Trace-level determination of pyrethroid, neonicotinoid and carboxamide pesticides in beeswax using dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry

Abstract

The aim of the work was to develop an analytical procedure able to quantify traces of 13 neonicotinoids and pyrethroids as well as carboxamide in beeswax at low levels (ng g⁻¹) to evaluate the contamination. For this purpose, an efficient sample preparation procedure was developed based on solid–liquid extraction using dispersive diatomaceous earth and acetonitrile. This step was followed by a selective and sensitive analysis based on ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (ESI-MS/MS). This analytical procedure was validated based on International Conference on Harmonization guidelines. The limits of quantification ranged from 1 ng g⁻¹ (thiamethoxam, clothianidin, imidacloprid, acetamiprid, thiacloprid and boscalid) to 40 ng g⁻¹ (lambda-cyhalothrin). The method was then successfully applied to 60 samples of beeswax collected in several areas of France. The presence of thiacloprid, boscalid, imidacloprid and deltamethrin in beeswax was confirmed. The most frequently quantified pesticide was boscalid.

Keywords:

• neonicotinoids
• pyrethroids
• boscalid
• LC-MS/MS multiresidue method
• beeswax
• sample preparation

Acknowledgement

The authors thank the beekeepers from FNOSAD and ADARA for their beekeeping expertise and sampling.

Additional information

Funding

Funding for this project was provided by a grant from the Rhône-Alpes Region.