Título:	Analytical method validation to evaluate dithiocarbamates degradation in biobeds in South of Brazil.
Autoria:	VARELI, C. S. PIZZUTTI, I. R. GEBLER, L. CARDOSO, C. D. GAI, D. S. H. FONTANA, M. E. Z.
Afiliação:	Catiucia S. Vareli, UFSM – Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Campus, 97105-900 Santa Maria, RS, Brazil Ionara R. Pizzutti, a UFSM – Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Campus, 97105-900 Santa Maria, RS, Brazil LUCIANO GEBLER, CNPUV Carmem D. Cardoso, a UFSM – Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Campus, 97105-900 Santa Maria, RS, Brazil Daniela S.H. Gai, a UFSM – Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Campus, 97105-900 Santa Maria, RS, Brazil Marlos E.Z. Fontana, a UFSM – Federal University of Santa Maria, Chemistry Department, Center of Research and Analysis of Residues and Contaminants (CEPARC), Campus, 97105-900 Santa Maria, RS, Brazil.
Ano de publicação:	2018
Referência:	Talanta, v. 184, p. 202-209, 2018.
Conteúdo:	In order to evaluate the efficiency of biobeds on DTC degradation, the aim of this study was to apply, optimize and validate a method to determine dithiocarbamate (mancozeb) in biobeds using gas chromatography-tandem mass spectrometry (GC-MS). The DTC pesticide mancozeb was hydrolysed in a tin (II) chloride solution at 1.5% in HCl (4 mol L−1 ), during 1 h in a water bath at 80 °C, and the CS2 formed was extracted in isooctane. After cooling, 1 mL of the organic layer was transferred to an auto sampler vial and analyzed by GC-MS. A complete validation study was performed and the following parameters were assessed: linearity of the analytical curve (r2 ), estimated method and instrument limits of detection and limits of quantification (LODm, LODi, LOQm and LOQi, respectively), accuracy (recovery%), precision (RSD%) and matrix effects. Recovery experiments were carried out with a standard spiking solution of the DTC pesticide thiram. Blank biobed (biomixture) samples were spiked at the three levels corresponding to the CS2 concentrations of 1, 3 and 5 mg kg−1 , with seven replicates each (n = 7). The method presented satisfactory accuracy, with recoveries within the range of 89?96% and RSD ≤ 11%. The analytical curves were linear in the concentration range of 0.05?10 µg CS2 mL−1 (r2 > 0.9946). LODm and LOQm were 0.1 and 0.5 mg CS2 kg−1 , respectively, and the calculated matrix effects were not significant (≤ 20%). The validated method was applied to 80 samples (biomixture), from sixteen different biobeds (collected at five sampling times) during fourteen months. Ten percent of samples presented CS2 concentration below the LOD (0.1 mg CS2 kg−1 ) and 49% of them showed results below the LOQ (0.5 mg CS2 kg−1 ), which demonstrates the biobeds capability to degrade DTC.
NAL Thesaurus:	Biodegradation Degradation
Palavras-chave:	Biobed Biomixture Dithiocarbamates GC-MS
Tipo do material:	Artigo de periódico
Acesso:	openAccess
Aparece nas coleções:	Artigo em periódico indexado (CNPUV)