Abstract
A selective and reliable method was developed and validated for the determination of 14 lipophilic pesticides in raw propolis by gas chromatography–tandem mass spectrometry (GC-MS/MS) analysis. A test portion of milled sample was extracted with n-hexane followed by back extraction with acetonitrile and cleanup using EMR-Lipid and Florisil column adsorption. Matrix-matched standards were used to compensate for matrix effects. Typical linear correlation coefficients (R2) were ≥ 0.989 in concentration range of 0.001–0.200 μg/mL. Method validation was carried out at three spiking levels and three individual days, and it was found that the mean interday average recoveries were 61.0–106.8% with relative standard deviations ≤ 16.9%. Limits of quantification were ranged from 0.002 to 0.020 μg/g. Analysis of market propolis samples showed contamination by pesticides (e.g., tau-fluvalinate) to some degree.
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Acknowledgments
The draft version was revised with the help of Dr. Steven J. Lehotay from USDA Agricultural Research Service.
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This work was financially supported by The Natural Science Foundation of Zhejiang Province (LQ14B070004).
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Xiangyun Wang declares that there is no conflict of interest. Zhiwei Wang declares that there is no conflict of interest. Shanshan Di declares that there is no conflict of interest. Xiaofeng Xue declares that there is no conflict of interest. Yinyin Jin declares that there is no conflict of interest. Peipei Qi declares that there is no conflict of interest. Xinquan Wang declares that there is no conflict of interest. Lijun Han declares that there is no conflict of interest. Yingping Xiao declares that there is no conflict of interest. Shungeng Min declares that there is no conflict of interest.
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Wang, X., Wang, Z., Di, S. et al. Determination of 14 Lipophilic Pesticide Residues in Raw Propolis by Selective Sample Preparation and Gas Chromatography–Tandem Mass Spectrometry. Food Anal. Methods 13, 1726–1735 (2020). https://doi.org/10.1007/s12161-020-01712-8
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DOI: https://doi.org/10.1007/s12161-020-01712-8