QuEChERS结合质谱法测定食用菌中13种农药残留

Determination of 13 kinds of pesticide residues in edible fungi by QuEChERS combined with mass spectrometry

中文关键词:  农药残留  气相色谱-串联质谱法  液相色谱-串联质谱法  食用菌

英文关键词:pesticide residues  gas chromatography-tandem mass spectrometry  liquid chromatography-tandem mass spectrometry  edible fungi

中文摘要:

      目的 建立QuEChERS前处理结合气相色谱-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)测定食用菌中13种农药残留的分析方法。方法 冬菇、草菇和金针菇3种食用菌分别以乙腈提取, 改良的QuEChERS方法净化, 气相色谱-串联质谱法采用Agilent HP-5MS ultralnert柱(30.0 m×250 μm, 0.25 μm)分离, 液相色谱-串联质谱法采用农残色谱柱ACQUITY UPLC?BEH C18 (2.1 mm×50 mm, 1.7 μm)分离, 气相色谱-串联质谱仪和液相色谱-串联质谱仪外标法测定。结果 本方法在5~500 μg/L范围内线性关系良好, 相关系数大于0.99, 在3个水平下13种农药的回收率为68.2%~119.8%, 相对标准偏差(relative standard deviation, RSD)为0.7%~12.5%。结论 此方法适用但不限用于食用菌中13种农药残留的测定。

英文摘要:

      Objective To establish an analytical method for the determination of 13 kinds of pesticide residues in edible fungi by QuEChERS (quick, easy, cheap, effective, rugged and safe) pretreatment, gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Three kinds of edible fungi, including Volvariella edodes, Volvariella volvacea and Flammulina velutipes, were extracted with acetonitrile and purified by improved QuEChERS method, GC-MS/MS was performed on an Agilent HP-5MS ultralner column (30.0 m×250 μm, 0.25 μm), LC-MS/MS was performed on acquity UPLC column ? BEH C18 (2.1 mm×50 mm, 1.7 μm) separation. GC-MS/MS and LC-MS/MS were used for external standard determination. Results The linear relationship was good in the range of 5-500 μg/L, and the correlation coefficients were greater than 0.99. Under 3 levels, the recoveries of 13 pesticides were 68.2%-119.8%, and the relative standard deviations (RSD) were 0.7%-12.5%. Conclusion This method is applicable, which is not limited to the determination of 13 kinds of pesticide residues in edible fungi.