Determination of fipronil and its metabolites in fruits and vegetables by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
Determination of fipronil and its metabolites in fruits and vegetables by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
Objective To establish a method for the determination of fipronil,fipronil sulfone and fipronil sulfoxide in veg-etables and fruits by using QuEChERS method for pre-treatment and ultra high performance liquid chromatoplc-tandem mass spectrometry.Methods The edible parts of vegetables and fruits on the market were crushed and sampled,extracted by acetonitrile oscillating ultrasonic,added to solid phase extraction salt pack,supernatant was passed through QuEChERS small column,purified liquid after centrifugation was passed through 0.22 μm filter,determined by ultra-high performance liquid chromatography-tandem mass spectrometry,and matrix curve was used for quantification.Results The three insec-ticides had good linearity relationship in the concentration range of 1.0-100.0 ng/ml,and the phase relationship values were all＞0.995.The limits of detection were 0.5 μg/kg,and the limits of quantification were 1.5 μg/kg.The standard re-coveries ranged from 74.1％to 118.9％,and the relative standard deviations(RSD)were from 3.2％to 9.6％.Conclusion The method is simple and sensitive,and can simultaneously determine the residues of fipronil,fipronil sulfone and fipro-nil sulfoxide in vegetables and fruits,and provide technical reference for their daily monitoring.
关键词
超高效液相色谱-串联质谱法/氟虫腈/氟虫腈砜/氟虫腈亚砜/QuEChERS/水果/蔬菜
Key words
Ultra high performance liquid chromatoplc-tandem mass spectrometry/Fipronil/Fipronil sulfone/Fipronil sulfoxide/QuEChERS/Fruits/Vegetables
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