固相萃取-高效液相色谱-串联质谱法测定茶叶中啶虫脒、吡虫啉和氟虫腈残留量

Determination of imidacloprid, acetamiprid and fipronil residues in tea by high performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction

中文关键词:  固相萃取  高效液相色谱-串联质谱  啶虫脒  吡虫啉  氟虫腈  农药残留  茶叶

英文关键词:solid-phase extraction  high performance liquid chromatography-tandem mass spectrometry  imidacloprid  acetamiprid  fipronil  pesticide residues  tea

中文摘要:

      目的 建立茶叶中吡虫啉、啶虫脒和氟虫腈三种农药残留的固相萃取-高效液相色谱-串联质谱测定方法。方法 样品用水浸泡, 乙腈提取, 经石墨化碳-氨基复合固相萃取小柱净化, 采用Agilent Eclipse AAA色谱柱分离, 以0.1%乙酸水溶液和乙腈为流动相梯度洗脱, 正、负离子切换扫描, 多反应监测(MRM)模式检测, 外标法定量。结果 在3个添加水平下, 吡虫啉、啶虫脒和氟虫腈的平均回收率分别为78.8%~91.5%, 81.3%~92.8%, 和72.8%~90.0%; 相对标准偏差分别为2.6%~10.6%, 3.7%~6.6%和3.6 %~7.4%。啶虫脒、吡虫啉和氟虫腈的检出限均为0.5 μg/kg, 定量限为2 μg/kg。结论 建立的方法简便、快速, 灵敏度高, 可满足出口茶叶中吡虫啉、啶虫脒和氟虫腈残留同时检测的要求。

英文摘要:

      Objective To establish a method for the determination of imidacloprid, acetamiprid and fipronil residues in tea based on solid-phase extraction (SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were soaked with water, extracted with acetonitrile and cleaned up with Carb/NH2 solid phase extraction column, In the chromatographic analysis, 3 compounds were separated on an Agilent Eclipse AAA column with the gradient elution using the mobile phases of acetonitrile and water containing 0.1% acetic acid. The extractions were detected by HPLC-MS/MS using external standard method. Results The recoveries of at 3 spiking levels were ranged from 78.8% to 91.5%, 81.3% to 92.8% and 72.8% to 90.0% for imidacloprid, acetamiprid and fiproni, respectively. The relative standard deviations (RSDs) were ranged from 2.6% to 10.6%, 3.7% to 6.6% and 3.6 % to 7.4% for imidacloprid, acetamiprid and fiproni, respectively. The limits of detection (LOQ, S/N≥10) were 0.5 μg/kg. The limits of quantification (LOD, S/N≥3) were 2.0 μg/kg. Conclusion The method is simple, fast and sensitive. It is suitable for the simultaneous determination of imidacloprid, acetamiprid and fipronil residues in tea.