色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-负化学离子源质谱测定大豆和玉米中12种三唑类杀菌剂的残留量

沈伟健1*,桂茜雯1,余可垚1,孙宁宁1,赵增运1,沈崇钰1,吴斌1,蒋原1,储晓刚2   

  1. 1.Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • 收稿日期:2008-07-07 修回日期:2008-10-02 出版日期:2009-01-30 发布日期:1983-03-25
  • 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).

Determination of 12 azole fungicide residues in beans and corn by offline disperse solid phase extraction and gas chromatography-negative chemical ionization mass spectrometry

SHEN Weijian1*, GUI Qianwen1, YU Keyao1, SUN Ningning1, ZHAO Zengyun1,   

  1. 1.Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Received:2008-07-07 Revised:2008-10-02 Online:2009-01-30 Published:1983-03-25
  • Contact: SHEN Weijian

PDF

699

被引次数

48

摘要： 建立了一种可用于大豆和玉米中12种三唑类杀菌剂残留量测定的分散固相萃取-气相色谱-负化学离子源质谱方法。样品经含1%冰醋酸的乙腈提取,分散固相萃取法净化,采用气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定与确证,外标法定量。12种农药在50～1000 μg/L范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于8 μg/kg;在10，20和40 μg/kg 3个添加水平下所有农药的回收率为70%～130%,相对标准偏差(RSD)≤13.9%。该方法在检测大豆和玉米基质时无干扰现象出现。

关键词: 大豆, 分散固相萃取, 气相色谱-负化学离子源质谱, 三唑类杀菌剂, 选择离子监测, 玉米

Abstract: A confirmatory method is proposed for the determination of 12 azole fungicide residues in beans and corn with the technique of offline disperse solid phase extraction (DSPE) and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The pesticides interested were extracted from the samples with acetonitrile containing 1% acetic acid and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate plus sodium acetate followed by a simple cleanup step known as dispersive solid-phase extraction. The aliquot was determined and confirmed by GC-NCI/MS using external standard method. The recoveries of all pesticides were between 70% and 130% at the three spiked levels, 10 μg/kg, 20 μg/kg and 40 μg/kg. The relative standard deviations were less than 13.9%. The linearity of method was good from 50 to 1000 μg/L. The limits of quantification (LOQ) were less than 8 μg/kg. The method is selective with no interference and is suitable for the confirmatory of pesticide residues in beans and corn.

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