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Int. J. Environ. Res. Public Health 2014, 11(11), 11421-11437; doi:10.3390/ijerph111111421

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

1
Laboratório Nacional Agropecuário, Ministério da Agricultura, Pecuária e Abastecimento, Estrada da Ponta Grossa, 3036 Porto Alegre, RS 91785-340, Brazil
2
Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Av. Ipiranga, 2752 Porto Alegre, RS 90610-000, Brazil
3
Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves, 9500 Bairro Agronomia, Porto Alegre, RS 91501-970, Brazil
*
Author to whom correspondence should be addressed.
Received: 22 July 2014 / Revised: 15 October 2014 / Accepted: 27 October 2014 / Published: 5 November 2014
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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. View Full-Text
Keywords: Doehlert design; GC-MS/MS; GC-ECD; pyrethroids; bovine milk Doehlert design; GC-MS/MS; GC-ECD; pyrethroids; bovine milk
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Meneghini, L.Z.; Rübensam, G.; Bica, V.C.; Ceccon, A.; Barreto, F.; Ferrão, M.F.; Bergold, A.M. Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis. Int. J. Environ. Res. Public Health 2014, 11, 11421-11437.

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