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多壁碳纳米管分散固相萃取-LC-MS/MS法分析烟草中114种农药残留

Simultaneous Determination of 114 Pesticide Residues in Tobacco by Multi-walled Carbon Nanotube-based Dispersive Solid Phase Extraction and LC-MS/MS

  • 摘要: 建立了一种以多壁碳纳米管(MWCNTs)为吸附剂的分散固相萃取(DSPE)、液相色谱-串联质谱(LC-MS/MS)测定烟草中114种农药残留的分析方法。通过优化实验,选择并确定了MWCNTs的型号和用量,在QuEChERS方法的基础上改善了样品净化效果。结果表明:①以外径> 50 nm、用量5 mg的MWCNTs为净化剂材料,可以获得比N-丙基乙二胺(PSA)更好的净化效果。②工作曲线线性良好(r2 > 0.999),3个添加水平(0.02,0.05,0.20 mg/kg)的平均回收率为69%~119%,相对标准偏差为1%~19%,方法定量限(LOQ)在0.2~40.0μg/kg之间。该方法准确度高、灵敏度好、操作简便,适合用于烟草样品中114种农药残留的检测。

     

    Abstract: A method combining dispersive solid phase extraction(DSPE), wherein multi-walled carbon nanotubes(MWCNTs) were used as adsorption material, with liquid chromatographytandem mass spectrometry(LC-MS/MS) was developed for simultaneously determining 114 pesticide residues in tobacco. The type and adding rate of MWCNTs were optimized by experiments, and the purification of samples was improved by Qu ECh ERS method. The results showed that: 1) It was more efficient using 5 mg MWCNTs of above 50 nm in external diameter than using N-Propylethane-1, 2-diamine(PSA) in sample purification. 2) The calibration curve presented good linearity(r2 > 0.999). The average recoveries at spiked levels of 0.02, 0.05 and 0.20mg/kg ranged from 69% to 119% with the relative standard deviations of 1%-19%, and the LOQs of the method were in the range of 0.2-40.0 g/kg. The developed method is accurate, sensitive, convenient, and suitable.

     

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