UPLC-Q-Exactive测定茶叶中的氟虫腈及其代谢物

Determination of Fipronil and its Metabolites in Tea by UPLC-Quadrupole-Electrostatic Field/Orbitrap High Resolution Mass Spectrometry

目的建立一种UPLC-四极杆-静电场/轨道阱质谱仪(UPLC-Q-Exactive)快速筛查茶叶中氟虫腈及其代谢物。方法将茶叶样品均质后,加乙腈超声提取,再加NaCl、无水Na2SO4除水,最后加N-丙基乙二胺(PSA)粉末、C18粉末以及Na2SO4去除杂质、净化样品。选用Thermo Syncronis C18柱(100 mm×2.1 mm,1.7μm)色谱柱对待测物进行色谱分离,分别采用一级全扫(Full MS/t-SIM)及二级平行监测(PRM)扫描模式进行定量定性分析。结果氟虫腈及其代谢物在0.1~2.0μg/L线性范围内线性良好,其平均回收率和相对偏差为90.2%~106.7%和2.035%~5.438%(Full MS/t-SIM),92.0%~103.2%和1.075%~5.930%(PRM)。结论本方法操作简便、快速、重现性好、稳定性好、灵敏度高,适用于高通量茶叶中氟虫腈及其代谢物的快速定性定量筛查。

Objective A UPLC-quadrupole-electrostatic field/orbitrap high-resolution mass spectrometry was developed for rapid screening of fipronil and its metabolites in tea.Methods After homogenizing the tea samples,ultrasonic extraction with acetonitrile was added,then sodium chloride and anhydrous sodium sulfate were added to remove water.Finally,PSA powder,C18 powder and anhydrous sodium sulfate were added to remove impurities and purify the samples.Thermo Syncronis C18 column(100 mm×2.1 mm,1.7μm)was used for chromatographic separation of the samples.Data were collected under the Full MS/t-SIM and PRM scanning mode of Q-Exactive for qualitative and quantitative analysis.Results The linearity of Fipronil and its metabolites was good in the concentration range of 0.1-2.0μg/L.The average recovery and RSD of the two scanning modes were 90.2%-106.7%and 2.035%-5.438%(Full MS/t-SIM),92.0%-103.2%and 1.075%-5.930%(PRM).Conclusion The method is simple,rapid,reproducible,stable and sensitive.It is suitable for rapid qualitative and quantitative screening of Fipronil and its metabolites in tea.