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Article

Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry

1
Faculty of Chemistry and Chemical Technology, University of Ljubljana, 1000 Ljubljana, Slovenia
2
Department of Environmental Sciences, Jožef Stefan Institute, 1000 Ljubljana, Slovenia
3
Jožef Stefan International Postgraduate School, 1000 Ljubljana, Slovenia
4
Slovenian Beekeepers’ Association, 1225 Lukovica, Slovenia
*
Author to whom correspondence should be addressed.
Academic Editor: Soraia I. Falcão
Molecules 2020, 25(24), 5870; https://doi.org/10.3390/molecules25245870
Received: 28 October 2020 / Revised: 7 December 2020 / Accepted: 9 December 2020 / Published: 11 December 2020
In this study, a method was developed for the determination of five neonicotinoid pesticides (acetamiprid, clothianidin, imidacloprid, thiacloprid, and thiamethoxam) in propolis. Two sample preparation methods were tested: solid-phase extraction and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The identities of analytes were confirmed using liquid chromatography–tandem mass spectrometry (LC-MS/MS) in the selected reaction monitoring mode. Solid-phase extraction resulted in cleaner extracts; therefore, the SPE-LC-MS/MS method was validated according to the SANTE protocol in triplicate at two spiking levels (10 ng/g and 50 ng/g). The average recoveries of analytes ranged from 61% to 101%, except for clothianidin (10–20%). The LOD ranged from 0.2 ng/g to 4.4 ng/g, whereas the LOQ was in the range of 0.8 ng/g–14.7 ng/g. In order to compensate for the matrix effect, matrix-matched calibration was used. Good accuracy (relative error: 1.9–10.4%) and good linearity (R2 > 0.991) were obtained for all compounds. The optimised method was applied to 30 samples: 18 raw propolis and 12 ethanol tinctures. Acetamiprid, imidacloprid, and thiacloprid were detectable in seven samples but were still below the LOQ. This study is the first to report the determination of several neonicotinoid residues in propolis. View Full-Text
Keywords: neonicotinoids; propolis; SPE; QuEChERS; LC-MS/MS neonicotinoids; propolis; SPE; QuEChERS; LC-MS/MS
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MDPI and ACS Style

Tomšič, R.; Heath, D.; Heath, E.; Markelj, J.; Kandolf Borovšak, A.; Prosen, H. Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry. Molecules 2020, 25, 5870. https://doi.org/10.3390/molecules25245870

AMA Style

Tomšič R, Heath D, Heath E, Markelj J, Kandolf Borovšak A, Prosen H. Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry. Molecules. 2020; 25(24):5870. https://doi.org/10.3390/molecules25245870

Chicago/Turabian Style

Tomšič, Rok, David Heath, Ester Heath, Jernej Markelj, Andreja Kandolf Borovšak, and Helena Prosen. 2020. "Determination of Neonicotinoid Pesticides in Propolis with Liquid Chromatography Coupled to Tandem Mass Spectrometry" Molecules 25, no. 24: 5870. https://doi.org/10.3390/molecules25245870

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