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Food Analytical Methods

, Volume 9, Issue 8, pp 2182–2193 | Cite as

Fast Preconcentration of Pesticide Residues in Oilseeds by Combination of QuEChERS with Dispersive Liquid–Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

  • M. Andraščíková
  • S. HrouzkováEmail author
Article

Abstract

A fast, efficient, and simple method for determination of pesticide residues in pumpkin seeds has been developed combining QuEChERS and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography and mass spectrometry (GC-MS). Parameters affecting the DLLME performance such as solvent selection and volume of extractive and dispersive solvent, salt effect, and extraction time were studied. Under the selected conditions (50 μL extractive solvent chloroform, 1 mL QuEChERS extract, and 3 mL water), the developed method was validated. Linearity was evaluated at nine concentrations in the broad range of 0.1–500 μg/kg with correlation coefficients from 0.9842 to 0.9972. The relative standard deviations at lowest calibration level varied from 0.3 to 22 %. Under the optimum conditions, an enrichment factor was 6–17-fold and detection limits 0.01–12.17 μg/kg were achieved. Finally, the developed and validated method was successfully applied for the extraction and determination of pesticide residues in 16 real samples with 2 positive findings below maximum residue limits (MRL). Limits of detection (LODs) of the proposed method are below the MRLs established by the European Union.

Keywords

Dispersive liquid–liquid microextraction QuEChERS Oilseeds Validation 

Notes

Compliance with Ethical Standards

Funding

This work was supported by the Scientific Grant Agency of the Ministry of Education of the Slovak Republic and the Academy of Sciences (VEGA, project no. 1/0503/14) and by the Slovak Research and Development Agency under contract no. APVV-0797-11.

Conflict of Interest

Mária Andraščíková declares that she has no conflict of interests. Svetlana Hrouzková declares that she has no conflict of interests.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.

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Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  1. 1.Institute of Analytical Chemistry, Faculty of Chemical and Food TechnologySlovak University of Technology in BratislavaBratislavaSlovak Republic

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