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
作者:
作者单位:

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

作者简介:

刘迪 男 工程师 研究方向为食品质量安全与检测 E-mail: 448301588@qq.com

通讯作者:

中图分类号:

R155

基金项目:

国家重点研发计划项目(2018YFC1602302);湖北省重点研发计划项目(2020BCA091)


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

1.Hubei Provincial Institute for Food Supervision and Test, Hubei Wuhan 430075, China;2.Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food for State Market Regulation, Hubei Wuhan 430075, China;3.Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Hubei Wuhan 430075, China

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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MgSO4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C18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(R2)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。

    Abstract:

    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 MgSO4 dispersed solid phase extraction. Methanol and 5 mmol/L ammonium acetate (containing 0.1% formic acid) were used as mobile phases for gradient elution. C18 column 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 (R2) 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 between 62.3% 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.

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刘迪,韩莉,余婷婷,张莉,李珉,江丰,王会霞.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[J].中国食品卫生杂志,2022,34(4):715-723.

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  • 收稿日期:2021-12-24
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  • 在线发布日期: 2022-08-26
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