改进的石墨烯分散固相萃取-液相色谱-串联质谱法测定茶叶中15种氨基甲酸酯类农药的残留量

Determination of 15 kinds of carbamate pesticides in tea by improved graphene dispersive solid-phase extraction-liquid chromatography-tandem mass spectrometry

中文关键词:  石墨烯  分散固相萃取  茶叶  氨基甲酸酯类农药

英文关键词:graphene  dispersive solid-phase extraction  tea  carbamate pesticides

中文摘要:

      目的 以石墨烯为吸附剂, 建立分散固相萃取-液相色谱-串联质谱法测定茶叶中多种氨基甲酸酯类农药残留量。方法 样品采用水浸泡、乙腈提取, 石墨烯作为吸附剂祛除杂质后, 液相色谱-串联质谱仪测定, 外标法定量。结果 15种氨基甲酸酯类农药在0.001~0.02 μg/mL范围内线性良好, 相关系数均大于0.990, 且定量限均可达到0.01 mg/kg。空白样品在0.01、0.02和0.10 mg/kg 3个添加水平下, 回收率范围为61%~106%, 相对标准偏差为4.6%~13%。结论 本方法操作简便、快速、成本较低, 适用于茶叶中氨基甲酸酯类农药的检测。

英文摘要:

      Objective To establish a method for determination of 15 kinds of carbamate pesticides in tea by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with dispersive solid-phase extraction using graphene as adsorbent. Methods The samples were rehydrated, extracted with acetonitrile, and cleaned up by graphene. The determination was carried out by LC-MS/MS with external standard method for quantification. Results The calibration curves were linear in the range of 0.001~0.02 μg/mL with the correlation coefficients above 0.990, and the limits of quantification for 15 kinds of carbamate pesticides were 0.01 mg/kg. The spiked recoveries for 15 kinds of carbamate pesticides were in the range of 61%~106% at 3 spiked levels of 0.01, 0.02 and 0.10 mg/kg, with the relative standard deviations of 4.6%~13%. Conclusion This method is simple, rapid and less expensive, which is suitable for the determination of carbamate pesticides in tea.