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Fast analysis of multiple pesticide residues in apple juice using dispersive liquid–liquid microextraction and multidimensional gas chromatography–mass spectrometry

Cunha, S.C. ; Fernandes, J.O. ; Oliveira, M.B.P.P.

Journal of Chromatography A, 2009-12, Vol.1216 (51), p.8835-8844 [Periódico revisado por pares]

Amsterdam: Elsevier B.V

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Título:
Fast analysis of multiple pesticide residues in apple juice using dispersive liquid–liquid microextraction and multidimensional gas chromatography–mass spectrometry
Autor: Cunha, S.C. ; Fernandes, J.O. ; Oliveira, M.B.P.P.
Assuntos: apple juice ; Beverages - analysis ; Biological and medical sciences ; Chemical Fractionation - methods ; Deans switch ; dispersive liquid-liquid microextraction ; Dispersive liquid–liquid microextraction (DLLME) ; Environmental Monitoring ; Fast-GC, Multidimensional gas chromatography–mass spectrometry (MD-GC/MS) ; food contamination ; Food industries ; Fruit and vegetable industries ; Fundamental and applied biological sciences. Psychology ; gas chromatography ; Gas Chromatography-Mass Spectrometry - methods ; Juices ; Limit of Detection ; Malus - chemistry ; mass spectrometry ; microextraction ; Molecular Weight ; multidimensional gas chromatography-mass spectrometry ; multiresidue analysis ; Non alcoholic beverage industries and mineral waters ; pesticide residues ; Pesticide Residues - analysis ; Pesticides ; rapid methods ; Reference Standards ; Reproducibility of Results ; Sodium Chloride - chemistry ; Solvents
É parte de: Journal of Chromatography A, 2009-12, Vol.1216 (51), p.8835-8844
Notas: http://dx.doi.org/10.1016/j.chroma.2009.10.051
Descrição: A method for the rapid trace analysis of 24 residual pesticides in apple juice by multidimensional gas chromatography–mass spectrometry (MD-GC/MS) using dispersive liquid–liquid microextraction (DLLME) was developed and optimized. Several parameters of the extraction procedure such as type and volume of extraction solvent, type and volume of dispersive solvent and salt addition were evaluated to achieve the highest yield and to attain the lowest detection limits. The DLLME procedure optimized consists in the formation of a cloudy solution promoted by the fast addition to the sample (5 ml) of a mixture of carbon tetrachloride (extraction solvent, 100 μl) and acetone (dispersive solvent, 400 μl). The tiny droplets formed and dispersed among the aqueous sample solution are further joined and sedimented (85 μl) in the bottom of the conical test tube by centrifugation. Once extracted, all the 24 pesticides were directly injected and separated by a dual GC column system, comprising a short wide-bore DB-5 capillary column with low film thickness connected by a Deans switch system to a second chromatographic narrower column, with identical stationary phase. The instrumental setting used, in combination with carefully optimized operational fast GC and MS parameters, markedly decreased the retention times of the targeted analytes. The total chromatographic run was 8 min. Mean recoveries for apple juice spiked at three concentrations ranged from 60% to 105% and the intra-repeatability ranged from 1% to 21%. The limits of detection of the 24 pesticides ranged from 0.06 to 2.20 μg/L. In 2 of a total of 28 analysed samples were found residues of captan, although at levels below the maximum limit legal established.
Editor: Amsterdam: Elsevier B.V
Idioma: Inglês

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Fast analysis of multiple pesticide residues in apple juice using dispersive liquid–liquid microextraction and multidimensional gas chromatography–mass spectrometry

Cunha, S.C. ; Fernandes, J.O. ; Oliveira, M.B.P.P.

Amsterdam: Elsevier B.V

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