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当前位置: 首页 > 文章 > QuEChERS-气相色谱-串联质谱-同位素内标法快速测定茶叶中氟虫腈及其代谢物残留量 食品科学 2020 (12) 312-317
Position: Home > Articles > Quick Determination of Residues of Fipronil and Its Metabolites in Tea by QuEChERS Coupled with Gas Chromatography-Tandem Mass Spectrometry with Isotope Internal Standard Calibration FOOD SCIENCE 2020 (12) 312-317

QuEChERS-气相色谱-串联质谱-同位素内标法快速测定茶叶中氟虫腈及其代谢物残留量

作  者：
倪韵晨;徐小民;黄百芬;徐美佳;李祖光
单  位：
浙江工业大学教育科学与技术学院;浙江省疾病预防控制中心理化毒理所;浙江工业大学化学工程学院
关键词：
氟虫腈及其代谢物;同位素内标法;QuEChERS技术;气相色谱-串联质谱法;茶叶
摘  要：
采用QuEChERS前处理技术,建立气相色谱-三重四极杆串联质谱联用仪测定茶叶中氟虫腈及其代谢物残留量的分析方法。样品添加氟虫腈-~(13)C_2,~(15)N_2同位素内标后,用水浸润后乙腈提取,NaCl、无水MgSO_4盐析脱水,N-丙基乙二胺和石墨化碳黑净化,多反应离子监测模式测定,内标法定量。氟虫腈及其代谢物在0.4～100?μg/L范围内呈良好线性关系,相关系数(r2)均不小于0.995,定量限均为1?μg/kg,在4个添加水平(1、5、20、200?μg/kg)下的加标回收率为76.72%～96.53%,相对标准偏差(n=6)为4.76%～13.07%。该方法简单、灵敏、准确,适用于茶叶中氟虫腈及其代谢物的快速定量测定,方法的灵敏度满足日本、欧盟的残留限量要求。
译  名：
Quick Determination of Residues of Fipronil and Its Metabolites in Tea by QuEChERS Coupled with Gas Chromatography-Tandem Mass Spectrometry with Isotope Internal Standard Calibration
作  者：
NI Yunchen;XU Xiaomin;HUANG Baifen;XU Meijia;LI Zuguang;College of Education, Zhejiang University of Technology;Institute of Physical Chemistry and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention;College of Chemical Engineering, Zhejiang University of Technology;
关键词：
fipronil and its metabolites;;isotope internal standard;;QuEChERS;;gas chromatography-tandem mass spectrometry;;tea
摘  要：
Based on the quick, easy, cheap, effective, rugged and safe(QuEChERS) technique, a method for the simultaneous determination of the residues of fipronil and its metabolites in tea was developed by gas chromatography-tandem mass spectrometry(GC-MS/MS). The samples were added with the internal standard of fipronil-~(13)C_2,~(15)N_2, and then extracted with acetonitrile after water soaking. The extract was dehydrated with sodium chloride(NaCl) and anhydrous magnesium sulfate(MgSO_4) and purified by dispersive solid phase extraction with N-propyl ethylenediamine(PSA) and graphite carbon(GCB) sorbents. The analytes were detected by tandem mass spectrometry using multiple reaction monitoring(MRM), and quantified by the internal standard method. A good linearity in the concentration range of 0.4–100 μg/L with correlation coefficients(R~2) > 0.995 was observed. The limits of quantification(LOQs) for both fipronil and its metabolites were 1 μg/kg. The recoveries of fipronil and its metabolites at four spiked levels(1, 5, 20 and 200 μg/kg) were in the range of 76.72%–96.53% with relative standard deviations(RSDs, n = 6) between 4.76% and 13.07%. The method was found to be simple, sensitive, accurate and suitable for the rapid quantitative analysis of fipronil and its metabolites in tea. Its sensitivity could meet the requirement for the residual limitation of the EU and Japan.

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