吸头式改良QuEChERS-高效液相色谱-串联质谱法测定蔬菜水果中2种新型吡啶酰胺类农药残留

Determination of 2 kinds of new types picolinamide pesticide residues in vegetables and fruits by pipette-tip based modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  吸头式改良QuEChERS  液相色谱-串联质谱法（LC-MS/MS）  苯哌沙米  吡啶菌酰胺  农药残留

英文关键词:pipette-tip based modified QuEChERS  high performance liquid chromatography-tandem mass spectrometry  fenpicoxamid  florylpicoxamid  pesticide residue

中文摘要:

      目的 建立吸头式改良QuEChERS-高效液相色谱-串联质谱法检测蔬菜水果中苯哌沙米和吡啶菌酰胺两种新型吡啶酰胺类农药残留的方法。方法 蔬果样品中加入QuEChERS盐包后用乙腈振荡提取, 用装有净化吸附材料的一次性吸头净化。采用HPLC column Shim-pack GIST C18色谱柱(100 mm×2.1 mm, 2 μm)分离, 以乙腈-0.1%甲酸水为流动相进行梯度洗脱, 在多反应监测模式下对化合物进行高效液相色谱-串联质谱法检测, 以基质标准曲线外标法定量。结果 两种农药在1~40 ng/mL质量浓度范围内线性关系良好(相关系数r>0.994), 定量限为0.01 mg/kg; 添加水平为0.01~0.10 mg/kg时, 在沃柑、芹菜、苹果、大葱、葡萄干等5种基质中的平均回收率为62.6%~119.1%, 相对标准偏差为1.98%~13.10%。结论 该方法操作简便、快捷高效, 适用于蔬菜水果中两种新型吡啶酰胺类农药残留的快速筛查与准确定量。

英文摘要:

      Objective To establish a method for the determination of fenpicoxamid and florylpicoxamid residues (2 kinds of new types picolinamide pesticide) in vegetables and fruits by pipette-tip based modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry. Methods The vegetable and fruit samples were extracted by shaking with acetonitrile assisted with QuEChERS salts, and purified using disposable tips packed with clean-up sorbents. The analytes were separated by a HPLC Shim-pack GIST C18 column (100 mm×2.1 mm, 2 μm) with acetonitrile-0.1% formic acid in water as the mobile phase by gradient elution mode. The target compounds were analyzed by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode, and quantified by the external standard method with matrix-matched calibration curves. Results The linear relationship between the 2 kinds of pesticides was good within the mass concentration range of 1–40 ng/mL (correlation coefficient r>0.994), and the limits of quantitation were 0.01 mg/kg, could meet the requirements of residue detection. Method validation was conducted in 5 kinds of matrices including Wogan mandarin, celery, apple, scallion and raisin, and the average recovery rates at the spiked levels of 0.01–0.10 mg/kg were 62.6% to 119.1% with the relative standard deviation of 1.98% to 13.10%. Conclusion The proposed method is simple, rapid and efficient, and is suitable for the rapid screening and accurate quantitation of 2 kinds of novel picolinamide pesticide residues in vegetables and fruits.