• 中文核心期刊
  • CSCD来源期刊
  • 中国科技核心期刊
  • CA、CABI、ZR收录期刊

纳米四氧化三铁在茶叶农药残留检测中的应用及方法优化

Optimized Application of Fe3O4 Nanoparticles for Pesticide Detection in Tea

  • 摘要:
      目的  建立高效液相色谱-串联质谱测定茶叶中7种农药的分析方法,提高检测效率、降低检测成本。
      方法  以多菌灵、嘧霉胺、三环唑、吡虫啉、啶虫脒、灭多威、噻虫嗪等7种农药为目标物,纳米Fe3O4作为净化材料,考察其对茶叶中色素的去除效果,并进行方法评价。
      结果  茶叶基质中纳米Fe3O4组的7种农药回收率明显高于石墨化碳黑(GCB)组,最佳用量为300 mg。通过Phenomenex Luna C8 (150 mm × 2.0 mm × 3.0 µm)色谱柱梯度洗脱,流动相A为含0.1 %甲酸和5 mmol·L−1乙酸铵的水,B为乙腈,多反应监测模式(MRM)监测。在0 ~ 50 µg·L−1方法线性良好,相关系数(R2)大于0.995;在5、10、50 ng·g−1添加水平下回收率为71.6%~107.7 %,相对标准偏差(RSD)为3.95%~13.62 %,检出限为0.15~0.60 µg·kg−1,定量限为0.5~2.0 µg·kg−1
      结论  基于纳米Fe3O4建立了高效液相色谱-串联质谱测定茶叶中农药残留的分析方法,该方法稳定、可靠,有效提高了茶叶中农药残留检测的回收率,降低了检测成本。

     

    Abstract:
      Objective  A newly modified analytical method for detecting pesticide residues in tea was developed to improve test efficiency and reduce cost.
      Method   Fe3O4 nanoparticles were used to replace the conventional pigment-removing material prior to measurements on pesticide residues, including carbendazim, pyrimethanil, tricyclazol, imidachloprid, acetamiprid, methomyl, and thiamethoxam, in tea by liquid chromatography-tandem mass spectrometry. The methodology was evaluated according to its applicability and validated in a spiked residue test.
      Result  The recovery rates on the 7 pesticides under the modified method using 300 mg Fe3O4 nanoparticles for pigment removal pretreatment were higher than graphitizing with carbon black (GCB). The pigment-removed tea extracts were separated with a Phenomenex Luna C8 (150 mm × 2.0 mm × 3.0 µm) by using 0.1 % formic acid and 5 mmol·L-1 ammonium acetate as Phase A and acetonitrile as Phase B for the mobile phase prior to the tandem mass spectrometric analysis under the multiple reaction monitoring mode with external standards. A linearity on the measurements by the new method was achieved within the pesticide concentrations of 0-50 µg·L-1 showing correlation coefficients (R2) greater than 0.995 for all 7 pesticides. On 5, 10, and 50 ng·g-1 spiked pesticide samples, average recovery rates of the new method ranged from 71.6 % to 107.7 % with relative standard deviations of 3.95%-13.62 %. The limits of detection (LOD) on the pesticides by the method were between 0.15 µg·kg-1 and 0.60 µg·kg-1, and the limits of quantitation (LOQ) between 0.5 µg·kg-1 and 2.0 µg·kg-1.
      Conclusion  The newly developed pesticide detection method was stable, repeatable, and accurate for the designed purpose.

     

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