食品科学

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凝胶渗透色谱-超高效液相色谱-串联质谱测定茶叶中吡虫啉和啶虫脒

段 兵,何太喜,范媛媛,郑 冰   

  1. 顺德出入境检验检疫局,广东 顺德 528303
  • 出版日期:2016-02-25 发布日期:2016-02-23
  • 通讯作者: 郑 冰

Determination of Imidacloprid and Acetamiprid in Tea by Gel Permeation ChromatographyUltra Performance Liquid Chromatography-Tandem Mass Spectrometry

DUAN Bing, HE Taixi, FAN Yuanyuan, ZHENG Bing   

  1. Shunde Entry-Exit Inspection and Quarantine Bureau, Shunde 528303, China
  • Online:2016-02-25 Published:2016-02-23
  • Contact: ZHENG Bing

摘要:

建立用凝胶渗透色谱-超高效液相色谱-串联质谱仪测定茶叶中吡虫啉和啶虫脒残留的方法。样品经乙酸乙酯-环己烷(1∶1,V/V)溶液涡旋混匀后超声提取,经凝胶渗透色谱净化后,采用超高效液相色谱-串联质谱仪测定。结果显示,2 种农药在0.5~100 μg/L范围内线性良好,相关系数R2均大于0.99。吡虫啉和啶虫脒的检出限分别为2.0 μg/kg和1.0 μg/kg,定量限分别为5.0 μg/kg和3.0 μg/kg。吡虫啉和啶虫脒在3 个水平的加标平均回收率为76.94%~91.68%,相对标准偏差为2.67%~7.90%。

关键词: 吡虫啉, 啶虫脒, 凝胶渗透色谱, 超高效液相色谱-串联质谱, 茶叶

Abstract:

A method was developed for the determination of imidacloprid and acetamiprid residues in tea using gel
permeation chromatography (GPC)-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
Tea samples were extracted with acetonitrile under ultrasonic irradiation and cleaned up with GPC. The elution fractions
at retention times between 10 and 17 min were collected for subsequent analysis. The portions collected from GPC were
blown to dryness under nitrogen gas stream and then the residue was re-dissolved with acetonitrile-0.1% formic acid. The
calibration curves developed were linear in the range of 0.5–100 μg/L with a correlation coefficient higher than 0.99. The
limits of detection (LODs) for imidacloprid and acetamiprid were 2.0 and 1.0 μg/kg, and the limits of quantification (LOQs)
were 5.0 and 3.0 μg/kg, respectively. The average recoveries of the method at three different spiked levels ranged from
76.94% to 91.68% for imidacloprid and acetamiprid with relative standard deviations (RSDs) from 2.67% to 7.90%.

Key words: imidacloprid, acetamiprid, gel permeation chromatography (GPC), ultra performance liquid chromatographytandemmass spectrometry (UPLC-MS/MS), tea

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