固相萃取-气相色谱-质谱联用法筛查食用菌中的农药残留

Screening of Multi-Pesticide Residues in Edible Fungi by SPE and GC-MS

采用气相色谱-质谱联用结合NAGINATA^TM软件建立了筛查食用菌中多种农药残留的分析方法。采用乙腈提取,Carbon-NH2固相萃取小柱净化,气相色谱-质谱联用检测后NAGINATA^TM软件全智能分析,对照每个化合物的质谱质量精度以及质谱谱图的谱库给出匹配度,通过保留时间锁定对化合物作定性判断。结果表明,18种农药在香菇中检出限为0.001-0.050 mg/kg;平均回收率为77%-110%;相对标准偏差为1.1%-6.9%。应用所建立的方法对35个市售食用菌样品进行了筛查,检测出2种农药残留,残留量均低于GB 2763—2014《食品中农药最大残留限量》的限量。该方法操作便捷、快速高效,适用于食用菌中农药多残留的快速筛查。

A gas chromatography-mass spectrometry（GC-MS） combined with NAGINATA^TM software method was developed for screening multi-pesticide residues in edible fungi. The pesticide residues in samples were extracted with acetonitrile, cleaned up with Carbon-NH2 solid-phase extractor, detected by GC-MS, and finally analyzed by NAGINATA^TM software. Based on the quality precision and retention time of each compound, the possible hazardous chemical compounds were screened out by matching mass spectra with mass spectral library. Under the optimal conditions, the limits of detection（LOD） of the established method were in the range of 0.001–0.050 mg/kg, and the average recovery rates for 18 pesticide residues spiked in a blank sample were 77%–110% with relative standard deviations（RSDs） of 1.1%–6.9%. The method was applied on 35 edible fungi purchased from local markets, and two pesticides were detected. which were below the maximum residue limit（MRL） stipulated by the Chinese national standard GB 2763—2014. This method proved to be rapid, simple, efficient and suitable for the fast screening of pesticide residues in edible fungi.