Determination of fipronil and its metabolites in edible oil by pollen based solid-phase extraction combined with gas chromatography-electron capture detection

Determination of fipronil and its metabolites in edible oil by pollen based solid-phase extraction combined with gas chromatography-electron capture detection
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花粉固相萃取-气相色谱-电子捕获检测法测定食用油中氟虫腈及其代谢物

DOI:
10.1016/j.foodchem.2021.132021
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发表时间:
2022-01
期刊:
影响因子:
8.8
通讯作者:
Qin Zhao
Qin Zhao
中科院分区:
农林科学1区
文献类型:
--
作者:
Yi-Lian Zhou;Shi-Wen Yue;Bing-Wei Cheng;Qin Zhao

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建立了一种方便、经济的花粉固相萃取法测定食用油中氟虫腈及其3种代谢物的方法。花粉作为一种天然物质,由于其特殊的功能结构,对某些极性化合物表现出良好的吸附能力。它们稳定的组成和合适的粒度也使它们适用于SPE。本研究以天然松花粉为吸附剂,利用氢键作用,从食用油中选择性分离富集氟虫腈及其3种代谢产物。考察了影响萃取回收率的几个参数。采用气相色谱-电子捕获检测器(GC-ECD)联用技术,建立了食用油中氟虫腈及其代谢物的分析方法。线性范围为2-200 ng/g,相关系数R2> 0.999。食用油中3种添加浓度的回收率在80.1-96.0%之间,日内RSD小于10.6%,日间RSD小于11.5%。4种目标分析物的检测限(LOD)在0.2-0.6 ng/g范围内,与以往报道的方法相当。最后,将所建立的方法成功地应用于检测几种不同品牌的油脂样品中的氟虫腈及其代谢产物。
In this study, a convenient and economic method for the determination of fipronil and its three metabolites in edible oil was developed based on pollen grain solid-phase extraction (SPE). As a natural material, pollen grains exhibit well absorption capacity for some polar compounds due to their special functional structures. Their stable composition and appropriate particle size also make them suitable for SPE. In the present study, natural pine pollen grains without broken wall were used as sorbent for selective isolation and enrichment of fipronil and its three metabolites from edible oils based on hydrogen bond interaction. Several parameters influencing the extraction recoveries were investigated. By coupling with gas chromatography-electron capture detection (GC-ECD), a new method for analysis of fipronil and its metabolites in edible oils was established. The linearity range was 2–200 ng/g with correlation coefficient R2more than 0.999. The recoveries in edible oils at three spiked concentrations were in the range of 80.1–96.0% with the RSDs less than 10.6% (intra-day) and 11.5% (inter-day). The limit of detection (LOD) for four target analytes were in the range of 0.2–0.6 ng/g, which was comparable to the previous reported methods. Finally, the established method was successfully applied to detect fipronil and its metabolites in several oil samples with different brands from local market.
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影响因子: 2.9
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