Clean-up Procedure Development and Method Validation for Pesticide Residues Analysis in Carrots
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Clean-up Procedure Development and Method Validation for Pesticide Residues Analysis in Carrots Márcia H. S. Kurz 1 & Juliana L. da S. Batista 1 & Lenise G. de Oliveira 1 & Rodrigo Hoff 2 & Manoel L. Martins 1 & Fábio F. Gonçalves 1 Received: 9 April 2018 / Accepted: 6 September 2018 # Springer Science+Business Media, LLC, part of Springer Nature 2018
Abstract In this work, a method was developed, validated, and applied to determination of ten pesticide residues (trifluralin, carbofuran, chlorothalonil, pendimethalin, captan, tebuconazole, pyraclostrobin, difenoconazole, deltamethrin, and azoxystrobin), from seven distinct classes, in carrot samples, employing a QuEChERS procedure for the analyte extraction and gas chromatography coupled to mass spectrometry (GC-MS) for quantification. The dispersive clean-up step was optimized using different sorbents at different concentrations and mixings. The method proved to be efficient and robust, showing recoveries in the range 72–117%, and RSD ranging from 4.9 to 16.6% (except for chlorothalonil and captan) at fortification levels of 45, 90, 180, and 450 μg kg−1 with seven replicates analyzed for each level (n = 28). Chlorothalonil and captan could not be validated due to analyte stability problems. Detection limits were between 15 and 45 μg kg−1, and the quantification limits were between 45 and 90 μg kg−1. The method was successfully applied to real samples. Keywords Pesticide residues . Carrot . QuEChERS . Clean-up . GC-MS
Introduction Carrot (Daucus carota L.) is a vegetable of the Apiaceae family, which has great socioeconomic importance for Brazilian agrobusiness and is among the five most consumed vegetables in Brazil (Guimarães et al. 2012). Consume of carrot stands out because it is one of the main natural sources of carotenoids. The β-carotene, representing 45–70% of total carotenoids from carrots, is responsible for a variety of beneficial effects on human health. It acts in the preservation and maintenance of mucous membranes, skin and bones, and when associated with vitamin C, also present in carrots, contributes to reduce the risk of cataract (Fariña et al. 2007). Carrot is very rich in other vitamins such as B1 and B2, which help the regulation of the nervous system and * Márcia H. S. Kurz [email protected] 1
Escola de Química e Alimentos, Universidade Federal do Rio Grande, Santo Antônio da Patrulha, RS 95500-000, Brazil
2
Laboratório Nacional Agropecuário – LANAGRO/RS, Ministério da Agricultura, Pecuária e Abastecimento do Brasil, Estrada da Ponta Grossa 3036, Porto Alegre, RS, Brazil
digestive tract function (Gallagher 2005). For humans, just 100 g of carrots are sufficient to meet the daily needs of vitamin A (CEASA 2018). In contrast, exposure even to small amounts of pesticides can cause adverse and irreversible effects on human health. According to the National Health Surveillance Agency (ANVISA 2018a), 25 compounds have maximum residue limits (MRLs) established for use in carrot. Moreover, carrot edible parts are precisely those ones immerse
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