气相色谱-三重四极杆质谱法测定粮谷中咪鲜胺及其代谢物残留量

Determination of prochloraz and metabolites residue in grains by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  气相色谱-三重四极杆质谱法  多重反应离子监测模式  粮谷  咪鲜胺及其代谢产物  残留

英文关键词:gas chromatography-triple quadrupole mass spectrometry  multiple reaction ion monitoring mode  grains  prochloraz and its metabolites  residue

中文摘要:

      目的 建立粮谷中咪鲜胺及其代谢产物2,4,6-三氯苯酚残留测定的气相色谱-三重四极杆质谱(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)的分析方法。方法 试样加水涡旋混匀经1%乙酸乙腈提取, 通过N-丙基乙二胺(primary secondary amine, PSA)、C18吸附剂、及增强型脂质去除产品(enhanced mode removal-lipid, EMR-lipid)净化提取液, 以气相色谱-三重四极杆质谱多重反应离子监测模式(multiple reaction monitoring, MRM)检测, 外标法定量。结果 2,4,6-三氯苯酚在0.25~10.0 μg/L、咪鲜胺在2.5～100.0 μg/L范围下均具有良好的线性关系, 相关系数(r2)均大于0.999, 2,4,6-三氯苯酚在0.5、1.0、2.0、5.0 μg/kg的添加水平下回收率在80.2%～118.6%内, 相对标准偏差在1.8%～8.8%内, 定量限为0.5 μg/kg; 咪鲜胺在5.0、10.0、20.0、50.0 μg/kg的添加水平下回收率在80.6%～115.5%内, 相对标准偏差在1.8%～5.9%内; 定量限为5.0 μg/kg。结论 该方法操作高效快捷、检测灵敏度高, 抗基质效应强, 适用于快速处理高通量粮谷中咪鲜胺及其代谢产物的残留量检测。

英文摘要:

      Objective To establish an analytical method for the determination of prochloraz and its metabolites 2,4, 6-trichlorophenol residues in grain by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods The sample was mixed with water vortex and extracted by ethyl acetate, the extract was purified by primary secondary amine (PSA), C18 adsorbent and enhanced mode removal lipid (EMR lipid), determined by multiple reaction ion monitoring mode (MRM) of GC-MS/MS, and quantified by external standard method. Results The 2,4,6-trichlorophenol has a good linear relationship in the range of 0.25?10.0 μg/L and prochloraz in the range of 2.5?100.0 μg/L, and the correlation coefficients (r2) were all higher than 0.999. The spiked recoveries of 2,4,6-trichlorophenol at 0.5, 1.0, 2.0 and 5.0 μg/kg were within 80.2%?118.6%, and the relative standard deviation (RSD) was within 1.8%?8.8%, with the quantitative limit of 0.5 μg/kg. The spiked recoveries of prochloraz at 5.0, 10.0, 20.0, and 50.0 μg/kg were within 80.6%?115.5%, and the RSD was within 1.8%?5.9%, with the quantitative limit of 5.0 μg/kg. Conclusions This method is efficient and fast in operation, high in detection sensitivity, and strong in anti-matrix effect, and is suitable for the rapid determination of prochloraz and its metabolite residue detection in large quantities of grains.