Matrix solid-phase dispersion extraction of organophosphorous pesticides from beeswax

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...

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Bibliographic Details
Published in:International journal of environmental analytical chemistry 2017-07, Vol.97 (9), p.831-840
Main Authors: Medina-Dzul, K., Medina-Peralta, S., Carrera-Figueiras, C., Sánchez, M., Muñoz-Rodríguez, D.
Format: Article
Language:English
Subjects:
Acetates
Acetic acid
Agrochemicals
Alcohols
Aliphatic alcohols
Aliphatic compounds
Beeswax
Carotenoids
Clean-up procedures
Coumaphos
Detection
Diazinon
Dichlorvos
Dispersion
Environmental cleanup
Ethyl acetate
Extraction
Gas chromatography
GC/MS
Legislation
Lipophilic
Malathion
Mass spectrometry
Mass spectroscopy
Methods
Methyl parathion
MSPD
organophosphorous pesticides
Parathion
Pesticides
rapid method
Solids
Waxes
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Summary: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.
ISSN:0306-7319
1029-0397
DOI:10.1080/03067319.2017.1363195