凝胶净化色谱-三重四级杆串联气相色谱质谱法检测植物源性食品中氟虫腈及其代谢物残留量

目的采用凝胶净化色谱-三重四级杆串联气相色谱质谱法(GPC-GC/MS/MS)对植物源性食品中氟虫腈及其代谢物氟甲腈、氟虫腈亚砜、氟虫腈砜农药残留量进行分析。方法样品经乙腈超声提取后采用QuECHRS萃取包净化,用SH-Rxi-5il MS(30 m×0.25 mm,0.25μm)毛细管色谱柱分离,外标法定量分析。结果用本法测定,氟虫腈及其代谢物氟甲腈、氟虫腈亚砜、氟虫腈砜色谱峰得到很好的分离,在0.01μg/ml^0.5μg/ml浓度内呈现良好的线性关系。相关系数均达到0.9999,方法检出限均为0.003 mg/kg,氟虫腈及其代谢物在3个浓度添加水平下的加标回收率为89%~116%,相对标准偏差在1.10%~7.22%。结论该方法实现了氟虫腈及其代谢物检测的自动化、快速、高灵敏度和高稳定性分析,能够满足目前植物源性食品中氟虫腈及其代谢物残留检测限量的要求。

Detection of fipronil and its metabolites in plant-based foods by GPC-GC/MS/MS

Objective Gel purification chromatography-triple quadrupole tandem gas chromatography-mass spectrometry(GPC-GC/MS/MS)was used to detect fipronil and its metabolites fipronil desulfinyl,fipronil sulfone and fipronil sulfide in plant-based foods.Methods The targets were extracted by ultrasound from samples with acetonitrile,and purified by QuECHRS extraction package.Then,The analytes were separated by SH-Rxi-5il MS(30 m×0.25 mm,0.25μm)capillary column and quantified by external standard method.Results Fipronil and its metabolites fipronil desulfinyl,fipronil sulfone and fipronil sulfide were well separated by this method.A good linear relationship was obtained in the range of 0.01μg/ml to 0.5μg/ml with correlation coefficients of 0.9999.All LODs were 0.003 mg/kg and the recoveries were in range of 89%to 116%at three spiked levels with RSDs of 1.10%-7.22%.Conclusion The method realized the fast automation detection of fipronil and its metabolites with high sensitivity and stability.Therefore,it can be used to determine the residues of fipronil and its metabolites in plant-based foods.