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. 2018 Oct 9;23(10):2582.
doi: 10.3390/molecules23102582.

Comparison of Two Methods for the Determination of Selected Pesticides in Honey and Honeybee Samples

Żaneta Bargańska  1 , Piotr Konieczka  2 , Jacek Namieśnik  3
Affiliations

Comparison of Two Methods for the Determination of Selected Pesticides in Honey and Honeybee Samples

Żaneta Bargańska et al. Molecules. .

Abstract

Developed and validated analytical methods for the determination of a wide spectrum of pesticide residues in honey and honeybee samples after the modification of QuEChERS extraction in combination with gas chromatography⁻tandem quadrupole mass spectrometry (GC-MS/MS) and liquid chromatography⁻tandem quadrupole mass spectrometry (LC-MS/MS) were discussed and compared. The developed methods were evaluated regarding the utilized equipment and reagents using Eco-Scale and compared in terms of extraction time, accuracy, precision, sensitivity and versatility, with similar procedures. The results proved that the QuEChERS protocol in combination with LC and GC techniques fulfills the requirements of green analytical chemistry, so it can be used as a tool in environmental monitoring. The recovery was 85⁻116% for honey and 85.5⁻103.5% for honeybee samples. The developed methods were successfully applied in monitoring real samples collected from three districts of Pomerania in Poland. Analysis of real samples revealed the presence of the following pesticides: bifenthrin, fenpyroximate, methidathione, spinosad, thiamethoxam, triazophos, metconazole and cypermethrin at levels higher than the MRLs established by the EU.

Keywords: Eco-Scale; GC-MS/MS; LC-MS/MS; QuEChERS; environmental monitoring; honey; honeybees; pesticides.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Differences in recovery found during the extraction process when using 3 mL versus 1.5 mL of n-hexane for removing wax from honeybee samples using modified QuEChERS method for selected pesticides.
Figure 2
Figure 2
Distribution of matrix effects for selected pesticides: A Honey B Honeybee.
Figure 3
Figure 3
Information on the identification and detection of the selected analytes using the developed analytical methods (LC and GC).
Figure 4
Figure 4
The sample chromatograms obtained during analysis of extracts from real sample in which selected pesticide residues was detected above MRLs level: A—honey samples, B—honeybee samples.
Figure 5
Figure 5
Scheme of pesticide extraction procedures from honey and honeybee samples using the QuEChERS extraction before final analysis.
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