Rok Tomšič (Author), David John Heath (Author), Ester Heath (Author), Jernej Markelj (Author), Andreja Kandolf (Author), Helena Prosen (Author)

Abstract

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 (R$^2$ > 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.

Keywords

neonikotinoidi;propolis;SPE;QuEChERS;LC-MS/MS;neonicotinoids;

Data

Language: English
Year of publishing:
Typology: 1.01 - Original Scientific Article
Organization: UL FKKT - Faculty of Chemistry and Chemical Technology
UDC: 543.544.5:543.51
COBISS: 42430723 Link will open in a new window
ISSN: 1420-3049
Views: 198
Downloads: 109
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Other data

Secondary language: Slovenian
Secondary keywords: neonikotinoidi;propolis;SPE;QuEChERS;LC-MS/MS;
Type (COBISS): Article
Pages: str. 1-12
Volume: ǂVol. ǂ25
Issue: ǂVol. ǂ24
Chronology: Dec. 2020
DOI: 10.3390/molecules25245870
ID: 14354383