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分散固相萃取-液相色谱-串联质谱法测定植源性油料油脂中67种除草剂 被引量:2

Determination of 67 herbicides in vegetable oil and fat by liquid chromatography tandem mass spectrometry coupled with dispersive solid phase extraction
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摘要 目的 建立分散固相萃取结合液相色谱-串联质谱同时测定油料油脂中 67 种除草剂残留的检测方法。方法 选取花生、大豆、油菜籽、花生油、大豆油及菜籽油为典型基质试样,经 1% 甲酸-乙腈提取,通过乙二胺基-N-丙基和无水 MgSO分散固相萃取净化。以甲醇和 5 mmol/L 乙酸铵(含 0. 1% 甲酸)为流动相梯度洗脱,采用 C色谱柱分离,ESI 离子源正负离子模式同时进行多反应监测(MRM),基质标准曲线外标法定量。结果 基质加标试验结果表明,0. 000 5~0. 08 mg/L 浓度范围内 67 种除草剂线性良好,决定系数(R~2)均>0. 992,定量限(LOD)为 0. 005~0. 02 mg/kg。3 个加标水平下(LOD、2LOD、10LOD)的回收率为 62. 3%~118. 1%,RSD(n=6)均<15%。结论 本方法稳定性高、特异性强、灵敏、准确、高效,可以用于油料油脂中多种除草剂残留的定性定量检测。 Objective A high-throughput method for simultaneous determination of 67 herbicide residues in oilseeds and oils by liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction was established.Methods Peanut,soybean,rapeseed and their oil were extracted with 1% formic acid-acetonitrile,and then purified by ethylenediamine-N-propyl and anhydrous MgSOdispersed solid phase extraction. Methanol and 5 mmol/L ammonium acetate(containing 0. 1% formic acid)were used as mobile phases for gradient elution. Ccolumn was used for separation,positive and negative ion mode of ESI ion source was used for simultaneous multi-reaction monitoring(MRM). And matrix standard curve external standard method was used for quantification.Results Under different substrates,the linear range of 67 herbicides was from 0. 000 5 to 0. 08 mg/L,the correlation coefficients(R~2)were all above 0. 992,and the limits of detection(LODs)were 0. 005~0. 02 mg/kg. The recoveries of three spiked levels(LOD,2LOD and 10LOD)were between62. 3% and 118. 1% with RSD(n=6)less than 15%.Conclusion This method is stable,specific,sensitive and accurate,and can be used for qualitative and quantitative detection of herbicides in oilseeds and oils.
作者 刘迪 韩莉 余婷婷 张莉 李珉 江丰 王会霞 LIU Di;HAN Li;YU Tingting;ZHANG Li;LI Min;JIANG Feng;WANG Huixia(Hubei Provincial Institute for Food Supervision and Test,Hubei Wuhan 430075,China;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation,Hubei Wuhan 430075,China;Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Hubei Wuhan 430075,China)
出处 《中国食品卫生杂志》 CSCD 北大核心 2022年第4期715-723,共9页 Chinese Journal of Food Hygiene
基金 国家重点研发计划项目(2018YFC1602302) 湖北省重点研发计划项目(2020BCA091)。
关键词 液相色谱-串联质谱 除草剂 油料 油脂 分散固相萃取 Liquid chromatography tandem mass spectrometry herbicide oilseed oil dispersive solid phase extraction
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