QuEChERS-气相色谱质谱法检测苹果中氟虫腈及其代谢物残留量

Determination of Fipronil and Its Metabolites in Apple by QuEChERS Method Coupled with Gas Chromatography-Mass Spectrometry

通过QuEChERS萃取净化、气相色谱质谱法检测,建立了一种苹果中氟虫腈及其代谢物的分析方法。苹果经乙腈提取、QuEChERS净化管净化,用气相色谱质谱法检测。结果显示,在0.02~1.00 mg/kg质量浓度范围内,氟虫腈及其代谢物与对应定量离子峰面积呈良好线性关系,相关系数大于0.999,方法定量限为0.01 mg/kg。在0.01,0.03和0.1 mg/kg 3个添加水平下,氟虫腈及其代谢物的回收率在83.1%~94.6%之间,相对标准偏差(S_(RSD),n=6)为1.9%~6.8%。该方法实用性强,操作简单,减少了试剂用量和分析时间,可以作为苹果中氟虫腈及其代谢物的分析方法。

It was to establish a method for the determination of fipronil and its metabolites in apple by QuEChERS method coupled with gas chromatography-mass spectrometry.Apple was extracted by acetonitrile,purified on a QuEChERS pipe,and determined by gas chromatography-mass spectrometry.The results showed that linear relationships between peak area and mass concentration of fipronil and its metabolites were obtained in the range of 0.02-1.00 mg/kg.The limit of quantitation was 0.01 mg/kg.When the spiked levels were 0.01,0.03 and 0.1 mg/kg,the recoveries of fipronil and its metabolites ranged from 83.1% to 94.6% with relative standard deviations(S_(RSD),n=6) between 1.9% and 6.8%.The method was practical and easy to operate,reducing the amount of reagent and analysis time.It could be used for the analysis of fipronil and its metabolites in apple.