论文部分内容阅读
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0.5μg/kg,定量限为2μg/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。
Objective To establish a method for the determination of three pesticide residues in tea by imidacloprid, acetamiprid and fipronil by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were soaked in water, extracted with acetonitrile, purified by carbonized carbon-amino composite solid-phase extraction cartridges, separated on an Agilent Eclipse AAA column and eluted with 0.1% acetic acid in water and acetonitrile as the mobile phase gradient. Multiple reaction monitoring (MRM) mode detection, external standard quantitative. Results The average recoveries of imidacloprid, acetamiprid and fipronil were 78.8% -91.5%, 81.3% -92.8%, and 72.8% -90.0%, respectively at three levels of addition. The relative standard deviations were 2.6% ~ 10.6%, 3.7% -6.6% and 3.6% -7.4%. The detection limits of acetamiprid, imidacloprid and fipronil were both 0.5μg / kg and the limit of quantification was 2μg / kg. Conclusion The established method is simple, rapid and sensitive. It can meet the requirement of simultaneous detection of imidacloprid, acetamiprid and fipronil in exported tea.