滤过型多次平衡净化结合超高效液相色谱-质谱法测定香蕉和豇豆中10种双酰胺类农药残留

    Rapid multi-plug filtration cleanup method for the determination of diamide pesticide residues in bananas and cowpeas by UHPLC-MS/MS

    • 摘要: 鉴于双酰胺类农药在香蕉、豇豆等果蔬中存在违规使用风险,且现有检测方法对复杂基质净化不彻底,本文建立了滤过型多次平衡净化(multi-plug filtration cleanup,m-PFC)结合超高效液相色谱-串联质谱联用技术同时检测香蕉和豇豆中10种双酰胺类农药残留的方法。香蕉和豇豆样品经过乙腈提取和盐析分层,上清液经装填无水硫酸镁、N-丙基乙二胺(primary secondary amine-Z,PSA-Z)、氨基化-多壁碳纳米管(aminated multi-walled carbon nanotubes,NH2-MWCNTs)和短-氨基化-多壁碳纳米管(s-NH2-MWCNTs)复合净化材料柱,采用多反应监测模式(MRM)分析,使用基质匹配标准曲线外标法定量。结果表明:在0.002~0.2 mg/L质量浓度范围内,10种双酰胺类农药均具有良好的线性关系,决定系数(R2)均高于0.993。添加回收率为71%~119%,相对标准偏差(RSD)为0.9%~5.2% (n = 6),定量限(LOQ)为0.005 mg/kg。该方法无需固相萃取柱活化、平衡、洗脱等复杂步骤,对基质中色素和糖等干扰物吸附效果显著,适用于香蕉和豇豆中双酰胺类农药残留的快速筛查分析。

       

      Abstract: Given the risk of unauthorized use of diamide pesticides in fruits and vegetables such as bananas and cowpeas, and the inadequate purification of complex matrices by existing detection methods, this study established a method for simultaneous detection of 10 diamide pesticide residues in banana and cowpea by multi-plug filtration cleanup (m-PFC) method combined with ultra-high performance liquid chromatography-tandem mass spectrometry. Banana and cowpea samples were extracted with acetonitrile, and inorganic salts were added to the system to separate the extracts into organic and aqueous phases. The upper acetonitrile phase was purified by m-PFC column filled with anhydrous magnesium sulfate, PSA-Z, aminated multi-walled carbon nanotubes (NH2-MWCNTs) and shortened-NH2-MWCNTs (s-NH2-MWCNTs) purification materials. The 10 target compounds were analyzed at multiple reaction monitoring (MRM) mode and were quantified by matrix-matched calibration curves. The results showed that within the range of 0.002 to 0.2 mg/L, the 10 diamide pesticides had good linearity, and the coefficient of determination (R2) was all higher than 0.993. The limit of quantification (LOQ) was 0.005 mg/kg, and the spiked recoveries were 71% to 119%. The relative standard deviation (RSD) ranges from 0.9% to 5.2% (n = 6). The developed method requires no activation, equilibrium, or elution steps, and was proven to be effective in removing the matrix interferences such as pigments and sugars. This method is applicable for rapid screening of diamide pesticide residues in banana and cowpea matrices.

       

    /

    返回文章
    返回