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Kaczynski P.,Institute of Plant ProtectionNational Research Institute | Lozowicka B.,Institute of Plant ProtectionNational Research Institute
Food Analytical Methods | Year: 2016

A one-step quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach to extraction and cleanup in multiresidue pesticide analysis is presented for the first time. The experiment was designed to detect 23 sulfonylurea herbicides in a complex cereal matrix. The challenge was to choose the optimal conditions of one-step extraction and cleanup. Chitin, diatomaceous earth, and octadecyl were investigated as cleanup sorbents. Chitin, citrate buffer, and 1 % formic acid in acetonitrile yielded the best results. The effectiveness of sulfonylureas extraction was evaluated at three different spiking levels (0.005, 0.05, and 0.5 mg kg−1) in wheat, rye, and oat using liquid chromatography–tandem mass spectrometry. The one-step QuEChERS provided recoveries in the 70–120 % range for 23 sulfonylureas in all cereal matrices. Matrix effects were evaluated and were not significant for all herbicides, showing suppression or enhancement (between −19 and 13 %). Precision, calculated as relative standard deviation (RSD), was below 20 %. A linear dependence was observed in the range of 0.005–2.0 mg kg−1, and the correlation coefficient was R2 > 0.999. Expanded measurement uncertainty was estimated to be between 9 and 24 %, on average. The validated method was employed in analysis of 89 real grain samples. © 2016 The Author(s)

Cholewa R.,University of Life Sciences in Poznań | Beutling D.,Free University of Berlin | Budzyk J.,Zaklad Higieny Weterynaryjnej | Pietrzak M.,University of Life Sciences in Poznań | Walorczyk S.,Institute of Plant ProtectionNational Research Institute
Journal of Environmental Science and Health - Part B Pesticides, Food Contaminants, and Agricultural Wastes | Year: 2015

A highly selective and sensitive method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) to identify and quantify persistent organochlorine pesticides, (18 compounds including primary compounds and metabolites), in animal internal organs (kidneys, liver, and brain) has been developed. Tandem mass spectrometric conditions were individually optimized for each target compound in Multiple Reaction Monitoring (MRM) mode to obtain maximum sensitivity. Prior to instrumental analysis, a sample preparation method based on matrix solid phase dispersion (MSPD) followed by acidic digestion with sulfuric acid to reduce matrix co-extractives was employed. Analyses of real samples were carried out on coypus (Myocastor coypus) from the autumn slaughter of 19 animals. In the analyzed samples, three of the target compounds, namely DDE-pp′ (DDT metabolite), HCB and lindane, were detected. Their concentration levels fell in the ranges of 0.003–0.007, 0.003–0.025, and 0.003–0.021 mg kg−1 (0.005, 0.010, and 0.010 mg kg−1 on average) in the case of DDE-pp′, HCB and lindane, respectively. Although low quantities of organochlorine pesticides do not pose an immediate danger to consumers' health, they should be of public health concern considering long-term, low-dose exposure. © 2015, Copyright © Taylor & Francis Group, LLC.

Walorczyk S.,Institute of Plant ProtectionNational Research Institute | Kopec I.,Institute of Plant ProtectionNational Research Institute | Szpyrka E.,Institute of Plant ProtectionNational Research Institute
Food Analytical Methods | Year: 2015

A multiresidue method for the analysis of over 140 multiclass pesticides in fruiting vegetables, based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation procedure followed by gas chromatography-tandem mass spectrometry (GC-MS/MS), was established. In the validation study, the overall recoveries from spiked samples were 102 ± 7, 95 ± 7, and 95 ± 7 % with RSD values of 7 ± 3, 7 ± 4, and 7 ± 3 % at the spiking levels of 0.01, 0.05, and 0.5 mg kg−1, respectively, demonstrating fitness for purpose of the method. The limit of quantification (LOQ) was 0.01 mg kg−1 for more than 90 % of the target compounds. The analysis of over 300 samples of tomatoes, sweet peppers, and cucumbers was carried out in 2006–2014. Of these samples, 52 % contained pesticide residues but the results of the assessment of dietary exposure supported the conclusion that the presence of pesticide residues was unlikely to have a negative effect on the health of consumers. Although some of the pesticides detected in years 2006–2009 are no longer approved in the European Union member countries (namely endosulfan, oxadixyl, procymidone, propargite, and tolylfluanid), the consumer dietary exposure was low and did not exceed 12 % of the acceptable daily intake (ADI) considering both adults’ and children’s diet. Regarding short-term exposure (acute), in only one case of procymidone in sweet pepper, the acute reference dose (ARfD) for children was exceeded by 139.6 % of the ARfD. © 2015 Springer Science+Business Media New York

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