Fromberg, Arvid

Poulsen, Mette Erecius

Online Research Database In Technology

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Downloaded from orbit.dtu.dk on: Dec 20, 2017Pesticide residues in feeding stuff for laying hens – results from samples collected in20 EU member statesPoulsen, Mette Erecius; Fromberg, ArvidPublication date:2012Document VersionPublisher's PDF, also known as Version of recordLink back to DTU OrbitCitation (APA):Poulsen, M. E., & Fromberg, A. (2012). Pesticide residues in feeding stuff for laying hens – results from samplescollected in 20 EU member states. Poster session presented at 9th European Pesticide Residue Workshop ,Vienna, Austria.Pesticide residues in feeding stuff for laying hens – results from samples collected in 20 EU member states Mette Erecius Poulsen and Arvid Fromberg DTU National Food Institute, Moerkhoej Bygade 19, DK-2860 Soeborg, Denmark; e-mail : mpou@food.dtu.dk 1 EURL-CF: EU Reference Laboratory for pesticide Residues in Cereals and Feeding stuff . DTU National Food Institute, Moerkhoej Bygade 19, DK-2860 Soeborg, Denmark   e-mail :  crlcereals@foood.dtu.dk,  www.crl-pesticides.eu   Introduction: The EURL-AO and EURL-CF1 has initiated a study on ‘Pesticide residues in feed for laying hens and pesticide residues in eggs’. The aim of the project is to detect pesticide residues in the eggs when known pesticides residues are present in the feed provided for the laying hens. Included in the project was a survey on pesticide residues in the feeding stuff for laying hens in EU. The study will enable the estimation of the risk for consumers in relation to pesticide residues in eggs. To perform a survey to cover feeds in EU the NRL-CFs were asked to collect 2 samples of feeds for laying hens from local suppliers. 20 member states shipped 42 samples for analysis at the EURL-CF. The samples were mixed feeds with cereals and/or fatty matrices of plant origin, like soya/rape, vitamins and minerals. Analytical method: The homogenised sample was extracted by a Dionex ASE-300 ASE with acetone:hexane. The extract was concentrated into ethyl-acetat:cyclohexane and cleaned-up using Gilson ASPEC with a SX-3 GPC. Additional clean-up was performed after concentration into ethyl acetate, using NH2 SPE columns with dichloromethane as eluent. The extract was concentrated and analysed by GC/MS/MS and LC/MS/MS. The SPE clean-up step caused some decrease in recoveries but without SPE clean-up the GC chromatography deteriorated significantly for a part of the eluting peaks, resulting in bad peak shape and shift in retention time, see Figure 1. Figure 1. Chromatogramme of feed extract after CPC clean up and CPC and SPE clean-up Table 1. Pesticide residues in 42 feed for laying hens samples collected in 20 EU member states Validation: A validation was performed according to SANCO/12495/2011 on a mixture of feed samples, which were composed by different kind of cereals, oils, vitamins and minerals. Five parallel extractions at two concentration levels (0.01 and 0.1 mg/kg) were analysed. Recoveries between 70-120% were obtained for 90 GC/MS/MS and 48 LC/MS/MS compounds. Additionally, 25 compounds resulted in recoveries between 60-70% or 120-140% and 47 compounds below 50%. The LOQs obtained for most the validated compounds were between 0.01-0.02 mg/kg. In parallel with the analysis of the feed samples, EUPT-C6 and EUPT test materials were analysed twice. All validated pesticide residues were detected and z-scores were between ±2.0 (median -1.0).  Results: Pesticides residues were found in 31 of the 42 samples. In total 67 residues was detected at levels between 0.009 and 1.03 mg/kg, see Table 1. Twelve different pesticides were detected, mainly organo phosphorous pesticides (48 %). The most frequently found pesticides were pirimiphos-methyl (0.012-1.03 mg/kg) and 2-phenyl-phenol (0.009-0.107 mg/kg), both pesticides used post-harvest, the latter probably used for packing materials. The feed with the highest residues, pirimiphos-methyl, 1.03 mg/kg contained 62 % oat, wheat and maize for which MRL are 5 mg/kg. If the pirimiphos-methyl originated from the cereals in the feed, the MRL were not exceeded.  Conclusions: Validation of a method for mixed feeding stuff was performed successfully for 146 compounds. Analysis of 42 samples from 20 EU member states resulted in 67 findings of 12 different pesticides in 31 of the feed samples. None of the sample exceeded the MRLs, if the residues originated from the constituent with the highest MRL. GPC and SPE clean up GPC clean up Country 2-PhenylphenolBoscalidChlorpyrifosChlorpyrifos-methylCypermethrinDeltamethrinDicloranEndosulfan-alphaIsoprothiolaneMalathionPirimiphos-methylProcymidone1 0.055 0.6521 0.096 0.1052 0.050 0.836 0.1022 0.018 0.046 0.159 0.1013 0.0163 0.025 0.012 0.1213 0.0183 0.0154 0.0744 0.0434 0.014 0.012 0.0145 0.014 0.013 0.0575 0.019 0.042 0.0136 0.061 0.1026 0.010 0.01277889 0.057 0.010 0.0389 0.014 0.028 0.01210 0.01410 0.016 0.014 0.01211 0.01511 0.01412121313 0.009 0.0451414 0.0131515 0.02216 0.010 0.012 0.015 0.461161717 0.057 0.27518 0.10719 0.012 0.060 1.03519 0.015 0.03720 0.022 0.018 0.049 0.015 0.11620 0.010 0.059No of residues 17 1 3 9 6 4 3 2 1 2 18 1Minimum 0.009 0.014 0.010 0.012 0.013 0.028 0.013 0.012 0.010 0.159 0.012 0.014Maximum 0.107 0.014 0.018 0.060 0.096 0.057 0.050 0.121 0.010 0.836 1.03 0.014

Pesticide residues in feeding stuff for laying hens – results from samples collected in 20 EU member states

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Pesticide residues in feeding stuff for laying hens – results from samples collected in 20 EU member states

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