以QuEChERS法搭配液相及氣相層析串聯質譜儀建立動物產品中農藥多重殘留檢驗方法

Development of a Multi-residue Method for Pesticides in Foods of Animal Origin Using a Modified QuEChERS Method Combined with LC-MS/MS and GC-MS/MS

本研究係建立動物產品中農藥多重殘留檢驗方法，檢體前處理採用QuEChERS法，先以1%醋酸乙腈溶液進行萃取，再以醋酸鈉及無水硫酸鎂進行鹽析。離心後取乙腈層，添加PSA、C18、石墨碳粉及無水硫酸鎂進行淨化後作為分析檢液。分別以液相層析串聯式質譜儀（high performance liquid chromatograph/tandem massspectrometer, LC/MS/MS）及氣相層析串聯式質譜儀（gas chromatograph/tandem massspectrometer, GC/MS/MS）進行75及68項農藥檢測，層析時間皆在30分鐘內。以豬里肌肉、豬肝臟、雞肉、魚肉作為測試基質，分別添加0.01及0.05 ppm之各項農藥標準品於測試基質中，進行重複性及添加回收率試驗評估，結果88%以上之農藥品項準確度（平均回收率介於60 - 120%之間）及精密度（變異係數在20%以下）良好，84%以上之農藥品項定量極限可達0.01 ppm。

The purpose of this study was to establish a multi-residue method for pesticides in foods of animal origin. The QuEChERS method was used for sample preparation. The foods of animal origin were extracted by acetonitrile containing 1% of acetic acid, and then salted out with anhydrous magnesium sulfate and sodium acetate. After followed centrifugation, the buffered acetonitrile extract was cleaned up via clean-up powder containing primary secondary amine, C18, graphitized carbon and anhydrous magnesium sulfate before analysis. Totally 75 and 68 pesticide compounds were analyzed by LC-MS/ MS (liquid chromatograph/tandem mass spectrometer) and GC-MS/MS (gas chromatograph/tandem mass spectrometer) respectively in a 30 min single run. The recovery and repeatability tests were conducted at the concentrations of 0.01 and 0.05 ppm in four matrices including pork, pork liver, chicken and fish. The validated results showed that good accuracy (recovery between 60 - 120%) and good precision (coefficient of variation ＜ 20%) were found in 88% of all the tested pesticides. Besides, 84% tested pesticides obtained limit of quantitations of 0.01 ppm.