Solid phase-extraction procedure for the determination of amitraz degradation products in honey

ABSTRACT

Solid-phase extraction (SPE) was carefully optimised for preconcentration of 2-4-dimethylaniline (2,4-DMA) and 2,4-dimethylformanilide (DMF) from honey samples. Liquid chromatography with tandem mass spectrometry (LC-MS/MS) was used for the separation and quantification of these analytes. By applying the SPE procedure with 200 mg of OASIS HLB sorbent, the limits of detection achieved in honey samples can be lowered to 0.41 µg·kg⁻¹ for 2,4-DMA and 0.69 µg L⁻¹ for DMF. The proposed method achieves good recoveries (81.1–114%) and precision (RSD 1.07–4.05%, n = 3) for analysed honey sample spiked at two concentration levels 1 µg L⁻¹ and 2 µg L⁻¹. The results demonstrated our method can be applied as a simple way for sample preparation of honey samples for determination of amitraz degradation products. In 1 out of 5 of the analysed Polish honey samples, the DMF residues exceed the maximum residual limits (0.2 mg·kg⁻¹ for total amitraz residues).

GRAPHICAL ABSTRACT

KEYWORDS:

• Honey
• amitraz degradation products
• DMF
• 2,4-DMA
• solid-phase extraction (SPE)
• liquid chromatography mass spectrometry (LC-MS/MS)

Acknowledgments

The authors would like to thank Prof. Krystyna Pyrzyńska for her helpful advice on various technical issues examined in this paper. The authors would also like to thank the Structural Research Laboratory (SRL) at the Department of Chemistry of the University of Warsaw for making LC-MS/MS measurements possible.

Disclosure statement

No potential conflict of interest was reported by the authors.

Additional information

Funding

This work was supported by the University of Warsaw, Faculty of Chemistry under grant [DSM 501-D112-86-0117700].