Utilize este identificador para referenciar este registo: http://hdl.handle.net/10400.22/3432
Título: Optimization of QuEChERS procedure coupled to GC-ECD for organochlorine pesticide determination in carrot samples
Autor: Correia-Sá, Luísa
Fernandes, Virgínia C.
Calhau, Conceição
Domingues, Valentina F.
Delerue-Matos, Cristina
Palavras-chave: QuEChERS
Organochlorine pesticides
Tandem mass spectrometry
Data: 2013
Editora: Springer
Relatório da Série N.º: Food Analytical Methods; Vol. 6, Issue 2
Resumo: An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO4) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EUmaximum residue limits (MRLs) for carrots, 10–50 μg kg−1, while the limit of quantification did exceed 10 μg kg−1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg−1), ranged from 66 to 111% with relative standard deviations in the range of 2– 15 % (n03) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg−1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg−1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.
Peer review: yes
URI: http://hdl.handle.net/10400.22/3432
ISSN: 1936-976X
Versão do Editor: http://link.springer.com/article/10.1007/s12161-012-9463-x
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