Rapid and sensitive detection of fipronil and its metabolites in edible oils by solid-phase extraction based on humic acid bonded silica combined with gas chromatography with electron capture detection
Rapid and sensitive detection of fipronil and its metabolites in edible oils by solid-phase extraction based on humic acid bonded silica combined with gas chromatography with electron capture detection
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腐殖酸键合硅胶固相萃取结合气相色谱电子捕获检测快速灵敏检测食用油中氟虫腈及其代谢物
DOI：
10.1002/jssc.201501250
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发表时间：
2016-06-01
影响因子：
3.1
通讯作者：
Feng, Yu-Qi
中科院分区：
文献类型：
--
作者：
Peng, Xi-Tian;Li, Yu-Nan;Feng, Yu-Qi
建立了腐植酸键合二氧化硅固相萃取-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的方法。为了获得最佳的萃取性能，我们系统地研究了一系列固相萃取参数。在优化条件下，对该方法进行了线性度、回收率和精密度的验证。当R-2大于0.9996时，所有分析物均具有良好的线性关系。三种加标浓度下的检出限为0.3 ~ 0.5 ng/g，加标回收率为83.1 ~ 104.0%，日内、日间相对标准偏差小于8.7%。最后，应用该方法对武汉市市场11份食用油样品中的氟虫腈及其代谢物进行了检测。在四个样品中检测到氟虫腈，浓度范围为3.0至5.2 ng/g。在中国，氟虫腈在部分蔬菜和玉米中的最大残留限量分别为20和100 ng/g （GB/T 2763-2014）。氟虫腈及其代谢物在商业食用油中的残留可能对人类健康构成某种潜在威胁，因为食用油是每日摄入量的一部分。
Solid-phase extraction based on humic acid bonded silica followed by gas chromatography with electron capture detection was developed to determine fipronil and its metabolites in edible oil. To achieve the best extraction performance, we systematically investigated a series of solid-phase extraction parameters. Under the optimized conditions, the method was validated according to linearity, recovery, and precision. Good linearities were obtained with R-2 more than 0.9996 for all analytes. The limits of detection were between 0.3 and 0.5 ng/g, and the recoveries ranged from 83.1 to 104.0% at three spiked concentrations with intra-and interday relative standard deviation values less than 8.7%. Finally, the proposed method was applied to determine fipronil and its metabolites in 11 edible oil samples taken from Wuhan markets. Fipronil was detectable in four samples with concentrations ranging from 3.0 to 5.2 ng/g. In China, the maximum residue limits of fipronil in some vegetables and maize are 20 and 100 ng/g (GB/T 2763-2014), respectively. The residues of fipronil and its metabolites in commercial edible oils might exhibit some potential threat to human health as a result of high consumption of edible oil as part of daily intake.