 12 10 2 2
TOTAL 3341 2050 1291 1152 139 133 6
23
FRANCE
YEAR 2001 REPORT ON THE FRENCH MONITORING OF PESTICIDE RESIDUES INPLANT PRODUCTS
SUMMARY
In 2001, a total of 4177 samples of crops (fruits, vegetables, juices, cereal products) were taken andanalysed for 223 active substances of pesticides.MRLs were exceeded in 226 samples (6.2%). The majority of theseexceedances concernedCommunity regulatory provisions (4.2%).Half of the samples did not contain the sought pesticideresidues.The analytical methods used detect most plant health molecules from the level of 0.01mg/kg.Tomatoes, lettuces and similar, apples, strawberries and grapes were sampled as part of theEuropean Commission harmonised monitoring programme. The Community MRLs fordithiocarbamates (maneb group) were exceeded for lettuces and similar; for methamidophos,tomatoes are more specifically affected; and for the benomyl group, strawberries were moreaffected.Targeted surveillance was carried out on lettuces to search for dithiocarbamates anddicarboximides—the most frequent exceedances were indeed caused by the maneb group but alsoby acephate and methamidophos.According to the overall information (table C), it appears that the exceedances for fruits reach 5.6%.This percentage is mainly due to cherries and strawberries. For tropical produce, mangos andpineapples, the exceedances result from a lack of information on these crops on the part of pesticidesuppliers. However, this does not lead to a human health problem because the skin, whichconcentrates residues, is not ingested.As for vegetables, the situation is improving slowly but surely. Peppers are still the worst problemwith lettuces, celeries and carrots. For lettuces, the exceedances observed result from the search forbromides, which can distort statistics with respect to other countries.As in previous years, large samplings of lettuces and similar were taken. They are over-representedwith respect to their dietary consumption in France. In fact 250 samples would be more in relationwith the consumption levels but DGCCRF’s action is also to strengthen surveillance and sometimes"enforcement" in sensitive sectors.Lastly, as regards cereals, only post-harvest pesticides were identified and the exceedances wereinsignificant.
INTRODUCTION
The Community monitoring programme for pesticide residues in plant products is carried out by theDirection Générale de la Concurrence, de la Consommation et de la Répression des Fraudes—DGCCRF (General Directorate for Fair Trading, Consumer Affairs and Fraud Control).The aims of this multi-year programme are to:
▪ monitor compliance with MRLs, and therefore compliance with approved usage ofpesticides in accordance with good agricultural practices.
▪ assess the real dietary exposure of consumers to pesticide residues.
Crops and processed foods are sampled by surveillance inspectors following the samplingprocedure requirements at growers, wholesalers, and retailers. The general sampling programme isdrawn up by the central authority and takes account of national and European priorities.This programme takes into account:
- the dietary proportion of plant products,
24
- the requirements of the EU coordinated programme,- the results of the 1999 monitoring programme,- the targeted inspection on certain fruits and vegetables (peppers and salads).
LABORATORIES
Six DGCCRF laboratories were involved in the monitoring programme and in the targetedsurveillance programme. The results were collected by the Massy laboratory which analysed them.The laboratories generally used multi-residue methods and sometimes specific adapted methods.Using multi-residue techniques, the samples were extracted by solvents (acetone or ethyl acetate),then partitioned by a liquid-liquid partition. Halogenated molecules were purified on adsorbents(Florisil or silica, SPE ) or by gel permeation. (bio beads) Determination and quantification wereperformed by GLC or HPLC with adapted detectors such as ECD, FPD, NPD, Hall, MS, UV,fluorimetry. GC/MS were used for confirmation most of the time.Specific methods were used for the determination of dithiocarbamates, inorganic bromides, maleichydrazide, chlormequat, and benzimidazoles.Several laboratories are accredited by COFRAC for these determinations. For instance, thelaboratory at Massy is accredited for determinations of organo-halogenated compounds,organophosphate compounds, benzimidazoles, dithiocarbamates, etc., and the laboratory inMontpellier for dithiocarbamates and benzimidazoles. (see table G)All the laboratories were involved in proficiency tests organised by BIPEA, FAPAS and/or CHECK
RESULTS
4177 samples were taken for the monitoring programme. Approximately 70% of them were fromnational production. 36% concerned fruits and 51% vegetables.
FRUITS
1505 samples were analysed. The results are presented below.
Breakdown of fruits
42%
52%
6%
sans résidu
avec résidu
dépassements
sans résidu = without residuesavec résidu = with residuesdépassements = exceedances
The situation is satisfactory for apples and bananas. Pears present a non-conformity rate of 5%.Chlormequat was detected in only two samples. The action undertaken over the past two years hastherefore led to a considerable improvement in imported pears.
25
Citrus fruits often contain chlorpyrifos-ethyl and some exceedances are due to post-harvesttreatments. The latter also appear in citrus fruits sold as ‘untreated’.
050
100150200250300350
citronorangem
andarinepom
me
poirepêchecerisefraiseavocatm
angues
EXAMPLES OF FRUITS
anomalies
nombre d'échantillons
anomalies = exceedancesnombre d’échantillons = number of samplesmangues = mangoes; avocat = avocado; fraise = strawberry; cerise = cherry; pêche =peach; poire = pear; pomme = apple; mandarine = mandarin; orange = orange; citron =lemon
VEGETABLES AND MISCELLANEOUS
2140 samples of vegetables were taken by the department. The results of the analyses are given inthe graphs below.
Residues situation in vegetables
58%
35%
7%
sans résidu
avec résidu
dépassements
sans résidu = without residues; avec résidu = with residues; dépassements = exceedances
26
310
29
272
6
78
11
516
53
18
3
33
7
33
5
0
100
200
300
400
500
600
légumesracines
poivrons herbes haricot
Examples of the situation of vegetables
dépassements
nombre d'échantillons
dépassements = exceedances; nombre d’échantillons = number of sampleslégumes racines = root vegetables; poivrons = peppers; herbes = herbs; haricot = beans516 samples are lettuces and similar
Peppers and celery contribute to a considerable extent to the percentage of MRL exceedances. Thissituation, compared with that of lettuces and similar, is more worrisome insofar as the number ofsamples is relatively less high than in the case of salads.For the remaining vegetables and miscellaneous, chicories, mushrooms and cabbages present fewexceedances.
CEREALS AND PROCESSED PRODUCTS
As in 2000, few MRL exceedances were observed in the 271 samples analysed. Two cases ofgamma-HCH presence were detected.
Raw cereals: contamination of 271 samples
0
2
4
6
8
10
12
14
16
0.01 0.02 0.05 0.1 0.2 0.5 1 2 5
chlorpyriphos méthyle
dichlorvos
malathion
pyrimiphos méthyle
chlorpyriphos méthyle = chlorpyrifos-methyl; dichlorvos = dichlorvos; malathion = malathion;pyrmiphos méthyle = pyrimiphos-methyl
27
Raw cereals: contamination of 271 organo-halogenated samples
0
2
4
6
8
10
12
14
0.01 0.02 0.05 0.1 0.2 0.5
deltaméthrine
gamma HCH
deltaméthrine = deltamethrin; gamma HCH = gamma-HCH
As can be seen, cereals contamination is very low. For gamma-HCH (lindane), the maximumcontamination is 0,4 mg/kg; two other samples contain far lower levels.For deltamethrin, the results are satisfactory: in effect the MRL is 1 mg/kgReferring to organophosphate compounds, it should be recalled that the MRLs are respectively 2,2.8 and 5 mg/kg for chlorpyrifos-methyl, dichlorvos, malathion and pyrimiphos-methyl.
Breakdown of the most often incriminatedsubstancesmanébe groupe
15%bénomyl groupe
14%
chlorprophame4% bromures
7%thiabendazole4%
chlorothalonil3%
captane3%
prochloraz5%
quintozéne4%
methamidophos3%
vinclozolinepyriméthanil
3%
procymidone5%
iprodione3%
cyprodinil
oxadixyl5%
dicofol4%
endosulfan9%
pyridabéne3%
acéphate3%
diéthion3%
manébe groupebénomyl groupecaptanechlorothaloniliprodioneprocymidonepyriméthanilvinclozolinecyprodiniloxadixylacéphatepyridabéneendosulfandiéthiondicofol
Main active substances in exceedances (crops)
manébe groupe = maneb group; bénomyl group = benomyl group; captane = captan; chlorothalonil= chlorothalonil; iprodione = iprodione; procymidone = procymidone; pyriméthanil = pyrimethanil;vinclozoline = vinclozolin; cyprodinil = cyprodinil; oxadixyl = oxadixyl; acéphate = acephate;pyridabéne = pyridaben; endosulfan = endosulfan; diéthion = ethion; dicofol = dicofol;methamidophos = methamidophos; quintozéne = quintozene; prochloraze = prochloraz;thiabendazole = thiabendazole; chlorprophame = chlorpropham; bromures = bromides
28
Breakdown of exceedances
France62%
South America7%
Spain15%
other European4%
Africa12%
amérique du sud
afrique
autres europe
Espagne
France
Compared with the year 2000, a decrease in methamidophos exceedances can be seen. Maneb andbenomyl groups are the main causes of exceedances.
Origin of samples with exceedances ( EC harmonised MRLs)
Amérique du sud = South America; Afrique = Africa; autres Europe = other European; Espagne =Spain; France = France
The proportion of exceedances for France should be related to the proportion of samples. Thesamples of nonconforming French products represent 62% of the total nonconforming products butFrench products account for two-thirds of the products sampled in the market. The situation ofFrench production is therefore no more critical than that of the other European countries in relationto the same means of surveillance.
Plurality of pesticides in the same sample
fréquence de plusieurs pesticides sur l'échantillon
2 pesticides51%
3 pesticides27%
4 pesticides12%
5 pesticides7%
6 pesticides2%
7 pesticides1%
10 pesticides0%
9 pesticides0%
8 pesticides0%
2 pesticides
3 pesticides
4 pesticides
5 pesticides
6 pesticides
7 pesticides
8 pesticides
9 pesticides
10 pesticides
Most samples contain one or two pesticides. The probability therefore of finding in the same sampletwo molecules of the same family appears quite low; on the other hand, a finer analysis would benecessary to ensure that the modes of action on all the results are not equivalent.
29
CONCLUSIONS
In 2001, there were fewer alerts than in previous years. Chlormequat in pears still requiressurveillance but the number of exceedances of the limits has decreased. Methamidophos is still anactive substance to be monitored but the situation has improved. Lettuces and similar are still asource of concern, particularly for dithiocarbamate exceedances. Initiatives are being taken by theFrench committee studying the impact of phytosanitary products (commission française destoxiques) to find a solution. The solution would consist in authorising, for salads, onlyphytosanitary formulations in which dithiocarbamates are combined with other molecules. This willhelp reduce the product dose applied per hectare, thereby reducing dithiocarbamate levels.
The situation of French laboratories regarding accreditation is improving since a third laboratorywas accredited in 2001 for pesticide analyses and in 2002 two other units obtained this status.Research should be developed mainly on widely used pesticides.
30
IRELAND
Irish Pesticide Monitoring Results for 2001.
The Irish pesticide monitoring programme for pesticide residues in food is undertaken bythe Pesticide Control Service of Department of Agriculture, Food and Rural Development as aservice contract to the Irish Food Safety Authority. The objectives of the programme are to ensurethat
- pesticides are correctly applied to foodand that
- consumers are not exposed to unacceptable pesticide residues in food.
In 2001 some 645 samples were analysed for pesticide residues of which 301 were fruit/vegetables,30 were cereals and the remainder were food of animal origin.
Fruit and vegetables:60 different types of fruit and vegetables were analysed as part of the monitoring
programme. 29.2% of the samples were of domestic origin and the remaining 70.8% were either ofimported or unknown origin. The samples were analysed for residues of up to 89 pesticides andtheir metabolites. 49.5% of samples were found to contain pesticide residues while 3.3% of the totalnumber of samples analysed contained residues in excess of the MRL.
Enforcement action is taken by Ireland only in respect to those pesticide MRL’s which are definedin the EU residue directives, 76/895, 86/362, 86/363, 90/642 and their amending directives.
Details of the pesticide residues detected are provided in the attached tables. In the fruit andvegetable samples analysed residues of 37 different pesticides were detected. MRL’s exist for 30 ofthese compounds and have yet to be established for the remaining 7.
The pesticides most commonly encountered in fruit and vegetables were Thiabendazole (13.5%),carbendazim (7.1 %), captan (6.9%), chlorpyriphos (5.1%), iprodione ( 5.0%), dimethoate (4.4%),dicofol (4.2%), vinclozolin (3.8%), chlorothalonil (3.5%) and chlorfenvinphos (3.4%) etc were theresidues most commonly detected in the pesticide residue monitoring programme.
The distribution of pesticides found in 2001 is consistent with the results of previous years.Thiabendazole is primarily detected in citrus, pome fruit and miscellaneous fruit.;Carbendazim was detected in a range of fruit;Captan was found in fruit generally but mainly in pome fruit. Only in the case of pears wereresidues of captan and folpet found together in the same sample. ;Chlorpyriphos was primarily detected in citrus fruit ;Iprodione was found in a range of fruit and vegetables, particularly the leafy vegetable groups.;Dimethoate was detected more often in 2001 than in previous years and while found in both fruitand vegetables it was present most often in apples and in lettuce.;Dicofol was, as in previous years, found predominantly in citrus fruit;Vinclozolin was found in a range of fruit and vegetables but was found most frequently in kiwifruit.;In all 40 samples (13.5%) contained residues of 2 pesticides, 21 samples (7.1%) contained residuesof 3 pesticides, 2 samples (0.7%) contained residues of 4 pesticides, 3 samples (1 %) containedresidues of 5 pesticides.
31
Cereals:Cereal samples, 18 barley and 12 wheat, were analysed for residues of 89 pesticides and theirmetabolites. The barley samples were all of domestic origin while 75% of the wheat was ofimported origin. A residue of Pirimiphos-methyl was detected in one wheat sample analysed. NoMRL exceedance was detected for the cereal samples analysed.
MRL violations:10 samples of fruit and vegetables were found to contain pesticide residues in excess of the
EU MRL’s. 2 of these samples were of domestic origin while the remainder were imported ( 5 EUproduction and 3 from outside the EU). 9 of the 10 exceedances related to MRL’s which were set atthe LOD which suggests that, at least within the EU, the pesticides were applied to crops illegally.An assessment of the risk associated with the dietary intake of the pesticide /crop combinations inthose cases where the MRL was exceeded did not indicate any risk to the consumer for all of the 10samples concerned.
Quality Control Practices in the laboratory:- The laboratory works to the ISO 17025 accreditation standard which was achieved in
December of 2000.- The laboratory participates in both EU proficiency (when available) and in a series of
annual FAPAS proficiency programmes for pesticide residues in fruit and vegetables.- The work of the laboratory takes into account the guidelines set out in the EU Quality
Control Criteria as agreed by the EU residue analysts in co-operation with the EUcommission.
32
ITALY
No data were provided by Italy
33
LUXEMBOURG
Pesticide residues monitoring in fruits and vegetables and cereals in Luxembourg in 2001
SummaryThis report comprises the results of the coordinated and the national pesticide monitoringprogramme in fruits, vegetables and cereals on the Luxembourgian market in 2001.
The samples were collected by a food inspector according to an annual sampling plan. Importedproducts were sampled at wholesaler distribution points, local products were sampled at retailers atthe central market in the City of Luxembourg. Only routine sampling (no follow-up enforcementsampling) was done. As far as practicable sampling was done according to directive 79/700/EEC.
The samples were analysed by the division of food control being part of the Laboratory of NationalHealth. All samples were analysed by a gas chromatographic multiresidue method with ECD, NPDand MSD (DFG S19, modified). A relative standard deviation of 30% for the analysis was takenwhen deciding whether a MRL was exceeded or not.
Of the pesticides recommended to monitor by the Commission, acephate, azoxystrobin, thiometon,the maneb-group and the benomyl-group were not determined in the 2001 exercise.Disulfoton and phorate are not authorized in Luxemburg in fruits and vegetables, thiometon has aMRL of 0.5 mg/kg for fruits and vegetables, oxydemeton-methyl one of 0.4 mg/kg (except carrots),respectively.
A total of 171 samples were analysed consisting of 157 samples of fruits and vegetables, 10 cerealsamples and 4 processed products. 17.5% of the products were of Luxembourgian origin. Sevensamples contained residue levels higher than EC MRL.
Table: Summary of the 2001 monitoring programme (co-ordinated (EC) and national programme)
Number of samplesanalysed
(fruits, vegetables andcereals)
No of sampleswithout residues
No of sampleswith residues at
or below theMRL
No of samplesexceeding EC-
MRL
No of samplesexceeding N-
MRL
171 109 52 7 3
Pyrimethanil, iprodione and procymidone were found most frequently (35 times), the MRLs wereexceeded only once by these fungicides, however. The fungicide metalaxyl was found in 5 samples,exceeding the MRL twice in strawberries. Methidathion was found 3 times in lemons, 2 times theMRL was exceeded by the insecticide. Of the commodities analysed, pesticides were mostfrequently detected in lettuce, grapes and strawberries.
As methidathion was below reporting limit in all four composite samples, the single units were notfurther analysed.
34
NETHERLANDS
SUMMARY
During 2001 about 2900 samples, both domestic and non-domestic products, were analysed in thenational and coordinated monitoring program. This number was slightly higher than the number ofsamples analysed in 2000 (ca. 2600). Domestic products made up 44 % of the samples, 27 % of thesamples came from other EU countries, 28 % from non-EU countries. Imported products in generalshow higher percentages of MRL-violations. Domestic products show residues above the reportinglimit in about 43 % of the samples, whereas non-domestic products contain residues in 68 % (EU)and 60 % (non EU) of the cases, respectively.In 2001 the violation rate was comparable with 2000. Dutch products contained residues above theMRL in 3,9 % of the cases, non-domestic products had violation rates of about 13 %.
INTRODUCTION
Pesticide residue control has been a task of the Dutch Inspectorate for Health Protection/FoodInspection Service for many years. Therefore, a suitable infrastructure is present for the EU-monitoring as required by directives 90/642/EEC (products of plant origin), 86/362/EEC (cereals)and Recommendation 2001/42/EU (the harmonised specific program 2001).After a strong decrease of sample numbers due to a reorganisation in 1998 the centralised pesticideresidue analysis unit came to full capacity in 2000. By further increasing efficiency more samplescould be analysed.Therefore, the number of samples has risen to 2900 in 2001, compared to 2600 in2000.
SAMPLING
The samples are taken without prior information about the presence of pesticides in the sample.Therefore, they represent the situation on the market for the product at that time. However,sampling is directed relatively more to products that need attention because of the violation rate inprevious years. Therefore, high violation rates can indicate both an efficient sampling strategy andproblems in the agricultural practice. As required by EU-directive 90/642/EU, a monitoring plan ismade accordingly.The monitoring program is primarily directed to major products in the consumption pattern, butsome capacity is reserved to minor products.In the monitoring program special attention was given to chlormequat on pears, because of the highlevel of exceedances in 1999.It was not possible to obtain suitable samples for the homogeneity exercise.The sampling procedure, i.e. the number of subsamples taken from a lot is regulated by the DutchFood and Commodity Law. This regulation is the implementation of the EC-directive 79/700/EEC.
ANALYSIS AND QUALITY ASSURANCE
The general strategy is detecting as many pesticides as possible in one analysis by using Multi-Residue-Methods (MRMs). The Dutch method consists of an acetone extraction and a partition stepof the residues into dichloromethane/petroleum ether followed by a chromatographic separation andselective detection of residues. The main detection method is gas chromatography (GC) followed byIon-Trap Mass Spectrometric Detection (ITD). Only for some analytes not detectable sensitivelyenough by ITD, a few additional methods are used:- GC with Electron Capture Detection (ECD)- GC with Nitrogen/Phosphorus (NPD) and Phosphorus/Sulphur detection (FPD)
35
For pesticides not amenable to GC, High Performance Liquid Chromatography (HPLC) MRMs areused- with UV-detection for the detection of fungicides thiabendazole and carbendazim- with post-column derivatisation and fluorimetric detection of N-methylcarbamates
Dithiocarbamates are analysed as CS2 using GC-ECD after decomposing with acidic tin-chloridesolution and extraction into iso-octane.All these MRMs together detect about 300 analytes of the 450 pesticides that have an MRL. In 2001the MRM of benzoylurea herbicides was not performed. The remaining pesticides must be analysedby Single-Residue-Methods (SRMs), which are not performed in routine but on a survey base. In2001 special surveys were conducted for imidacloprid and propamocarb, applying LC-MS.Table A2 gives information about the scope of the MRMs (6.1).The validity of the analytical results is governed by a quality assurance system complying withISO17025. The multi-residue methods are within the scope of the accreditation of the laboratory.The centralised laboratory implemented the EU Guideline on Quality Control (6.2). In order tocheck system performance and to avoid false negative results, reference pesticides standardmixtures containing 76 analytes are run in each batch of samples at the lowest calibration level(LCL), which corresponds to the reporting limit. For these mixtures, also 3-point calibration andrecovery checks are performed.
REGISTRATION AND COMPILATION OF DATA
The 5 Regional Inspectorates for Health Protection have a uniform database-system for the storageof sample data and analytical results. The applied MRMs and SRMs are recorded and the results arestored. Because of the registration of MRMs and the scope of the method, also the absence of aresidue can be established.In this report all results above the MRL increased with a default measurement uncertainty of 20 %are considered to be violating. This procedure has been applied in the 2000 report as well. For thecomparison with previous years results from those years have been reevaluated then in the sameway. In the past, the reporting has not been consistent in all cases,e.g.samples not taken accordingto the official procedure were not always indicated as non complying.
MONITORING RESULTS
During 2001 about 2900 samples, both Dutch and non-domestic products, were analysed in thenational and coordinated monitoring program. During the last 10 years the percentage of samples ofimported products has been increased and brought more in line with the consumption pattern(Figure 1). Imported products in general show higher percentages of MRL-violations (Figure 2).Dutch products show residues above the reporting limit in about 43 % of the samples, whereas non-domestic products contain residues in 68 % (EU) and 60 % (non EU) of the cases, respectively(Figure 3).As a follow up to the incident with chlormequat on pears in 1999 about 100 pear samples wereanalysed for this compound. Only 15% of the samples did not contain any detectable residue ofchlormequat. The results did not differ much from the 2000 data. No MRL violations were observedin Dutch pears. The majority of the samples were below 0,2 mg/kg, showing that the growers
36
strongly changed their agricultural practice compared with 1999 and earlier. However, an Italian lotwas tracked containing more than the EU-MRL of 0,5 mg/kg. The lot was destroyed.It was noted in 2000 that in the production of carrots-with-leaves chlormequat was used to obtain abetter (shorter) leaf structure. In 2001 no chlormequat was found in this product. Some other growthregulators, like trinexapac-ethyl and daminozide weren't present either.In 2001 the violation rate of the monitoring samples was comparable with 2000.Dutch products contained residues above the MRL in 3,6 % of the cases, non-domestic productshad violation rates of about 13,9 % (EU-products) and 12,2 % (non-EU products). Tables A.1 andA.2 show summarised statistical data on sampling and residues. Table 2 gives results on mainproducts in the year 2001.
A comparison is made with the results of previous years. For the main products in the nationalprogram considerably more violations were observed with spinach.Fewer violations were observed with:- pear, banana, sweet pepper, melon, carrot, lettuce.
Some other minor products, not within the national program show a considerable violation rate too:- celery, pineapple, grapefruit, raspberry.
Figure 3a. Residues in Dutch
No residue Res. <MRL Res. >MRL
Figure 3b. Residues in products from EU-countries
No residue Res. <MRL Res. >MRL
Figure 3c. Residues in products fromnon-EU-countries
No residue Res. <MRL Res. >MRL
Figure 1. Number of samples not includingincidents
0
2500
5000
7500
10000
12500
avg'87/90
avg'91/93
avg'94/96
'97 '98 '99 '00 '01
Num
ber
sam
ples
NL EU non-EU non-NL
Figure 2. Percentage of MRL violations notincluding incidents
0,0
5,0
10,0
15,0
20,0
avg'87/90
avg'91/93
avg'94/96
'97 '98 '99 '00 '01
%>
MR
L
NL EU non-EU non-NL
37
Some pesticide/product combinations contribute considerably to the overall violation rates of theproducts. Some of these combinations of products and analytes that exceed the MRLs most oftenare given in Table 1. It is remarkable that all these cases regard violations of MRLs at the LOD andimported products. In most cases a majority of the violations stemmed from one origin. Probablythese violations could have been avoided, if the registrant of the pesticide had requested an importtolerance in the Netherlands. Many of these cases regard MRLs not harmonised in the EU.
Several pesticides have been authorized in other countries, but have not only not an importtolerance in the Netherlands, but no MRL at all. These occurrences (about 120) of cyprodinil,fenazaquin, fenhexamid, flufenoxuron, mepanipyrim, quinoxyfen and trifloxystrobine would havegiven additional exceedances in case MRLs at the LOD had existed.
Table 1. Combinations of crops and pesticides that exceed the MRLs most frequently.
Product Pesticide number of % samples MRL main
samples >MRL country of origin
Cucumber oxadixyl 53 7,5 0,05 * Spain
Grape fludioxonil 180 10,6 0,05 * Italy
Grape penconazole 180 6,1 0,02 * Italy
Grape pyrimethanil 180 9,4 0,05 * Italy, South Africa
Grape tebuconazole 180 2,2 0,05 * Italy
Pepper cypermethrin 54 7,4 0,5 * Thailand
Pepper methamidophos 54 16,7 0,01 * Thailand
Pineapple triadimefon 22 27,3 0,05 * Costa Rica
Pineapple triadimenol 22 22,7 0,1 * Costa Rica
* MRL at LOD
LITERATURE
Analytical Methods for Pesticide Residues in Foodstuffs, Sixth Edition, Inspectorate for HealthProtection, Ministry of Public Health, The Hague/Rijswijk, 1996.Quality Control Procedures for Pesticide Residue Analysis, EU Document 3023/2000,http://europa.eu.int/comm/food/fs/ph_ps/pest/qualcontrol_en.pdf
38
Table 2. Samples of crops taken in monitoring program 2001, with percentage MRL violations,comparing origin and previous years.
PRODUCT consumption(g/day)
year EU-coordinated
program
Dutchprogram
2001
samples2001
% samples> MRL
2001
% samples> MRL
2001 Dutch
% samples> MRL
2001 EU
% samples> MRL
2001 non-EU
samplesa year
1999-2000
% samples> MRL
1999-2000
samplesa year
1987-1998
% samples> MRL
1987-1998
Tangerines 13,4 97/02 100 83 4,8 6,5 2,8 46 8,8 159 6,2
Orange 93,7 98/02 150 119 6,7 8,5 4,3 88 10,8 324 4,7
Apple 74,4 96/01 100 131 0,8 0,0 3,0 0,0 91 1,6 601 0,7
Pear 10,8 97/02 50 112 2,7 0,0 13,6 0,0 325 20,5 145 1,7
Peach/nectarine 3,5 98/02 50 81 14,8 13,2 40,0 21 12,2 159 6,5
Grape 14,4 96/01 150 180 27,8 37,4 14,1 101 29,7 348 11,6
Straw berry 4,8 96/01 100 132 9,1 5,9 16,7 21,1 104 6,8 946 3,8
Banana 19,7 97/02 50 54 1,9 1,9 30 11,7 34 0,5
Carrot 13,6 98/02 100 64 3,1 1,9 9,1 0,0 52 11,5 204 5,6
Onion 14,5 04 50 24 4,2 0,0 50,0 0,0 5 0,0 32 0,4
Tomato 26,9 96/01 100 109 6,4 1,6 14,7 8,3 109 7,8 336 1,5
Sw eet pepper 4,2 99/03 100 54 5,6 0,0 4,8 28,6 264 40,3 403 5,9
Cucumber 7,9 00/03 50 53 13,2 0,0 26,9 0,0 69 8,8 270 1,9
Melon 3,3 99/03 50 70 7,1 3,6 9,5 42 33,7 55 3,5
Cauliflow er 14,9 99/03 50 53 0,0 0,0 0,0 47 0,0 145 0,7
Red Cabbage 4,2 00/03 50 17 0,0 0,0 8 0,0 35 0,0
White Cabbage 6,2 00/03 21 0,0 0,0 8 0,0 25 0,0
Lettuce 4,2 96/01 100 108 5,6 4,1 18,2 74 14,2 1073 3,8
Iceberg lettuce 3,3 96/01 31 3,2 8,3 0,0 0,0 32 1,6 156 3,5
Endive 7,3 100 75 9,3 7,0 50,0 43 10,5 549 5,7
Spinach 8,9 98/02 100 41 12,2 6,1 28,6 17 6,1 213 6,5
Beans (fresh) 3,2 97/02 100 96 7,3 4,0 0,0 10,5 55 9,2 272 1,7
Green peas (fresh) 12,6 00/03 50 27 7,4 0,0 0,0 9,1 0 5 0,8
Leek 12,3 04 50 44 9,1 9,8 0,0 34 7,5 173 1,1
Potato 172,6 97/02 100 61 0,0 0,0 0,0 0,0 36 1,4 302 3,0
Rice 10,1 00/03 50 38 0,0 0,0 0,0 22 0,0 35 3,5
Wheat 130,6 00/03 50 164 0,0 0,0 0,0 0,0 81 1,9 58 0,8
Products in program 695,4 2000 2042 7,2 2,6 14,2 7,6
Total 838,8 2500 2894 9,0 3,9 13,9 12,2 2254 15,0 10379 4,1
39
AUSTRIA
PESTICIDE RESIDUE MONITORING IN AUSTRIA, 2001
A total of 962 samples were analysed under the co-ordinated, national pesticide monitoring programand routine samples. Most of the samples were fresh fruits and vegetables. Beside that otherproducts like cereals were analyzed.
The national pesticide monitoring is done according to a nation-wide sampling plan designed by theInstitute of Applied Statistics and System Analysis (Joanneum Research, Graz) in co-operation withthe Federal Minister of Social Security and Generations. The plan was based on data concerningdietary consumption, production and import of fruits and vegetables and results of formermeasurements. The analytical and budgetary possibilities were taken into account, too.The co-ordinated programme of the European Commission was of course also done.
The samples were taken by trained officials from the local Food Inspection Service(„Lebensmittelaufsicht“).
The analysis of the co-ordinated programme, the national monitoring programme and routinesamples also were made by two federal laboratories for food control (Bundesanstalt fürLebensmitteluntersuchung und –forschung in Wien und Bundesanstalt fürLebensmitteluntersuchung in Innsbruck). Two federal laboratories for food control(Bundesanstalten für Lebensmitteluntersuchung in Graz and Linz) made the analyses of somesamples of the national monitoring programme and routine samples. The federal laboratories arepart of the Austrian Agency for Health and Food Safety since 1st june 2002.
The analytical methods were adopted from published methods of the Dutch federal laboratories(„Analytical Methods for Pesticide Residues in Foodstuffs“, 6th Ed., General Inspectorate for HealthProtection, Ministry of Public Health, Welfare and Sport, The Netherlands) and validated in thelaboratories. The fruits and vegetables were analysed up to a maximum of 149 pesticides. Themethods used were a GC multimethod with ECD-, NPD- and FPD-detection. GC/MS-methods areprimarily applied for confirmation purposes of the other GC methods, a HPLC-method forbenzimidazolfungicides and a spectrophotometric method for the sum of dithiocarbamates.
All laboratories involved in the co-ordinated programme and the national monitoring programmeincluding the routine samples got the accreditation in the year 1998.
Summary of results are shown in the following table and figures:
national programme(including routine samples)
co-ordinated programme
fruit and vegetables
number % number %samples analysed 902 60without residues 513 56,9 27 45with residues below MRL 321 35,6 31 51,7with residues above MRL 68 7,5 2 3,3
40
sum of all samples
samples withoutresidues56.1%
samples withresidues
exceeding theMRL7.3%
samples withresidues below
MRL36.6%
Coordinated programm
s am ples without
r es idues45,0%
samples wi th
residues belowMRL
51,7%
s am ples withresidues
exceeding theMRL
3,3%
national programm and routinesamples
s am ples without
res idues56,9%
s am ples withres idues below
MRL35,6%
s am ples with
residuesexceedin g the
MRL7,5%
The most frequently found residues were in the co-ordinated and national programme and routinesamples: Imazalil, Procymidone, Endosulfane, Iprodione, Chlorpyriphos, Dimethoate,Thiabendazole, Methidathion, Metalaxyl and Tolclophos-methyl
The figures below shall demonstrate the individual statistics of the different commodities analysedin the co-ordinated programm and of the six specific commodities analysed in the nationalmonitoring programme:
Co-ordinated programmeDue to the fact, that 12 samples per commodity has to been analysed, only one sample with residuesabove the MRL results in 8,3 % „samples with residues exceeding the MRL“. This has to be takeninto account if evaluating the austrian data isolated from other data.
Apples
sa m ples withoutresi dues
25,0%
sa mp les withre sidues below
MRL75,0%
samples wi th
res iduesexcee ding the
MRL0,0 %
Tomatoes
s am ples withoutres idues
58,3%
s am ples withres idues below
MRL41,7%
s am ples with
residuesexceeding the
MRL0,0%
41
Lettuce
samples wi thoutresidue s
50,0%
sa mp les withre sidues below
MRL41,7%
sa mp les wi thresid ues
exceeding th eMRL
8,3%
Strawberries
s am ples without
res idues66,7%
samples withresidues below
MRL33 ,3%
s am ples with
residuesexceeding the
MRL0 ,0%
Grapes
sample s with out
residues25 ,0%
s am ples with
res id ues b elowMRL
66,7%
s am ples with
res iduesexcee ding the
MRL8 ,3%
42
National programmeDue to the fact, that there were commodities for the national programme isolated, of which higher risk forresidues was identified in the last years, these specific data are representative for the austrian market, but themonitoring has to be seen as „targeted monitoring“. It was the aim, to reflect to the results of the last yearsand to choose special commodities of interest for further examination. This type of monitoring is foreseen forthe next years. Additionally the amount of intake of commodity will be taken into account.
Broccoli
s am ple s with ou tres idu es
92 ,1%
s am ples withres idues below
MRL5 ,6%
samples wi th
res iduesexcee ding the
MRL2,2 %
Lettuce (Bummerl/Eissalat)
s am ples withoutres idues
64,9%
samples wi thre sidues below
MRL
25,7%
samples wi th
res iduesexceeding th e
MRL9,5%
Lettuce (Kopfsalat)
sam ples wi tho utresid ues
5 1,5%
samples wi thresid ue s below
MR L35,4%
s am ples with
resi duese xceed ing the
MRL13,1%
Orangessamples with
residues
exceeding theMR L
4,1%
samples withresidues below
MRL75,3%
s am ples withoutres idues
20,6%
Grapessa mp les wi th
resid uesexceedi ng th e
MRL1 2,5%
sa mp les withre sidues below
MRL55,7%
sam ples wi tho utresid ues
3 1,8%
Zucchinisample s wi th
residue sexceeding th e
MRL3,3%
s am ples with
res idu es belowMRL
30,0%
s am pl es withoutres idues
6 6,7%
43
PORTUGAL
Pesticide residue monitoring in foodstuffs of vegetable originPortugal 2001
Throughout 2001, 496 samples of fruits, vegetables and cereals, and 108 samples of processedproducts were analysed. Nearly 69% of the sampling of fruits, vegetables and cereals were domesticproduction and the remainder products imported from other Member-states and third countries.Processed products, specially covering tomato concentrates and wines, were mostly domestic.
The national programme for fruits and vegetables was based on the EU co-ordinated monitoringprogramme and further complemented with crops selected according to the national averageconsumption and according to results or rates of infringements found in previous years. This latterone was specifically the reason for the inclusion of spinach, peppers and rice. Less important crops,such as sub-tropical fruits, were sampled as part of a rolling programme. The numbers of samplesand pesticides analysed were planned according to the analytical capabilities and availableresources in the participating laboratories.
The great majority of samples were taken by food inspectors of Directorate General of Food QualityControl and Inspection (DGFCQA) and by food inspectors of the homologous regional bodies.These samples were taken mostly at wholesale commerce and wholesalers warehouses. In theautonomic region of Madeira, sampling was carried out by the Regional Inspectorate of EconomicalActivities (IRAE), and samples were generally taken in retail due to the small number and smallsize of wholesalers in that region. Grain cereals were often sampled from milling plants and a smallfraction of samples were collected at farm gate by the regional phytosanitary services. Part of thespinach sampling was carried out by the Consumer Institute at retail commerce.
The following pesticide residue laboratories contributed to the 2001 national monitoringprogramme: Directorate General of Crop Protection, DGPC, (lab 1), Regional AgriculturalDirectorate of Madeira (lab 2) and Regional Agricultural Directorate of Entre Douro e Minho (lab3). A total of 114 individual pesticides plus 2 groups (maneb group and benomyl group) wereanalysed, although not all of them were sought in all the commodities or samples. Lab 1 covered111 pesticides and the 2 groups, lab 2 covered 61 pesticides and the maneb group, and lab 3 covered20 organophosphorous pesticides and the maneb group.
In labs 1 and 3 the GC multi-residue method (MRM) with selective detectors was based in ethylacetate extraction and GPC clean up; lab 2 used acetone, dichloromethane and petroleum ether asextracting solvents. Besides different columns, different selective detectors and/or GC-MS wereused in labs 1 and 2 for confirmation of results. For the determination of the dithiocarbamates thespectrophotometric method was used in labs 1 and 3, and the GC method in lab 2. The N-methylcarbamates were analysed in labs 1 and 2 by extraction with acetone, dichloromethane andpetroleum ether and determination by LC-FLD with on-line OPA derivatization. Besides usingdifferent elution systems for confirmation of results, LC-DAD was also used in lab 2. Thebenzimidazole carbamate group was determined (lab1) by LC-UV after ethyl acetate extraction andacid-base partition and/or ethyl acetate extraction with sodium hydroxide followed by GPC cleanup. This latter method was also used for the determination of pyrimethanil.
The insecticides dissulfoton and phorate are not registered in Portugal and have not been monitored.Oxydemeton-methyl is approved for use in apples, pears, tomatoes and strawberries; thiometon isonly approved for apples. In spite of that, oxydemeton-methyl was not monitored at all, andthiometon was only monitored in the samples analised by lab 2. Validation of the analytical methodwas initiated in lab 1 but it could not be concluded in time to include these compounds.
44
Nevertheless, it should be noted that thiometon (parent), thiometon sulphone, phorate (parent),phorate sulphone and the sulphone of oxydemeton-methyl showed a good performance in lab 1through the MRM, and therefore they would have been detected, if present.
As stated in Table G, none of the laboratories is accredited yet, the main reason being the lack ofadequate facilities, which is also hampering the full implementation of some of the quality controlprocedures. Re-installation of labs 1 and 3 into new facilities is expected to happen in the first halfof 2003 and accreditation in the second half. Accreditation of lab 2 is not foreseen before 2004.
In nearly 60% of the whole sampling of fruits, vegetables and cereals (57% fruits and vegetablesand 79% cereal grains) no residues of any pesticide sought were found. In the remainder samples offruits and vegetables, residues of 45 different pesticides were detected; the ten most frequent ones,by decreasing order, were: maneb (group), benomyl (group), captan, phosalone, phosmet,procymidone, dimethoate, iprodione, diphenylamine and chlorpyriphos. In the remainder samples ofcereals, only five different pesticides were found: malathion, pirimiphos-methyl, chlorpyriphos-methyl, diazinon and dichlorvos. Out of the total sampling of fruits, vegetables and cereals(surveillance and follow up enforcement sampling), 4,8% of the samples exceeded EC MRLs and5,8% exceeded national MRLs. The overall rate of 4,8% exceedances to EC MRLs corresponds toexceedance rates of 5,3% and 1,6% in fruits and vegetables and in cereals, respectively. The overallrate of 5,8% exceedances to national MRLs corresponds to exceedance rates of 6,4% and 1,6% infruits and vegetables and in cereals, respectively. Infringements were more frequent in spinach,lettuce and strawberries, the conclusion being that the control of these commodities must beincreased.
The majority of infringements found relate to both EC or national MRLs set at the limit ofdetermination. All exceedances detected are counted in this report as infringements, without takinginto account the uncertainty associated to the analytical result. However, administrative follow-upactions were generally taken by DGFCQA, IRAE and other regional inspection bodies only in thosecases where the levels found exceeded 1,4xMRL. For values up to 1,4xMRL action taken consistedof official warnings. For results of dithiocarbamates in lettuces and similar and in leafy brassicasadministrative follow-up actions are taken when 2xMRL is exceeded. As a result, a total of 12 caseswere instructed by the competent above mentioned bodies with a view to the levying of fines, andone case was sent to court due to questionable margin of safety. This same case was notified in theRapid Alert System.
Where violations to national MRLs in products originating from other Member-states have fallen inthe situation covered by Article 5º.A of directive 97/41/EC (tolclofos-methyl in peppers,tolylfluanid in apples and fenthion in grapes), the procedure foreseen was immediately initiatedwith a view to the possible adoption of the MRLs set for tolclofos-methyl and tolylfluanid in therespective Member-states of origin. However, the result of consumer risk assessment for fenthion ingrapes precluded acceptance of the MRL in force in the Member-state of origin.
Multiple pesticide residues have occurred in 72 samples of fruits, vegetables and cereals, whichrepresents 14,5% of the total sampling. The highest number of pesticide residues (5) was found inone sample of apples and one sample of lettuce.
With a view to the homogeneity exercise the combination apples/methidathion was selected andtherefore duplicate samples of apples were taken. However, as methidathion did not occur, thisreport contains no Tables F.
Monitoring of processed products included 108 samples, mostly tomato concentrates and wines. Forprocessed tomatoes only residues of the highly polar acephate and methamidophos were found in afraction of the samples. All the levels found were below the MRLs in force for fresh tomatoes and
45
far below the MRLs resulting from the application of the concentration factor (in average 5).Residues in wines were seldom found and, where occurring, levels were negligible in comparisonwith the respective MRLs set for grapes.
46
FINLAND
PESTICIDE RESIDUES MONITORING OF FRUIT, VEGETABLES AND CEREALS INFINLAND - 2001
SUMMARY
The national and EC co-ordinated pesticide residues monitoring was carried out according to theannual program of National Food Agency. Domestic samples were collected by local healthinspectors from farms or retail shops. The majority of import food samples were taken by Customsinspectors from wholesalers. The sampling procedure of directive 79/700/EEC was followed as faras practicable.
Total number of samples was 2439, including 2097 samples of fresh and frozen fruit andvegetables, 67 samples of cereals, and 275 samples of processed foods. For technical reasons theenforcement and surveillance sampling could not be separated in the report. However, in tables D1-4 the separation is made so that all cases where the lot was detained until the analysis was ready, areconsidered as enforcement samples. The enforcement samples have been taken as a follow-up ofviolation, but they are not necessarily from a specific farm or consignment.
Pesticide residues above the reporting limits were found in 47.8 % of the fruit, vegetable and cerealsamples but only in 20.7 % of processed products. The number of samples with residues exceedingthe MRL was 127 (5.2 %). Only cases, where a residue level above the MRL plus analyticaluncertainty was detected, were considered as confirmed residues exceeding the MRL. Six RASFFnotifications were sent during the year.
After each confirmed exceeding of MRL legal action was taken. In case of surveillance samples theholder of the product was ordered to withdraw the remaining parts (if any left) of the inspected lot.Follow up samples were taken from the next lots of the same origin. In case of enforcementsampling non-complying lot shall be destroyed or in some situations the lot may be processed tocomply with the MRL (e.g. aeration to decrease fumigant residues).
The analyses were carried out in two accredited laboratories; Finnish Customs Laboratory (87 % ofthe samples) and Environment Centre of the City of Helsinki (13 % of the samples). Most results ofthe report have been produced by the gas chromatographic multiresidue method, which method isaccredited in both laboratories. The number of pesticides monitored for in the two laboratories bythe multiresidue method was 160 and 89 respectively. In addition maneb and benomyl grouppesticides. inorganic bromide, hydrogen phosphide, maleic hydrazide, glyphosate, chlormequat anddiquat were analyzed in Customs Laboratory from selected samples. The quality control proceduresas described in Commission Recommendation 1999/333/EC have been implemented in bothlaboratories but some elements only partly. Customs Laboratory has participated in three FAPASproficiency tests in 2001 and organized a ring test of dithiocarbamate and bromide analysis amongsome Nordic laboratories.
The homogeneity studies could not be carried out as residues of phorate in potatoes and residues ofmethidathion in apples were not found.
47
SWEDEN
The Swedish Monitoring of Pesticide Residues in Foodof Plant Origin: 2001
Summary of results
In 2001, a total of 2 897 surveillance samples of fruits, vegetables, juices, fruit drinks, cereal grains,cereal products, vegetable oils, and oil seeds were analysed for residues of 224 pesticides (263analytes). National or EU harmonised Maximum Residue Limits (EC-MRLs) were exceeded by 57samples (2.0 %). One sample of domestically grown vegetables contained residues above theMRLs.Apples, strawberries, table grapes, lettuce and tomatoes, in all 555 samples, were analysed in the2001 EU co-ordinated programme. Three of these samples exceeded the EC-MRLs for thepesticides concerned.Detectable residues were found in 21 out of 74 samples of foods for infants and young children.A total of 52 enforcement samples of fruits and vegetables were collected and 17 lots (148.5 tons)were prohibited from being sold.The short-term intake was estimated for 18 pesticides based on the highest residue found in asurveillance (composite) sample and using UK consumption data. The acute reference dose (ARfD)was exceeded for toddlers in two cases, endosulfan in melons and monocrotophos in table grapesand in one case for adults, monocrotophos in table grapes.
Design of the national monitoring programme
The target number of samples to be collected of each food is roughly proportional to the food'sconsumption rate and takes into account both the amount of domestic production and the amount ofimports from EU-countries and third countries. However, the number is also based on theimportance of the foodstuff in the diets of infants and young children as well as residues found inprior samples. The National Food Administration (NFA) is responsible for the pesticide residuecontrol in Sweden.
Surveillance sampling
Samples collected in accordance with the monitoring programme were defined as surveillancesamples, i.e. there were no suspicions about excessive amounts of pesticide residues in the lots priorto sampling.Fresh fruit and vegetables were sampled at wholesalers' warehouses in the first trade channel. Nor-mally, a sample included three sub-samples, each of about 1–3 kg. The sub-samples were collectedfrom at least three different boxes or places throughout the lot. The sample was sealed and labelledwith a unique sample identity.Samples of domestic produced cereal grains were collected at the milling plants. The imported ce-real grains were sampled at the port where the shipment was discharged. Usually, one bulk sampleof about 3–5 kg was collected by stream sampling technique.Most of the samples of processed or frozen fruit and vegetables, juices, fruit drinks, rice, cerealproducts, vegetable oils, and oil seeds were collected in retail shops or department stores.Plant inspectors from the National Board of Agriculture collected most of the samples.
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Enforcement sampling
When a surveillance sample contained a pesticide residue above the national or EC-MRL, theNational Food Administration prescribed a condition for the offering for sale or other handling ofthe food or lot to which the food belonged. As a follow-up, next lots of the commodity from thegrower/exporter were detained and enforcement samples were collected.
Analytical methods and laboratory status
Practically all samples of fruit and vegetables were analysed by the multi-residue method. By thismethod, the samples were extracted with ethyl acetate, cleaned up on an S-X3 gel permeationcolumn and determined by capillary gas chromatography.In all, by using both multi-residue methods and single residue methods it was possible to determine224 pesticides corresponding to 263 analytes. A total of about394 000 residues (analyte/commodity combinations) were sought.All analyses were carried out at AnalyCen Nordic AB, Lidköping. This laboratory is accredited bythe Swedish accreditation authority SWEDAC for all analytical methods used for the NFA’s officialcontrol of pesticide residues in food of plant origin.
Quality control procedures and LODs
The EC guidelines “Quality Control Procedures for Pesticide Residue Analysis”, second edition,1999/2000 have been implemented as far as practicable. The laboratory has participated in sixproficiency tests (Table G).The majority of the pesticide residues were measured and reported from the limit of quantitation(determination), generally in the range of 0.01 - 0.2 mg/kg. For certain pesticides, e.g.cypermethrin, imazalil, methamidophos, procymidone and thiabendazole the EC-MRLs set at theLODs were not achievable in our routine monitoring.
Homogeneity exercise
In the EU co-ordinated programme the homogeneity factor should be determined for methidathionin apples and/or phorate in potatoes. No residues were found of methidathion in apples. Phorate isnot yet included in the Swedish monitoring programme. However, the homogeneity factor wasdetermined for eleven other pesticides. The factor varied between 1.4-5.6.
Authorisation status
None of the four pesticides disulfotone, oxydemeton-methyl, phorate and thiometon is authorisedfor use in Sweden.
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UNITED KINGDOM
THE UK PESTICIDES MONITORING PROGRAMMEBRIEF DESCRIPTION OF PROGRAMME, RESULTS AND MONITORING
1. BackgroundThe purpose of the UK monitoring is threefold: to back up the statutory approvals process for pesticides bychecking that no unexpected residues are occurring; to check that residues do not exceed statutory EU andUK maximum residue levels (MRLs) and to check that human dietary intakes of residues are at acceptablelevels. This monitoring, together with that carried out by local authorities and the food industry provided awide-ranging overview of the residues present in food. Only 0.7% of samples analysed contained residuesabove MRLs, and the majority of these would not lead to an exceedance of the acceptable daily intake (ADI).
The results from the programme of work were submitted to the European Commission in fulfilment ofobligations for reporting results of surveillance for pesticide residues established by Directives 86/362/EEC,86/363/EEC and 90/642/EEC. Results of the co-ordinated recommended monitoring programme carried outacross the EU were again included in the report.
2. Selection criteriaSamples for the main commodity rolling programmes have generally been obtained at fortnightly intervalsfrom two population centres in each of twelve regions of the UK. The centres selected are changed eachyear. Generally, the choice of foodstuffs to be analysed in the programmes represents a balance betweenthe levels of consumption of those foodstuffs, information on the possible levels of residues and the need toensure that as wide a range of commodities as possible is included in the surveillance. Where practicablesamples are taken, prepared and analysed according to CAC guidelines (Recommended Method ofSampling for the Determination of Pesticide Residues (Vol. 2, section 3, Codex Alimentarius, 1993) andPortion of Commodities to which Codex Maximum Residue Limits Apply and which is Analysed (Vol. 2,Codex Alimentarius, 1993). Samples are generally analysed unwashed and unpeeled, with the exception ofroot crops which are routinely washed. Only one variety, from a single source, is included in each sample.
In determining its surveillance programme, the Pesticide Residues Committee (PRC) considers data fromother sources including publications produced by other UK Agriculture departments. The UK also considersdata published on monitoring carried out by other governments, as well as data and intelligence fromindustry and other sources.
3. EnforcementWhen the level of pesticide residues found during PRC surveys indicates use of a non-approved pesticide, orthe use of a pesticide other than in accordance with the conditions of its approval, the source of the samplesinvolved is investigated to establish the cause of the residues. Further targeted surveillance is normallycarried out to check whether the result represented an isolated incident. For UK-produced commodities,enforcement involves the taking of samples from a grower's premises for analysis. If evidence of misuse isfound the grower is prosecuted. In the case of imported produce from third countries, sampling is normallycarried out at the point of entry while the consignment is detained. If unacceptable residues are found, thewhole consignment is refused entry to the UK, and other EU member states are notified. If problems areidentified in retail samples of produce of EU origin, the details are reported to the Member State concerned,to allow the relevant authorities to follow up the case.
4. The 2001 European Union recommended monitoring programmeSurveys were carried out in support of the Commission recommendation for a harmonised, specific, EUprogramme. Samples of apples, grapes, lettuce, strawberries and tomatoes were analysed for a range ofpesticides indicated in the recommendation. Residues were detected in 68 of the 252 apple samples, and29 contained multiple residues. No MRLs were exceeded. Residues were detected in 39 of the 72 grapesamples analysed, and 16 contained multiple residues. No MRLs were exceeded. Residues were detectedin 54 of the 180 lettuce samples analysed, and 17 contained multiple residues. The MRL was exceeded intwo samples. Residues were detected in 115 of the 179 strawberry samples analysed, and 68 containedmultiple residues. The MRL was exceeded in four samples. Residues were detected in 26 of the 144tomato samples analysed, and 8 contained multiple residues. No MRLs were exceeded.
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5. Implications of 2001 results for consumers0.7% of samples analysed contained residues in excess of an MRL. This confirmed that in the vastmajority of cases pesticides were being applied in accordance with their label requirements, andalso provided an assurance to consumers that, where they were being exposed to residues, they wereat safe levels. In all cases where MRLs were exceeded, or where there are potential intake issues, aseparate consumer risk assessment was carried out to establish whether the level of residues presentwould lead to an exceedance of the ADI or, where appropriate the ARfD, by a high level consumer.The risk assessments indicated that in the great majority of cases there would be no exceedance.Both the ADI and the ARfD incorporate safety margins and the risk assessments assume foodintake at the 97.5 percentile level in food surveys. Therefore, even where exceedances arecalculated, the risk to consumers is unlikely.
6. Methods of Work and Quality ControlFull details of the Committee's methods of work are contained inSurveillance: The Estimation ofDietary Exposure to Pesticides - Report of the Working Party on Pesticide Residues: 1991-1993which is published as Food Surveillance Paper Number 50 available from the Stationery Office(ISBN 0 11 243015 5).
6.1 Quality ControlAnalytical methods were deemed acceptable if the level of recovery of added pesticide was between60% - 140%, providing that routinely the mean recovery was in the range 70% - 110%. Resultswhich exceeded MRLs, or which were unusual in occurrence, or were otherwise of particularsignificance were required to be accompanied by acceptable recovery data and, whereverpracticable, to have been confirmed using mass spectrometry. The residues data provided in thisreport have not been corrected for recovery and are expressed, unless otherwise stated, on the basisof the fresh weight of the sample and as defined by the MRL.
6.2 Proficiency Testing ProgrammeAll laboratories carrying out work have taken part in proficiency testing exercises, including theDutch Chek Monitoring Programme and other international programmes. Recognising theimportance of proficiency testing, MAFF started a scheme in 1990 for laboratories known as theFood Analysis Performance Assessment Scheme (FAPAS). All of the laboratories which submitdata to the PRC participate in FAPAS. Since 1997, all laboratories have allowed the FAPASSecretariat to release their individual results and details of their performance to PSD. This allowsan independent check of the laboratories’ performance to be made. Additionally, all of thelaboratories meet the requirements of a recognised accreditation scheme, such as the UnitedKingdom Accreditation Service (UKAS) or the requirements of Good Laboratory Practice (GLP).
THE UK PESTICIDES MONITORING PROGRAMME
Country Total no. of samples No. of samples No. of samplesanalysed * with residues where 1 or more
detected <MRL MRL exceeded
UK 2010 733 27
*= Extract from UK programme. Results of monitoring:Fruit and vegetablesCereal products
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NORWAY
Pesticide Residue Monitoring in Fruit, Vegetables and Cereals in Norway - 2001
A total of 2431 samples of fresh and frozen fruits, vegetables and cereals, both imported (61 %) anddomestically produced (39 %) was included in the monitoring programme for 2001. The monitoringprogramme included also 152 samples of processed products and 35 follow-up samples. A total of132 different commodities were analysed.The samples were taken by trained inspectors from the food control authorities, mainly fromwholesaler’s warehouse in different parts of Norway. Samples from retails and farmgates were alsotaken. The number of surveillance samples of each commodity roughly reflects their share of themarket, but more samples were taken of commodities suspected to contain residues. For sampleswith residues exceeding the MRL compliance samples were collected as a follow-up. Whenanalysing the compliance samples the whole consignement is stopped until the results of theanalysis are ready. If the results of the follow-up again show an exceedance of the MRL the wholeconsignement is destructed. It is the responsibility of the local food control authority to carry out thenecessary procedures concering the follow-up of exceedances.The Norwegian Crop Research Institute, Pesticide Laboratory, did the analyses.All samples of fruit and vegetables were analysed using a GC multi-residue method, based onextraction with acetone (Luke methode), covering 144 pesticides, isomers and breakdown products.Five pesticides were analysed by LC/MS using the same extraction method. LC/MS was also usedfor analysis of N-methylcarbamates, chlormequat, diquat, dithianon and propamocarb. Biphenyl,orto-phenylphenol and progargite were analysed using GC/MS. The dithiocarbamates weredetermined with a spectrophotometric method. The reporting levels are the limit of determinationfor all methods.The Pesticide Laboratory was accredited on April 1st 1997. The accreditation is based on theEuropean Standard EN 45001 and also includes no. 2 and 7 of the OECD Principles of GoodLaboratory Practice, section II. The analyses were carried out in accordance with the QualityAssurance Manual of the Pesticide Laboratory and the EU Guidelines for Pesticide Analysis. As apart of the quality assurance programme the laboratory participate regularly in internationalintercalibrations / proficiency tests. When a pesticide residue exceeds the MRL, quantitativedetermination is carried out on three replicate samples using three-level calibration, recovery ischecked and the identity of the pesticide confirmed by GC/MS or LC/MS.The monitoring programme covered 179 pesticides including some isomers and breakdownproducts.Among the domestic products violations occurred most frequently in celery. Among the importedproducts carambola, mango and celeriac had the highest number of samples exceeding the MRL.Ninety samples of organic grown products were also analysed. A pesticide residue below MRL wasfound in one sample of carrot.
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ICELAND
Monitoring of pesticide residues in fresh fruits and vegetables in Iceland in 2001
An official monitoring program for pesticide residues in fruits and vegetables was carriedout in Iceland in 2001. Samples are taken at wholesaler’s warehouses in Reykjavík. Since fruits forcommercial purposes are not grown in Iceland, all fruits and a greater part of the vegetables areimported.
Around 300 samples are analysed each year. Approximately 85% are imported commoditiesand fruits count for 53% of all samples examined. Samples are analyzed by a GC/MS multi methodbased on ethyl acetate extraction, covering 40 pesticides.
As a main rule the maximum residue limits (MRL’s) conform to EU directives, but in fewcases, where EU has not set any limits, they are in accordance with either Codex Alimentarius orregulations from other Nordic countries. When a pesticide residue exceeds MRL, a new sample isanalyzed to confirm the results. No actions are taken unless the value exceeds the MRL plus astandard deviation.
In 2001 a total of 300 samples were examined for pesticides in fruits and vegetables.Imported samples were 242 and domestic samples 58. In 63% of all samples, no pesticide residues,which were looked for, were detected. 37% of the samples contained pesticide residues andviolations of maximum residue limits (MRL’s) were found in 3% of all samples. Commoditiesoriginated from 26 countries, most came from Spain (26%) and The Netherlands (19%). Thepesticides most frequently found were imazalil, thiabendazole, orthophenylphenol, chlorpyrifos,dicofol, metidation, tolylfluanid, chlortalonyl and iprodion.
The laboratory of the Environmental and Food Agency has taken part in FAPAS and willcontinue to do so in the future. The laboratory has not been accredited yet but is planning to initiatethe preparation work next year. It is estimated that it could take at least 2-3 years to receiveaccreditation.
Iceland participated only partially in the coordinated program.
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LIECHTENSTEIN
Pesticide residues monitoring in fruits and vegetables and cereals carried out inLiechtenstein in 2001
Introduction
This report summarizes the results of the co-ordinated and the national pesticide monitoringprogramme in fruits, vegetables and cereals on the Liechtenstein market in 2001. This report hasbeen prepared according to the recommendation of the ESA as far as technically possible.
Sampling
The samples were collected according to the annual sampling plan prepared by the office for foodinspection and veterinary affairs. The sampling plan is based on the domestic production situationin the agricultural sector and on the ESA co-ordinated monitoring programme. The programme hasstarted in the second half of the year 2001.Samples of fresh fruits, vegetables and cereals were collected mostly from retailers, but also fromfarms and food processing plants. Sampling is done mostly according to directive 79/700/EEC. Thesize of a laboratory sample was at least 1 kg.
Analysis
All samples were analysed by a gas chromatographic multiresidue method (modified germanofficial method DFG S19).This method consists of an acetone/cyclohexane/ethylacetate extraction and a clean-up on a biobeads S-X3 gel permeation column. The extract was analysed by GC with selective detectors (ECD,NPD and FPD) / exception: Carbendazim and Thiabendazol were analysed by HPLC. When apesticide residue exceeded the MRL, the identity of the pesticide was confirmed by GC-MS.Dithiocarbamates were also determined on each sample by using an CS2 evolution method. The CS2is determined by headspace analysing using GC with ECD (DIN 12396-2).
Accreditation and quality assurance
Analyses have been carried out in the Labor Dr. Matt AG, Im Alten Riet 36, FL-9494 Schaan. Thelaboratory is accredited in accordance with the provisions of article 3 of directive 93/99 (accordingto EN 45001[see copy of accreditation certificate in the annex]).
The analytical results are governed by a quality assurance system. The laboratory takes intoaccount, as far as it is possible for a laboratory of its size, of the document “Quality controlProcedures for Pesticide Residues Analysis“- as set out in Annex II to the Recommendation of theESA for the year 1999, OJ L 74, 23.3.2000.
Reporting levels
The lowest residue levels are the same as the limits of determination (generally in the range of0,005 - 0,05 mg/kg). The limits of determination are determined by recovery tests.
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Results
A total of 63 samples were analysed out of which 22 fruits, 37 vegetables and 4 cereals.In 46 samples no pesticide residues were detected. 16 samples showed pesticide contamination at orbelow MRL's national and EC. Two samples contained a residue level higher than the maximumEC and national level. The product pesticide combinations concerned were grape/Maneb group andcarrots/Diazinon, the first one is the sample from domestic production, the second one an importedsample.The total number of residues analyzed for is 32. The pesticides Disulfotone, Phorate, Thiomethoneand Oxydemethonmethyl were not searched for because their use on the products sampled was notauthorized.The most frequently found residues derived from the pesticides Folpet, Azinphosmethyl and fromthe Maneb group.
Summary of results:
Total nr. ofsamplesanalysed
Nr. ofsampleswithoutresidues
Nr. ofsamples withresidues at orbelow theMRL
Nr. ofexceedings
of EC-MRLs
Nr. ofexceedingsof N-MRLs
Co-ordinated and nationalprogramme, vegetablesand cereals
63 46 16 2 2
Schaan, January 9, 2003 PM/st
Encl.: Tables A - G