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  

Determination of 67 herbicides in vegetable oil and fat by liquid chromatography tandem mass spectrometry coupled with dispersive solid phase extraction

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)

机构地区：[1]湖北省食品质量安全监督检验研究院,湖北武汉430075 [2]国家市场监管重点实验室动物源性食品中重点化学危害物检测技术,湖北武汉430075 [3]湖北省食品质量安全检测工程技术研究中心,湖北武汉430075

出　　处：《中国食品卫生杂志》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)。

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.

关 键 词：液相色谱-串联质谱 除草剂 油料 油脂 分散固相萃取 

分 类 号：R155[医药卫生—营养与食品卫生学]