气相色谱-串联质谱法和液相色谱-串联质谱法快速测定葡萄中45种农药残留

Rapid determination of 45 kinds of pesticide residues in Vitis vinifera by gas chromatography-tandem mass spectrometry and liquid chromatography-tandem mass spectrometry

中文关键词:  多农药残留  QuEChERS  气相色谱-串联质谱法  液相色谱-串联质谱法  葡萄  快速测定

英文关键词:multiple pesticide residues  QuEChERS  gas chromatography-tandem mass spectrometry  liquid chromatography-tandem mass spectrometry  Vitis vinifera  rapid determination

中文摘要:

      目的 建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)和液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速检测葡萄中45种农药残留的分析方法。方法 葡萄样品使用乙腈经振荡提取和超声辅助提取后, 上清液用混合吸附填料进行分散固相萃取净化, 高速离心后过滤膜, 分别用GC-MS/MS的选择反应监测(selected reaction monitoring, SRM)模式和LC-MS/MS的多反应监测(multiple reaction monitoring, MRM)模式进行检测。结果 溴氰菊酯在0.1~1.0 mg/kg、克菌丹在0.2~3.0 mg/kg、甲霜灵等28种农药在0.04~1.00 mg/kg、甲氨基阿维菌素苯甲酸盐等15种农药在0.1~1.0 mg/kg的浓度范围内具有良好的线性关系, 相关系数达到0.99以上。检出限为0.00020~0.05000 mg/kg, 定量限为0.00050~0.15000 mg/kg。45种农药在3个不同加标水平的平均加标回收率为70.3%~117.0%, 相对标准偏差为0.01%~14.30%。结论 本方法无需复杂样品前处理设备即可实现葡萄中45种农药残留的快速检测, 准确性好, 操作简便, 能够很好满足葡萄中多农药残留日常监测分析工作的要求。

英文摘要:

      Objective To establish a method for the rapid determination of 45 kinds of pesticides residues in Vitis vinifera by gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The Vitis vinifera samples were first extracted with acetonitrile by vibration and ultra-sonic. Then the mix adsorbents were used in dispersive solid phase extraction to purify the extract. After high speed centrifugation and filtration, the samples were detected by GC-MS/MS using selected reaction monitoring (SRM) mode, and LC-MS/MS using multiple reaction monitoring (MRM) mode. Results Deltamethrin exhibited good linearity within the concentration range of 0.1 to 1.0 mg/kg, while captan showed linearity within the range of 0.2 to 3.0 mg/kg, 28 kinds of pesticides including metalaxyl showed good linear relationships within the concentration range of 0.04–1.00 mg/kg, and 15 kinds of pesticides including emamectin benzoate showed good linear relationships within the concentration range of 0.1–1.0 mg/kg, with correlation coefficients reached 0.99 or above. The limits of detection were in the range of 0.00020–0.05000 mg/kg, the limits of quantitation were in the range of 0.00050–0.15000 mg/kg. The spiked recoveries at 3 levels of 45 kinds of pesticides were in range of 70.3%–117.0%, the relative standard deviations were in range of 0.01%–14.30%. Conclusion With features such as accuracy and easy operation, this method can be used to fast determination of 45 kinds of pesticides in Vitis vinifera without any special samples pretreatment apparatus, and also satisfies the requirement of pesticide routine analysis.