Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis

Leonardo Zanchetti Meneghini, Gabriel Rübensam, Vinicius Claudino Bica, Amanda Ceccon, Fabiano Barreto, Marco Flores Ferrão and Ana Maria Bergold
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Leonardo Zanchetti Meneghini: Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
Gabriel Rübensam: Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
Vinicius Claudino Bica: Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
Amanda Ceccon: Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
Fabiano Barreto: Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
Marco Flores Ferrão: Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves, 9500 Bairro Agronomia, Porto Alegre, RS 91501-970, Brazil
Ana Maria Bergold: Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Av. Ipiranga, 2752 Porto Alegre, RS 90610-000, Brazil

IJERPH, 2014, vol. 11, issue 11, 1-17

Abstract: A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences ( p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed.

Keywords: Doehlert design; GC-MS/MS; GC-ECD; pyrethroids; bovine milk (search for similar items in EconPapers)
JEL-codes: I I1 I3 Q Q5 (search for similar items in EconPapers)
Date: 2014
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