食品科学 ›› 2009, Vol. 30 ›› Issue (4): 210-213.doi: 10.7506/spkx1002-6630-200904045

• 分析检测 • 上一篇    下一篇

固相萃取-GC-MS 测定水产品中禾草丹和呋喃硫威残留量

张金虎1,2,陈 晶1,2,林谷园2,林 荆2,赵建晖2,郑向东2   

  1. 1.福建华日食品安全检测有限公司 2.福清出入境检验检疫局
  • 收稿日期:2008-03-09 修回日期:2008-09-26 出版日期:2009-02-15 发布日期:2010-12-29
  • 通讯作者: 张金虎 E-mail:huzi_23_81@fairreach.com;huzi_23_81@163.com

Solid Phase Extraction and Gas Chromatography-Mass Spectrometry Determination of Thiobencarb and Furathiocarb in Aquatic Products

ZHANG Jin-hu1,2,CHEN Jing1,2,LIN Gu-yuan2,LIN Jing2,ZHAO Jian-hui2,ZHENG Xiang-dong2   

  1. 1. Fujian Fairreach Food Safety Testing Co. Ltd., Fuzhou 350015, China ;
    2. Fuqing Entry-exit Inspection and Quarantine Bureau, Fuqing 350300, China
  • Received:2008-03-09 Revised:2008-09-26 Online:2009-02-15 Published:2010-12-29
  • Contact: ZHANG Jin-hu E-mail:huzi_23_81@fairreach.com;huzi_23_81@163.com

摘要:

建立固相萃取-GC-MS 测定水产品中禾草丹、呋喃硫威残留量的分析方法。样品经乙腈均质提取,LCFlorisil(0.5g,6ml)+C18 填料(0.5g )+ 无水硫酸钠(0.5g)固相萃取柱净化,采用GC-MS 全扫描与标准谱库的谱图比较定性,选择离子(SIM)模式定量。两种农药的峰面积与其质量浓度有着良好的线性关系,相关系数为0.997~1.000,最低检测限为0.01mg/kg(S/N>10),样品回收率为82%~110%,RSD 为3.74%~8.18%。该方法操作简便快速、重现性好、净化效果好且成本低,并可以达到日本肯定列表中对两种农药的检测底限,满足进出口要求。

关键词: 固相萃取, 气相色谱-质谱法, 水产品, 残留量

Abstract:

This study aimed to establish an analytical method for the determination of thiobencarb and furathiocarb pesticide residues in aquatic products using solid-phase extraction (SPE) and gas chromatograph-mass spectrometry. Extraction with acetonitrile was used for sample preparation. The prepared sample was cleaned-up using SPE column (filled with 0.5 of C18 and 5 g of Na2SO4, and then eluted with 10 ml of acetonitrile). The total ion current (TIC) was identified by a spectrum library search. Selected ion monitoring (SIM) was used as a quantitative method. The two pesticides show good linearity in a detected concentration range with good correlation coefficient (r=0.997 to 1.000). The method recoveries are generally from 82% to 110% with relative standard deviation (RSD) of 3.74% to 8.18% and the limit of detection is 0.01 mg/kg (S/N >10). The method is effective, fast, accurate and economical, and it can meet the detection demand for import and export.

Key words: SPE, GC-MS, aquatic products, residue

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