Estimation of the uncertainties of extraction and clean-up steps in pesticide residue analysis of plant commodities

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Date

2013

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Taylor & Francis Ltd

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Abstract

Extraction and clean-up constitute important steps in pesticide residue analysis. For the correct interpretation of analytical results, uncertainties of extraction and clean-up steps should be taken into account when the combined uncertainty of the analytical result is estimated. In the scope of this study, uncertainties of extraction and clean-up steps were investigated by spiking 14C-labelled chlorpyrifos to analytical portions of tomato, orange, apple, green bean, cucumber, jackfruit, papaya and starfruit. After each step, replicate measurements were carried out with a liquid scintillation counter. Uncertainties in extraction and clean-up steps were estimated separately for every matrix and method combination by using within-laboratory reproducibility standard deviation and were characterised with the CV of recoveries. It was observed that the uncertainty of the ethyl acetate extraction step varied between 0.8% and 5.9%. The relative standard uncertainty of the clean-up step with dispersive SPE used in the method known as QuEChERS was estimated to be around 1.5% for tomato, apple and green beans. The highest variation of 4.8% was observed in cucumber. The uncertainty of the clean-up step with gel permeation chromatography ranged between 5.3% and 13.1%, and it was relatively higher than that obtained with the dispersive SPE method.

Description

Omeroglu, Perihan Yolci/0000-0001-8254-3401; BOYACIOGLU, DILEK/0000-0002-8160-0619

Keywords

ethyl acetate extraction, extraction and clean-up, gel permeation chromatography, measurement uncertainty, pesticide residues, QuEChERS

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3

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Volume

30

Issue

2

Start Page

308

End Page

320