固相萃取-气相色谱-串联质谱法测定大蒜中19种有机磷农药残留量

李萍萍; 吴小芳; 万瑶; 乐渊

doi:10.3969/j.issn.1008-7303.2014.06.14

固相萃取-气相色谱-串联质谱法测定大蒜中19种有机磷农药残留量

doi: 10.3969/j.issn.1008-7303.2014.06.14

1.
中国热带农业科学院分析测试中心, 海口 571101

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出版历程
- 收稿日期: 2014-07-02
- 修回日期: 2014-08-01
- 刊出日期: 2014-12-12

Determination of 19 organophosphorus pesticide residues in garlic using solid-phase extraction and gas chromatography-tandem mass spectrometry

1.
Analysis and Test Center, Chinese Academy of Tropical Agricultural Sciences, Haikou 571101, China

摘要

摘要: 建立了采用固相萃取(SPE)结合气相色谱-三重四级杆串联质谱(GC-MS/MS)测定大蒜中19种有机磷农药残留量的方法。采用V(乙酸):V(乙酸乙酯)=1:99混合溶液提取,Carbon/NH2 固相萃取小柱净化,在GC-MS/MS的多反应(MRM)模式下进行外标法定量。结果表明:在0.04～0.8 mg/L范围内,19种农药的色谱峰面积与其相应的质量浓度间均呈良好的线性关系;所有供试农药检测方法的定量限(LOQ)均低于0.01 mg/kg; 在0.01～0.2 mg/kg添加水平下,19种农药的平均回收率在68.0% ～130% 之间,相对标准偏差(RSD)≤15.6%。该方法背景干扰少,灵敏度高,适合基质复杂的大蒜样品中有机磷农药残留量的检测。
- 气相色谱-串联质谱 /
- 固相萃取 /
- 大蒜 /
- 有机磷农药 /
- 残留
Abstract: A method was developed for determination of 19 organophosphorus pesticides in garlic using solid-phase extraction (SPE) and gas chromatography-tandem mass spectrometry (GC-MS/MS). The pesticides were extracted with V(acetic acid):V(ethyl acetate)=1:99, and then cleaned up on a carbon/NH2 SPE column. The extracts were determined by mode of multiple reaction monitoring (MRM) of GC-MS/MS using external standard method quantification. The linearity range of the method between 0.04 mg/L and 0.8 mg/L was satisfying and the limit of quantitation (LOQ) of all pesticides were low than 0.01 mg/kg. The recoveries of all pesticides at the spiked level of 0.01 to 0.2 mg/kg in garlic matrices were in the range of 68.0% to 130%, with relative standard deviations (RSDs) less than 15.6%. It is demonstrated that this method is sensitive with low background, showing its potential inanalysis of organophosphorus pesticide residues in garlic.
- gas chromatography-tandem mass spectrometry (GC-MS/MS) /
- solid-phase extraction (SPE) /
- garlic /
- organophosphorus pesticide /
- residue

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参考文献(19)

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