色谱

色谱 ›› 2017, Vol. 35 ›› Issue (7): 778-784.DOI: 10.3724/SP.J.1123.2017.01012

• 技术与应用 • 上一篇    

气相色谱-三重四极杆质谱法测定植物源性食品中20种拟除虫菊酯类农药残留

曲栗1,2, 李优1, 曾静1, 盛永刚1, 伊雄海1, 程甲1   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 复旦大学, 上海 200032
  • 收稿日期:2017-01-11 出版日期:2017-07-08 发布日期:2013-10-18
  • 通讯作者: 曲栗,Tel:(021)38620529,E-mail:qul@shciq.gov.cn
  • 基金资助:

    上海市技术贸易措施应对专项（13TBT002）；国家质检总局科技项目（2015IK012）.

Determination of 20 pyrethroid residues in vegetable foods by gas chromatography-tandem mass spectrometry

QU Li1,2, LI You1, ZENG Jing1, SHENG Yonggang1, YI Xionghai1, CHENG Jia1   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Fudan University, Shanghai 200032, China
  • Received:2017-01-11 Online:2017-07-08 Published:2013-10-18
  • Supported by:

    Shanghai Project for Technical Barriers to Trade (No.13TBT002);Science and Technology Project of General Administration of Quality Supervision,Inspection and Quarantine (No.2015IK012).

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被引次数

1

摘要：

建立了气相色谱-三重四极杆质谱（GC-MS/MS）同时测定植物源性食品中20种拟除虫菊酯类农药残留量的方法。样品经丙酮-正己烷（1：1，v/v）提取，活性炭小柱净化，外标法定量。目标物在0.005~1.0 mg/L范围内呈良好的线性相关，相关系数（r2）均不小于0.990，方法的检出限（信噪比（S/N） > 3）均为2.0 μ g/kg，定量限（S/N > 10）均为5.0 μ g/kg。分别在11种基质中做低、中、高3个添加水平的加标回收试验，该方法的平均回收率为75.2%~107%，相对标准偏差（RSD，n=6）为3.08%~12.1%。该方法前处理步骤简便，特异性强，适用范围广，适用于植物源性食品中20种拟除虫菊酯类农药的筛查和确证。

关键词: 拟除虫菊酯类农药残留, 气相色谱-三重四极杆质谱法, 植物源性食品

Abstract:

A method of gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the simultaneous determination of 20 pyrethroid residues in vegetable foods. The samples were extracted by acetone-n-hexane (1:1, v/v), cleaned up by activated charcoal column and quantified by external standard method. The correlation coefficients (r2) of all the 20 pyrethroid pesticides in the range of 0.005-1.0 mg/L were not less than 0.990. The limits of detection (LODs) were 2.0 μ g/kg when signal/noise (S/N) > 3. The limits of quantification (LOQs) were 5.0 μ g/kg (S/N > 10). For recovery test, there were three levels (low, medium and high) spiked in 11 matrices. The average recoveries of the method were 75.2%-107% and the relative standard deviations (RSDs, n=6) were 3.08%-12.1%. The results demonstrated that the method is simple and has specific pretreatment steps. The method is suitable for the screening and confirmation of the 20 pyrethroid pesticides in vegetable foods.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), pyrethroid residues, vegetable foods

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