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1

Zastosowanie metody QuEChERS do analizy pozostałości pestycydów w pomidorach za pomocą GC-NPD/ECD

100%

Raczkowski M., Holodynska A., Nowacka A., Gnusowski B.

Progress in Plant Protection

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2011

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tom 51

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nr 2

The Quick Easy Cheap Effective Rugged and Safe pesticide multiresidue method (QuEChERS) has been validated for extraction of two fungicides: azoxystrobin and chlorothalonil, which are frequently detected pesticides in Polish tomato samples. The homogenized samples (10 g) were spiked with a small volume of an appropriate standard mixture solution and shaken with acetonitrile (10 ml). As a slight modification, the obtained mixtures were frozen to save volatile pesticides before addition of salt mixture, consisting of anhydrous magnesium sulphate (4 g), sodium chloride (1 g), disodium hydrogen citrate sesquihydrate (0.5 g), and trisodium citrate dihydrate (1 g). After centrifugation an aliquot of the acetonitrile phase was transferred into a centrifugation tube containing a mixture of anhydrous magnesium sulphate and PSA sorbent (0.9 g). After purification with PSA, the extracts were re-acidified by adding 50 μL of the 5% formic acid solution. The extracts were transferred to the glass tubes and carefully evaporated to the dryness. The last step was adding acetone/hexane solution. A mixture of azoxystrobin and chlorothalonil, amenable to gas chromatography (GC), was quantitatively recovered from spiked tomato samples and determined using gas chromatography with nitrogen phosphorus detector and electron capture detector (GC–NPD/ECD). The spiking levels for the recovery experiments were: 0.02, 0.2 and 2.0 mg/kg for GC–NDP/ECD analyses. Mean recoveries mostly ranged between 70 and 120% (83.7% on average), relative standard deviations (RSD) were generally below 20% (9.8% on average). Based on the results, this methodology has been proven to be highly efficient and suitable for determination of azoxystrobin and chlorothalonil in tomato samples.

2

Pesticide residues in crops produced in north-western Poland

64%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Raczkowski M., Holodynska A., Frackowiak D., Swoboda W.

Progress in Plant Protection

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2012

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tom 52

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nr 4

In 2011, 262 crop samples, originating from farms located in five voivodeships of north‐western Poland, were tested for the presence of pesticide residues. Studies were conducting in framework of official control and included 23 products and 230 compounds. Several multi‐residue methods based on gas chromatography and high performance liquid chromatography (GC‐ECD/NPD, GC‐MS/MS, HPLC‐UV/PDA, LC‐MS/MS) and one single‐residue method based on spectrophotometric analysis were used for determination of pesticide residues. Totally, 26 compounds were detected in 29.0% of analysed samples. Exceedances of maximum residue levels (MRLs) were found in 0.4% of analysed samples, while the use of unapproved plant protection products in 4.2% of the samples. Pesticide residues were found mostly in samples of apples (84.6%), carrots (56.0%) and potatoes (50.0%). The frequency of their occurrence in the samples taken from individual voivodeships has differed from the average for the entire study area and ranged from 15.9–39.6%, and was the highest in food products from Kujawsko‐pomorskie Voivodeship, while the lowest from Wielkopolskie Voivodeship.

3

Pesticide residues in Polish crops (2011)

39%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Raczkowski M., Holodynska A., Frackowiak D., Wojcik A., Ziolkowski A., Przewozniak M., Swoboda W., Rzeszutko U., Domanska I., Jurys J., Lozowicka B., Kaczynski P., Rutkowska E., Jankowska M., Hrynko I., Szpyrka E., Rupar J., Rogozinska K., Kurdziel A., Slowik-Borowiec M., Szala J., Szponik M., Michel M.

Progress in Plant Protection

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2012

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tom 52

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nr 4

In 2011, a total of 977 samples of domestic crops were tested in the official control of pesticide residues carried out by the Institute of Plant Protection – National Research Institute. The samples were taken randomly by the staff of Plant Health and Seed Inspection at production sites in the whole country. The monitoring programme covered 230 compounds and 38 products. 126 samples of fruit, 484 samples of vegetables, 346 samples of cereals and 21 samples belonging to other products groups were analysed. Residues of 43 compounds were detected in 21.7% of the samples. Violations of MRLs were found in 0.6% of analysed samples, while the unauthorised plant protection product use in 2.5% of samples tested. Pesticide residues were detected in 58.7% of fruit samples, 23.8% of vegetable samples and 4.9% of cereal samples and in 28.6% of other samples. They were found most often in samples of apples (60.5%), tomatoes (52.6%), sweet peppers (50.0%) and carrots (42.1%). Most of the residues detected in twenty five commodities were fungicides and insecticides, and their percentages from 335 findings were equal respectively to 63.9% and 32.5%. The most commonly found were residues of chlorothalonil in tomatoes (31.6%), chlorpyrifos in carrots (28.9%), prochloraz in mushrooms (26.1%), and dithiocarbamates in apples (25.4%), potatoes (24.2%) and tomatoes (21.1%).

4

Pozostałości środków ochrony roślin w płodach rolnych (rok 2008)

39%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Wojcik A., Raczkowski M., Holodynska A., Barylska E., Ziolkowski A., Chmielewska E., Rzeszutko U., Giza I., Lozowicka B., Kaczynski P., Rutkowska E., Szpyrka E., Rupar J., Rogozinska K., Machowska A., Slowik-Borowiec M., Kuzmenko A., Szala J.

Progress in Plant Protection

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2009

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tom 49

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nr 4

5

Pozostałości środków ochrony roślin w płodach rolnych (rok 2010)

39%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Raczkowski M., Holodynska A., Frackowiak D., Wojcik A., Ziolkowski A., Rzeszutko U., Domanska I., Jurys J., Lozowicka B., Kaczynski P., Rutkowska E., Jankowska M., Hrynko I., Szpyrka E., Rupar J., Rogozinska K., Kurdziel A., Slowik-Borowiec M., Michel M., Kuzmienko A., Szala J.

Progress in Plant Protection

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2011

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tom 51

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nr 4

In total, 1351 samples of fresh fruit, vegetables and agricultural crops of Polish origin were analysed in 2010 in five laboratories of the Institute of Plant Protection – National Research Institute. The monitoring programme covered 52 commodities and 143 pesticides including some isomers and breakdown products. Residues of 48 compounds, mainly fungicides (26), were detected. The percentage of samples with residues at or below the MRL was 24.2%. In 74.8% of the samples no residues were found. Violations of MRLs were stated in 1.0% of the samples, while the use of non-approved pesticides in 2.7% of the samples tested. Pesticide residues were detected most often in samples of fruit (41.7%), especially in samples of gooseberries (70.0%), cherries (61.3%) and apples (52.4%). Samples of vegetables, as well as agricultural crops were less contaminated with pesticide residues. However, a high sample percentage of tomatoes grown under cover (43.1%) or in the field (60.3%) contained pesticide residues.

6

Pozostałości środków ochrony roślin w płodach rolnych (rok 2009)

39%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Wojcik A., Raczkowski M., Holodynska A., Barylska E., Ziolkowski A., Chmielewska E., Rzeszutko U., Giza I., Jurys J., Lozowicka B., Kaczynski P., Rutkowska E., Jankowska M., Szpyrka E., Rupar J., Rogozinska K., Kurdziel A., Slowik-Borowiec M., Kuzmienko A., Szala J., Sadlo S.

Progress in Plant Protection

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2010

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tom 50

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nr 4

A total of 1 352 samples of fresh fruit, vegetables and arable crops of Polish origin were analysed in 2009 in five laboratories of the Institute of Plant Protection – National Research Institute. The monitoring programme covered 54 commodities and 132 pesticides including some isomers and breakdown products. Residues of 43 pesticides, mainly fungicides (24), were detected in 24.5% of samples analysed. Percentage of the samples without pesticide residues was equal to 75.5%. The residues lower than MRLs contained 23.1% of samples analysed. Violations of MRLs were found in 1.4% of the samples. The usage of not approved pesticides were stated in 3.3% of the samples analysed. Residues were detected in 43.3% of fruit samples especially in samples of raspberries (56.4%), apples (50.4%), sour cherries (48.5%), strawberries (44.8%), but the highest percentage of pesticide residues (66.7%) was found both in samples of greenhouse tomatoes and in the samples of celeriac. The samples of other products were less contaminated. Residues of dithiocarbamates were most often detected, in 13.4% of the samples. Four further pesticides captan, linuron, chloropiryfos and carbendazim were found in 8.7%, 5.1%, 4.1% and 4.1% of samples analysed respectively, while the other compounds in less than 2.6% of samples analysed.

7

Pesticide residues in agricultural crops (2013)

39%

Nowacka A., Gnusowski B., Walorczyk S., Drozdzynski D., Raczkowski M., Holodynska A., Frackowiak D., Ziolkowski A., Przewozniak M., Rzeszutko U., Domanska I., Pszczolinska K., Lozowicka B., Kaczynski P., Rutkowska E., Jankowska M., Hrynko I., Szyrka E., Rupar J., Matyaszek A., Kurdziel A., Podbielska M., Slowik-Borowiec M., Szponik M.

Progress in Plant Protection

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2015

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tom 55

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nr 4

Ograniczanie wyników

Zastosowanie metody QuEChERS do analizy pozostałości pestycydów w pomidorach za pomocą GC-NPD/ECD

Pesticide residues in crops produced in north-western Poland

Pesticide residues in Polish crops (2011)

Pozostałości środków ochrony roślin w płodach rolnych (rok 2008)

Pozostałości środków ochrony roślin w płodach rolnych (rok 2010)

Pozostałości środków ochrony roślin w płodach rolnych (rok 2009)

Pesticide residues in agricultural crops (2013)