Pesticide residues in fruits and vegetables from South America – A Nordic project

Food Control 22 (2011) 1701e1706

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Pesticide residues in fruits and vegetables from South America e A Nordic project K. Hjorth a, *, K. Johansen b, B. Holen b, A. Andersson c, H.B. Christensen a, K. Siivinen d, M. Toome e a

National Food Institute, Technical University of Denmark, Mørkhøj Bygade 19, DK-2860 Søborg, Denmark Bioforsk, Plant Health and Plant Protection Division, Høgskolevn. 7, NO-1430 Ås, Norway c National Food Administration, Box 622, SE 751 26 Uppsala, Sweden d Finnish Customs Laboratory, Tekniikanti 13, 02150 Espoo, Finland e Estonian Agriculture Research Centre, Teaduse 4/6, Saku 75501, Estonia b

a r t i c l e i n f o

a b s t r a c t

Article history: Received 14 December 2009 Received in revised form 27 April 2010 Accepted 4 May 2010

The aim of this study was to investigate the amount of pesticide residues in fruits and vegetables from South America. A total of 724 samples of 46 different fruits and vegetables from eight South American countries were collected in 2007. In 19% of the samples no residues were found, 72% of samples contained pesticide residues at or below MRL, and 8.4% of samples contained pesticide residues above MRL. Thiabendazole, imazalil and chlorpyrifos were the pesticide most frequently found. Thirty-seven pesticides were found with frequencies higher that 1% in the samples. The results emphasize the need for continuous monitoring of pesticide residues, especially in imported fruits and vegetables. Ó 2010 Published by Elsevier Ltd.

Keywords: Pesticides Residue analysis South America Fruit and vegetables

1. Introduction In a cooperation project between five countries: Denmark, Estonia, Finland, Norway and Sweden, the results from each countries national monitoring programme for pesticide residues in food were compiled. It was decided that for 2007 the focus would be on samples imported from South America. This Nordic collaboration makes it possible to monitor more samples from a specific area than the individually countries are capable of doing on their own. The outcome is a better statistic foundation to investigate the frequency of residues and to evaluate if the small number of monitoring samples from each country is adequate. The aim of this project was to gather as much information as possible on pesticide residues in crops imported from South America. Each of the five countries analysed the samples according to their own analytical scope, which means that the samples were analysed for 170 to 326 pesticides including metabolites and degradation products. For several years the use of pesticides have been escalating in the developing countries, particularly those in the tropical regions seeking to enter the global economy by providing off-season fresh fruits and vegetables to countries in more temperate climate. Such countries are becoming important fruit baskets to the world being capable of harvesting two or even three times each year (Ecobichon, 2001). However, the ambitions to increase the exported ‘cash’ crops * Corresponding author. Tel.: þ45 35887464. E-mail address: [email protected] (K. Hjorth). 0956-7135/$ e see front matter Ó 2010 Published by Elsevier Ltd. doi:10.1016/j.foodcont.2010.05.017

are driving the developing countries toward an increased use of pesticides. The heavy use of pesticides may result in environmental problems like disturbance of the natural balance, widespread pest resistance, environmental pollution, hazards to non-target organisms and wildlife, and hazards to humans. Control programmes for pesticide residues in the developing countries are often limited due to lack of resources and rigorous legislation is not in place. Moreover, training programmes for technical personnel and equipment for monitoring pesticide residues are often lacking. Another reason to focus on pesticide residues in samples from South America is that the annual EU monitoring report shows that pesticide residues in these samples more often contain residues above the Maximum Residue Limits (MRLs) compared to pesticide residues in samples from EU countries (EU Commission, 2006). The objective of this study was to investigate the amount of pesticide residues in fruits and vegetables from South America. The results will be used when designing future control programmes for this region and taking preventive actions to minimize human health risk.

2. Materials and methods 2.1. Sampling Samples of fruits and vegetables from South America were collected as a part of the national monitoring programme for

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Table 1 Main steps in the multi-methods used. Name of method

Country

GC/LC

Detector

No. of pest.

Method reference

Sample weight

Extraction solvent

Clean up

FP017

Denmark

GC

EC-NP-IT-MS/MS

105

(Poulsen & Granby, 2000)

25

GPC

JT-1.1 QuEChERS

Estonia Finland

GC GC

EC-NP-MS MS, EC, NP

118

EN 12393-1,2,3:1998 EN 1566.2

20 10

Acetone/ethyl acetate/ cyclohexane Acetone/dichloromethane Acetonitrile

Mini-Luke

Norway

GC

MS

183

20

Acetone

M200

Sweden

75

Ethyl acetate

None

Denmark

MS/MS MS/MS MS/MS

299

FP086

GC LC LC

10

Methanol

None

JT-1.1 QuEChERS

Estonia Finland

LC LC

MS/MS MSMS

129

(Luke, Froberg, Doose, & Masumoto, 1981) (Pihlstrom, Blomkvist, Friman, Pagard, & Osterdahl, 2007) (Granby, Andersen, & Christensen, 2004) EN 12393-1,2,3:1998 EN 15662

None Dispersive SPE with PSA None

25 10

Ethyl acetate Acetonitrile

Mini-Luke

Norway

LC

MS/MS

73

Internal

10

Acetone

None Dispersive SPE with PSA None

85

pesticide residues in each of the Nordic countries including Estonia. The sampling was done according to the EU directive 2002/63/EC (EU Commission, 2002) on sampling for official control of pesticide residues. The sampling was performed by authorized personnel from the food control authorities in the countries involved. The samples were mainly taken at importers and wholesaler’s warehouses in different parts of the countries. Some samples were taken at retailers or at marked places. A total of 724 samples of 46 different fruits and vegetables from eight South American countries were collected in 2007. The samples included 680 samples of fruits and 44 samples of vegetables. 2.2. Chemical analysis Pesticide analyses were carried out at regional or central food control laboratories in each of the participating countries. The laboratories were accredited for all analytical methods used for the official control of pesticide residues in food of plant origin. The analytical scope varied between the countries both in regard to pesticides included and the analytical methods used. The samples were analysed for 170 to 326 pesticides including metabolites and degradation products using (1) GC multi-methods with ECD, NPD, ITD, MS or MS/MS detection, (2) HPLC multi-methods with MS/MS detection, and (3) single residue methods for determination of dithiocarbamates and chlormequat. Tables 1 and 2 illustrate the important steps in the analytical procedures for the multi-residue methods and single residues methods, respectively. The methods are listed including the number of pesticides covered.

2.3. Quality assurance In accordance with ISO/IEC 17025:2005 (ISO, 2005), the analytical laboratories had documented quality control procedures. The EU’s guidelines for Method validation and quality control procedures for pesticide residues analysis in food and feed, (EU Commission, 2007) were implemented as far as practical in each country. Each analytical batch included one to two spiked recovery samples. Acceptable limits for individual recovery results should be in the range of; mean recovery  2  RSD (%) and may be adjusted using repeatability and/or intra-laboratory data as described in Point 64, ‘Acceptability of analytical performance for routine recoveries’ (EU Commission, 2007). When a pesticide residue in a sample exceeds the MRL, a second quantitative analysis is carried out to verify the first result. Recovery was checked and the identity of the pesticide was confirmed by GCeMS, GCeMS/MS or LCeMS/MS. If the residue result is above the MRL, the sample is defined as an exceedence. However, before any enforcement action was taken, the analytical uncertainty was subtracted from the measured value. If the result still exceeds the MRL, enforcement action was taken in form of stop of further distribution and selling of the lot, and follow-up sampling of subsequent lots of the same origin. 3. Results and discussion The pesticides included in the analytical scope were prioritized in relation to application, toxicity and persistency. A pesticide finding in another country is also a criterion for including the pesticide in the national programme. All pesticide residues at or

Table 2 Main steps for each countries single residue methods. Name of method

Country

GC/LC

Detector

No. of pest.

Method reference

Sample weight (g)

Dithiocarbamates

UV/Vis

UV/Vis

8

EN 12396-1

200

Distillation

Dithiocarbamates

Finland/ Norway Denmark

UV/Vis

UV/Vis

100

Distillation

Dithiocarbamates

Sweden

GC

FPD(S)

5

(Juhler, Lauridsen, Christensen, & Hilbert, 1999) Pihlström P. NFA, Sweden, Not published

Chlormequat Chlormequat and mepiquat

Denmark Sweden

LC LC

MS/MS MS/MS

1 2

(Alder & Startin, 2005)

50 10 20

Extraction solvent

Tín chloride/Hydrochloric acid isooctane Methanol/Water/acetic acid IS þ methanol

Clean up

K. Hjorth et al. / Food Control 22 (2011) 1701e1706

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Table 3 Main commodities distributed on countries of origin. Argentina Apple Banana Table grapes Pear Papaya Clementine/Mandarin Lime Lemon Mango Wine grapes Passion fruit Melon, Honey melon Plum Asparagus Orange Kiwi fruit 29 other commodities

51 6 32

Brazil

Chile

88 2 19

28 1 34 15

Columbia

Ecuador

Suriname

Uruguay 3

50

35

3 20

724

8 3

13

10

24 23 5

16 4

4 11 18

16 3

13 13

6

SUM 46 commodities

1

4

18

30

9 27

157

233

141

13

2

1 11

81

45

46

above the analytical limit of quantification (LOQ) are reported. The LOQ varies between 0.01 and 0.05 mg/kg for most of the compounds. The EU pesticide residues database provides for a search tool for all the EU-MRLs set in Reg. (EC) No 396/2005 (EU-MRL database). A maximum residue limit (MRL) for pesticide residues is the maximum concentration of a pesticide residue (expressed in mg/kg) legally permitted in or on food commodities and animal feed. 3.1. Pesticide residues The 724 samples of fruits and vegetables analysed in the Nordic Project “South America” in 2007 originated from eight different countries. Brazil, Argentina and Chile were the primary contributors with 32%, 22% and 19% of the samples, respectively. Most of the samples were fruits and less than 10% were vegetable samples. Of 46 different commodities taken, the main commodities were: apples (170), bananas (89) and grapes (63 table grapes and 20 wine grapes). Table 3 shows the 16 main commodities and the countries of origin. 3.2. Percent of samples containing pesticides residues The results show that residues at or below the MRL were detected in 72% of the samples and only 19% contained no pesticide residues. In 8.4% of the samples, the residues exceeded the MRLs. The individual results for each South America country are presented in Table 4.

1

SUM 170 89 63 47 41 39 24 23 20 20 18 16 16 13 11 10 104

1 4

33 13

Peru

3.3. Origin of samples exceeding the MRLs Pesticide residues above the MRLs (both national and EU harmonized) were found in 61 samples (8.4%). Brazil was the country with most samples containing residues above the MRLs (13%), followed by Uruguay (10%) and Columbia (10%). Only 19% of the samples had no detectable residues and Peru was the country with most samples without detectable residues (52%). Most of the exceedences were found in apples (34%), papayas (21%), passion fruits (11%), and table grapes (10%) as shown in Table 5. The highest concentration of a pesticide residue was 6.6 mg/kg of iprodione in a peach sample from Chile. The sample was analysed by Sweden and exceeded the MRL with 120%. Half of the 61 samples which residues above the MRLs did not exceed the MRL with more than 100%, but three samples exceeded the MRL with more than 1000%. The highest exccedence of an MRL, 3700%, was found in a sample of passion fruits from Colombia containing dithiocarbamates. 3.4. Pesticides most often found The frequency of the ten most often found pesticides is shown in Fig. 1. A total of 83 different pesticides were found. Thiabendazole, imazalil and chlorpyrifos were the pesticide most frequently found and were detected in 212 (29.3%), 184 (25.4%) and 122 (16.9%), respectively, out of the 724 samples analysed. Thirty-seven pesticides were found with frequencies higher that 1% in the samples. In the compiled report from the 2006 monitoring of pesticide residues within EU (EU Commission, 2006) it was shown that the

Table 4 The overall results of the Nordic pesticide monitoring project in 2007. Country

No. of Samples analysed

Argentina Brazil Chile Columbia Ecuador Peru Suriname Uruguay

157 233 141 81 45 46 1 20

SUM/% Average

724

No. of samples without detectable residues

%

No. of samples with residues at, below or without MRL

24 47 14 18 11 24 0 1

15 20 10 22 24 52 0 5

125 156 120 55 32 18 1 17

139

19

524

%

No. of samples with residues above MRL

%

80 67 85 68 71 39 100 85

8 30 7 8 2 4 0 2

5 13 5 10 4 9 0 10

72

61

8.4

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Table 5 Samples of fruits and vegetables containing pesticide residues above the MRLs. Food item

Country

Pesticide residue

Result (mg/kg)

MRL (mg/kg)

Exceedence of MRL (%)

Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Apple Figs Figs Lemon Lemon Lime Mandarin Melon Melon, Water melon Melon, Water melon Melon, Water melon Oregano Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Papaya Passion fruit Passion fruit Passion fruit Passion fruit Passion fruit Passion fruit Passion fruit Passion fruit Passion fruit Peach Pear Peas with pod Plum Table grapes Table grapes Table grapes Table grapes Table grapes Table grapes Tamarillo, tree tomato Wine grapes

Argentina Argentina Argentina Argentina Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Uruguay Uruguay Brazil Brazil Argentina Argentina Brazil Peru Brazil Brazil Brazil Brazil Chile Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Brazil Ecuador Ecuador Columbia Columbia Columbia Columbia Columbia Columbia Columbia Columbia Columbia Chile Argentine Peru Argentina Chile Chile Chile Chile Peru Peru Columbia Chile

Azinphos-methyl Lambda-cyhalothrin Thiophanate-methyl Thiophanate-methyl Carbaryl Dimethoate Dimethoate Famoxadone Famoxadone Famoxadone Famoxadone Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Fenitrothion Carbaryl Carbendazim (Sum) Dithiocarbamates Parathion-methyl Imazalil Imazalil Acephate Thiabendazole Acetamiprid Acephate Methamidophos Thiabendazole Endosulfan Chlorothalonil Chlorothalonil Dimethoate Dithiocarbamates Dithiocarbamates Dithiocarbamates Dithiocarbamates Dithiocarbamates Dithiocarbamates Dithiocarbamates Thiacloprid Chlorothalonil Methomyl (Sum) Cypermethrin Cypermethrin Cypermethrin Dithiocarbamates Dithiocarbamates Imidacloprid Lambda-cyhalothrin Propamocarb Thiabendazole Iprodione Carbendazim (Sum) Fenhexamid Dicofol (Sum) Captan Captan Captan Methomyl (Sum) Methomyl (Sum) Methomyl (Sum) Dithiocarbamates Fenhexamid

0.95 0.125 1.7 1.12 0.092 0.052 0.034 0.025 0.024 0.048 0.13 0.012 0.018 0.015 0.039 0.028 0.025 0.016 0.012 0.012 0.04 0.085 0.24 1.7 0.025 5.5 5.5 0.028 5.1 0.02 0.06 0.014 0.13 0.66 0.018 0.079 0.08 0.26 0.21 0.13 0.32 0.098 0.069 0.084 0.085 0.03 0.081 0.17 0.08 0.09 1.9 0.338 0.053 0.057 0.14 0.1 6.6 0.295 0.16 0.1 0.164 0.1 0.07 0.71 0.115 0.105 0.13 0.026

0.5a 0.1 0.5 0.5 0.05a 0.02a 0.02a 0.02a 0.02a 0.02a 0.02a 0.01a 0.01a 0.01a 0.01a 0.01a 0.01a 0.01a 0.01a 0.01a 0.01a 0.05a 0.2 0.05a 0.02a 5 5 0.02a 5 0.01a 0.02a 0.01a 0.05a 0.05a 0.01a 0.01a 0.02a 0.05a 0.05a 0.05a 0.05a 0.05a 0.05a 0.05a 0.02a 0.01a 0.05a 0.05a 0.05a 0.05a 0.05a 0.05a 0.05a 0.02a 0.1a 0.05a 3 0.2 0.05a 0.02a 0.02a 0.02a 0.02a 0.05a 0.05a 0.05a 0.05a 0.01a

90 25 240 124 84 160 70 25 20 140 550 20 80 50 290 180 150 60 20 20 300 70 20 3300 25 10 10 40 2 100 200 40 160 32 80 690 300 420 320 160 540 96 38 68 325 200 62 240 60 80 3700 576 6 185 40 100 120 48 220 400 720 400 250 1320 130 110 160 160

a

Denotes MRL set at the analytical limit of quantification.

K. Hjorth et al. / Food Control 22 (2011) 1701e1706

212

Thiabendazole (F)

184

Imazalil (F) 122

Chlorpyrifos (I)

104

Carbendazim, sum (F) Pesticide name

1705

80

Iprodione (F)

76

Azinphos-methyl (I) 45

Prochloraz (F) Fenhexamid (F)

44

orto-Phenylphenol (F)

42

Lambda-cyhalothrin (I)

42 592

73 other pesticides 0

100

200

300

400

500

600

Number of samples

F = Fungicide I = Insecticide

Fig. 1. Pesticides most common found in the samples from South America.

ten pesticides most often found in fruits and vegetables were: imazalil, thiabendazole, procymidone, benomyl group, chlorpyriphos, iprodione, cyprodinil, chlorpyrifos-methyl, imidacloprid, and maneb group. Four of these, imazalil, thiabendazole, chlorpyriphos and iprodione were also among the most often found pesticides in this project (see Fig. 1). Furthermore, seven out of the ten pesticides were fungicides and the others were insecticides. 3.5. Multiple residue findings Many samples contained several pesticide residues. A total of 1543 pesticide residues were found in the 585 samples containing residues. An overview of the number of residues per sample is shown in Table 6. The results in Table 6 show that 416 samples (71% of positive samples) contained more the one pesticide residue. About 13% of the samples contained five or more pesticide residues. The samples with highest number of pesticide residues were two samples of table grapes both with nine pesticide residues. Apples and table grapes, one sample of each, contained eight pesticide residues. The apple sample originated from Uruguay and the three table grapes samples were all from Chile. Even though these samples contained a large number of pesticide residue, only three of the four samples contained residues above the MRLs. Possible combination effects as a result of exposure to more than one pesticide is not a very well documented area. A growing demand to illuminate if these circumstances will change the current risk assessment, which are based on the assessment of an individual compound basis. 3.6. Acute intake and risk assessment The acute intake has been calculated for those pesticides for which an acute reference dose (ARfD) has been set, either by EFSA (European Food Safety Authority) or by JMPR (Joint Meeting on Pesticide Residues). The calculations have been done using the UK

Table 6 Number of pesticide residues in an individual sample. No. of findings

0

1

2

3

4

5

6

7

8

9

No. of samples %

139 19

169 23

143 20

113 16

82 11

43 6

21 3

10 1.4

2 0.3

2 0.3

model (PSD, 1998). For apples and pears a variability factor of seven and for table grapes a factor of five has been used in the calculations. In three samples the ARfD was exceeded. Methomyl, 0.71 mg/kg in a sample of table grapes from Chile, resulted in the highest intake, 1733% of the ARfD for toddler. The other two samples were 0.30 mg/kg carbendazim in a sample of pear, and 0.13 mg/kg lambda-cyhalothrin in a sample of apple both from Argentina. These two samples resulted in 115% ARfD for toddler. After notification, the EU Commission informed the Member States through the Rapid Alert Food Information Exchange System (RASFF) about this finding. 3.7. Pesticide residues in apples Residues found in the 2007 monitoring of apples from South America were compared with residues found in apples produced in the Nordic countries (Fødevarestyrelsen, 2008; Livsmiddelverket, 2008; Matttilsynet, 2008). Apples were chosen as they are commercially grown in the Nordic countries as well as in South America. In general, apples produced in the Nordic countries contained less pesticide residues than apples produced in South America (Table 7). In apples produced in the Nordic countries, pesticide residues were found in approximately 40% of the samples, whereas almost 73% of the South America produced apples contained residues. The percentages of samples with residues above the MRL was about 2.5 times higher for the apple samples from South America compared with those from the Nordic countries. Table 7 also includes results for apples, analysed within the 2004 EU co-ordinated monitoring program for pesticide residues (EU Commission, 2006). Apple was one of the eight commodities to be analysed for 47 pesticides by 22 EU Member States. These apple samples originated both from imports to EU and production in the EU countries. The percentage of apple samples with residues at or below the MRL from the EU monitoring program is about the same compared with the samples from South America (Nordic project), 59% and 61%, respectively. However, differences are obvious when comparing the percentage of samples with residues above the MRL. This figure is much lower for the EU monitoring program (1.8%) compared to South America samples (12%). It should be noted that the pesticide scope for the EU monitoring program is limited compared with the scope for this project and the National programmes within the Nordic countries.

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K. Hjorth et al. / Food Control 22 (2011) 1701e1706

Table 7 Pesticide residues in apples from different group of countries. Country

No. of Samples analysed

No. of samples without detectable residues

%

No. of samples with residues at, below or without MRL

%

No. of samples with residues above MRL

%

South America Nordic Countriesa EU monitoring 2004

170 98 3 133

44 59 1229

26 60 39

105 34 1848

61 35 59

21 5 56

12 5 1.8

a

Average of pesticide residues in apples on the Danish, Norwegian and Swedish market.

4. Conclusion In a Nordic project in 2007, a total of 724 samples of 46 different fruits and vegetables from eight South American countries were collected and the pesticide residues were analysed. Residues at or below the MRL were detected in 72% of the samples and 8.4% contained residues above the MRLs. Out of 83 different pesticides detected in the samples, the fungicide thiabendazole was most frequently found (29%). Thirty-seven pesticides were found with frequencies higher that 1% in the samples. The results show that residues are more common and the frequency of exceedences of the MRLs is higher in apples from South America compared to apples produced in the Nordic countries. The results also emphasize the need for continuous monitoring of pesticide residues, especially in imported fruits and vegetables. References Alder, L., & Startin, J. R. (2005). Determination of chlormequat and mepiquat in foods by liquid chromatography/mass spectrometry or liquid chromatography/ tandem mass spectrometry: interlaboratory study. Journal of AOAC International, 88(6), 1762e1776. Ecobichon, D. J. (2001). Pesticide use in developing countries. Toxicology,160(1e3), 27e33. EU Commission. (2002). Commission directive 2002/63/EC of 11 July 2002 e Establishing community methods of sampling for the official control of pesticide residues in and on products of plant and animal origin and repealing directive 79/700/EEC. http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri¼CELEX:32002L0063: en:NOT. Accessed 30.10.09. EU Commission. (2006). Monitoring of pesticide residues in products of plant origin in the European Union, Norway, Iceland and Liechtenstein report 2004. European Commission, Food and Veterinary Office. http://ec.europa.eu/food/fvo/ specialreports/pesticides_index_en.htm. Accessed 30.11.09.

EU Commission. (2007). Method validation and quality control procedures for pesticide residues analysis in food and feed. http://ec.europa.eu/food/plant/protection/ resources/publications_en.htm. SANCO/2007/3131. Accessed 30.11.09. EU pesticide residues database. EU pesticide residues database for all the EU-MRLs. Available at http://ec.europa.eu/food/plant/protection/pesticides/database_ pesticide_en.htm. Fødevarestyrelsen. (2008). Pesticidrester i fødevarer 2007 e Resultater fra den danske pesticidkontrol. http://www.foedevarestyrelsen.dk/Publikationer/Alle_ publikationer/2008/003.htm. Accessed 01.11.09. Granby, K., Andersen, J. H., & Christensen, H. B. (2004). Analysis of pesticides in fruit, vegetables and cereals using methanolic extraction and detection by liquid chromatographyetandem mass spectrometry. Analytica Chimica Acta, 520(1e2), 165e176. International Standard Organization. (2005). ISO/IEC 17025:2005 General requirements for the competence of testing and calibration laboratories. Juhler, R. K., Lauridsen, M. G., Christensen, M. R., & Hilbert, G. (1999). Pesticide residues in selected food commodities: results from the Danish National Pesticide Monitoring Program 1995e1996. Journal of AOAC International, 82(2), 337e358. Livsmiddelverket. (2008). The Swedish monitoring of pesticide residues in food of plant Origin:2007. Rapport 5, 2008. Uppsala, Sweden: National Food Administration. http://www.slv.se/en-gb/group3/Publications/Pesticides-residues-infood/ Accessed 14.11.09. Luke, M., Froberg, J., Doose, G., & Masumoto, H. (1981). Journal of the Association of Official Analytical Chemists, 64, 1178e1195. Matttilsynet. (2008). Rester av plantevernmidler i vegetabilske næringsmidler 2007. http://matportalen.no/artikler/2008/7/1215426702.27. Accessed 15.11.09. Pihlstrom, T., Blomkvist, G., Friman, P., Pagard, U., & Osterdahl, B. G. (2007). Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection. Analytical and Bioanalytical Chemistry, 389(6), 1773e1789. Poulsen, M. E., & Granby, K. (2000). Validation of a multi residue method for analysis of pesticides in fruit, vegetables and cereals by a GCeMS ion trap system. In Anonymous principles and practices of method validation (pp. 108e119). Cambridge: Royal Society of Chemistry. PSD. (1998). New UK technical policy on the estimation of acute dietary intakes of pesticides. York, UK: PSD. 13 January 1998.