色谱

色谱

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分散固相萃取气相色谱-负化学离子源质谱法测定大豆和玉米中20种农药的残留量

李春风1,2,沈伟健2*,蒋原2,沈崇钰2,赵增运2,余可垚2,桂茜雯2,孙宁宁2,袁宗辉1   

  1. 1.Institute of Veterinary Drug, Huazhong Agricultural University, Wuhan 430070, China; 2.Food Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • 收稿日期:2008-08-13 修回日期:2008-10-13 出版日期:2009-03-30 发布日期:1982-12-25
  • 通讯作者: 沈伟健
  • 基金资助:
    国家“十一五”科技支撑计划项目(2006BAK02A08)和质检公益性行业科研专项项目(200810099).

Determination of 20 kinds of pesticide residues in soybeans and corn using gas chromatography-negative chemical ionization mass spectrometry coupled with offline disperse solid-phase extraction

LI Chunfeng1,2, SHEN Weijian2*, JIANG Yuan2, SHEN Chongyu2, ZHAO Zengyun2, YU Keyao2, GUI Qianwen2, SUN Ningning2, YUAN Zonghui1   

  1. 1.Institute of Veterinary Drug, Huazhong Agricultural University, Wuhan 430070, China; 2.Food Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2008-08-13 Revised:2008-10-13 Online:2009-03-30 Published:1982-12-25
  • Contact: SHEN Weijian

PDF

903

被引次数

72

摘要： 建立了一种大豆和玉米中20种农药残留量的分散固相萃取气相色谱-负化学离子源质谱分析方法。样品经乙腈提取并浓缩后加入N-丙基乙二胺（PSA）、石墨化碳黑和C18 3种填料进行分散固相萃取净化,气相色谱-负化学离子源质谱分时段选择离子监测技术测定与确证,外标法定量。所有农药在20～400 μg/L范围内线性均良好;方法的定量限(LOQ)均不高于2 μg/kg;在5,10和20 μg/kg 3个添加水平下所有农药的平均回收率均处于70%～130%之间,相对标准偏差(RSD)低于17%;运用该方法检测大豆和玉米样品时没有干扰现象。

关键词: 大豆, 分散固相萃取, 农药残留, 气相色谱-负化学离子源质谱法, 选择离子监测, 玉米

Abstract: A method was developed for the determination of 20 kinds of pesticide residues in soybeans and corn with the technique of offline disperse solid-phase extraction and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The pesticides interested were extracted twice from the samples with acetonitrile. The combined extract was concentrated to dryness and redissolved in acetonitrile, then cleaned up by dispersive solid-phase extraction with sorbents of N-propyl ethylene diamine （PSA）, graphited carbon black, and C18, and determined and confirmed by GC-NCI/MS. The recoveries of all pesticides were in the range of 70%-130% at three spiked levels （5, 10 and 20 μg/kg）, and the relative standard deviations were below than 17%. The linearity of the method was good in the concentration range of 20-400 μg/L, and limits of quantification (LOQs) were no more than 2 μg/kg. The method is selective well with no interference and suitable for the confirmatory of pesticide residues in soybeans and corn.

Key words: corn , disperse solid-phase extraction, pesticide residues, selected ion monitoring, soybean, gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS)