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Monitoramento de agrotóxicos em áreas irrigadas por pivô central na microbacia do Tijunqueiro, município de Morrinhos, Goiás; Pesticides monitoring in irrigated areas by central pivot in the Tijunqueiro Watershed municipality of Morrinhos, Goias

Rocha, Aderbal Almeida
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 12/08/2011 PT
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16.88%
A importância dos agrotóxicos para o sistema de produção agrícola é indiscutível, uma vez que constituem parte dos insumos básicos. No entanto, é fundamental que sejam adequadamente utilizados para a preservação da qualidade não só do produto cultivado, mas também dos próprios recursos naturais, especialmente o solo e a água. Neste estudo, foi realizado o monitoramento dos agrotóxicos utilizados em lavouras irrigadas por pivô central, na microbacia do Tijunqueiro, município de Morrinhos, estado de Goiás, que apresentaram potencial de contaminação ambiental (critérios da Agência de Proteção Ambiental dos Estados Unidos EPA, índice GUS Groundwater Ubiquity Score, método GOSS e do Instituto Brasileiro de Recursos Naturais Renováveis e não Renováveis IBAMA) e sensíveis ao espectrômetro de massas (LC-MS/MS Cromatografia líquida acoplada ao espectrômetro de massas), no período entre fevereiro de 2009 e setembro de 2010, em amostras de águas superficial e subsuperficial, peixes e sedimentos. Os ingredientes ativos (agrotóxicos) monitorados foram: acefato, atrazina, azoxistrobina, buprofezina, carbofurano, ciproconazole, clorpirifós, difeconazole, diurom, imidacloprido, malationa, metamidofós, metolacloro...

Qualitative aspects and validation of a screening method for pesticides in vegetables and fruits based on liquid chromatography coupled to full scan high resolution (Orbitrap) mass spectrometry

Mol, Hans G. J.; Zomer, Paul; de Koning, Maarten
Fonte: Springer-Verlag Publicador: Springer-Verlag
Tipo: Artigo de Revista Científica
EN
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16.58%
The analytical capabilities of liquid chromatography with single-stage high-resolution mass spectrometry have been investigated with emphasis on qualitative aspects related to selective detection during screening and to identification. The study involved 21 different vegetable and fruit commodities, a screening database of 556 pesticides for evaluation of false positives, and a test set of 130 pesticides spiked to the commodities at 0.01, 0.05, and 0.20 mg/kg for evaluation of false negatives. The final method involved a QuEChERS-based sample preparation (without dSPE clean up) and full scan acquisition using alternating scan events without/with fragmentation, at a resolving power of 50,000. Analyte detection was based on extraction of the exact mass (±5 ppm) of the major adduct ion at the database retention time ±30 s and the presence of a second diagnostic ion. Various options for the additional ion were investigated and compared (other adduct ions, M + 1 or M + 2 isotopes, fragments). The two-ion approach for selective detection of the pesticides in the full scan data was compared with two alternative approaches based on response thresholds. Using the two-ion approach, the number of false positives out of 11,676 pesticide/commodity combinations targeted was 36 (0.3 %). The percentage of false negatives...

Decrease of Pirimiphos-Methyl and Deltamethrin Residues in Stored Rice with Post-Harvest Treatment

Yu, Chuanshan; Li, Yanjie; Zhang, Qian; Zou, Nan; Gu, Kejia; Li, Xuesheng; Pan, Canping
Fonte: MDPI Publicador: MDPI
Tipo: Artigo de Revista Científica
EN
Relevância na Pesquisa
16.58%
A modified quick, easy, cheap, effective, rugged (QuEChERS) method with multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid phase extraction (r-DSPE) material was applied to the analysis of pirimiphos-methyl and deltamethrin residues in stored rice. Two dustable powder (DP) formulations (2% pirimiphos-methyl and deltamethrin DP; 5% pirimiphos-methyl DP) were applied in simulated storehouse trials in the lab. The residues and dissipation of the two pesticides in stored rice were investigated. Slow dissipation of both pesticides was observed in stored rice. The half-lives of pirimiphos-methyl were 23.9–28.9 days, and those of deltamethrin were 23.9–24.8 days. Residues of pirimiphos-methyl from application rates of 4.5–6.75 a.i. mg/kg (active ingredient milligram per kilogram) and 10–15 a.i. mg/kg were 1.6–3.8 mg/kg and 3.0–4.5 mg/kg at 60 days Pre-harvest Interval (PHI). Residues of deltamethrin from an application rate of 0.5–0.75 a.i. mg/kg were 0.13–0.14 mg/kg at 60 days PHI. Both pesticides residues were below the Maximum Residue Limits (MRLs) established by the Codex Alimentarius Commission (CAC). Therefore, at the recommended dosages they are safe for use on stored rice.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

Silva, Catarina L.; Haesen, Nathaly; Câmara, José S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em /10/2012 ENG
Relevância na Pesquisa
37.33%
This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds. The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ)...