Matrix solid-phase dispersion extraction of organophosphorous pesticides from beeswax

ABSTRACT

Beeswax is a complex mixture of lipophilic compounds and other components such as aliphatic alcohols and carotenoids. Then, extraction and clean-up for pesticide analysis in beeswax is a challenge. In this work, a multiresidue method for the analysis of dichlorvos (DCV), diazinon, malathion, methyl parathion and coumaphos (CMF) in beeswax was developed. The proposed approach is based on matrix solid-phase dispersion extraction. The adsorbent for sample clean-up was studied and a simplex-centroid cubic statistical design was applied to evaluate pure solvents and their binary and ternary mixtures to elute the analytes. Finally, Florisil and ethyl acetate were chosen as solid support and eluting solvent, respectively. After extraction, pesticides were separated and detected by gas chromatography/mass spectrometry. The method achieved acceptable recoveries (70–85%; except for DCV, 24–38%) with relative standard deviations below 5%. The repeatability of the method was lower than 8% and interday variability was below 12%. The limit of detection (LOD) for the analytes varies between 0.2 and 2.6 µg⋅kg⁻¹ and limit of quantification from 0.93 to 8.8 µg⋅kg⁻¹. LOD reached for CMF was below the maximum residue limit allowed by the legislation of the United States and Canada.

KEYWORDS:

• Clean-up procedures
• organophosphorous pesticides
• beeswax
• GC/MS
• rapid method
• MSPD

Acknowledgements

The authors thank Dra. Yolanda Beatriz Moguel-Ordoñez for providing wax samples for our study.

Disclosure statement

No potential conflict of interest was reported by the authors.