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两种水产品中农药多残留分析的样品前处理方法及其在111种农药和相关化学品残留同时检测中的应用

苏建峰1,林谷园2,连文浩1,张金虎1,陈冬花1

  

  1. 1.Fujian Fairreach Food Safety Testing Co., Ltd., Fuzhou 350015, China;
    2.Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China
  • 收稿日期:2008-01-16 修回日期:2008-02-21 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 苏建峰

Two sample pretreatment methods and their applications in the determination of 111 pesticides and related
chemicals in aquatic products

SU Jianfeng1, LIN Guyuan2, LIAN Wenhao1, ZHANG Jinhu1, CHEN Donghua1

  

  1. 1.Fujian Fairreach Food Safety Testing Co., Ltd., Fuzhou 350015, China;
    2.Fuqing Entry-Exit Inspection and Quarantine Bureau, Fuqing 350300, China
  • Received:2008-01-16 Revised:2008-02-21 Online:2008-05-30 Published:1984-03-25
  • Contact: SU Jianfeng

摘要:

建立了两种针对水产品中农药多残留分析的快速样品前处理方法,并将其应用于111种农药及相关化学品残留检测。在样品前处理方法Ⅰ中,样品经丙酮-乙酸乙酯-正己烷(体积比为1∶1∶1)混合溶剂提取,乙腈转溶;在样品前处理方法Ⅱ中,样品用乙腈-水溶液均质,超声波辅助提取,液-液分配。两种方法所得到的提取液分别用Envi-18柱和PSA柱净化后进行气相色谱-质谱(GC-MS)分析。采用选择离子扫描(SIM)方式,外标法定量。该方法简便、快速,在优化的样品前处理条件和GC-MS分析条件下,方法的检出限(S/N=3)为0.001~0.026 mg/kg;在加标水平为0.25 mg/kg时,采用方法Ⅰ时的回收率为72%~113%,相对标准偏差(RSDs)为3.4%~12.1%;采用方法Ⅱ时的回收率为51%~127%(其中回收率为70%~120%的占94%),RSDs为3.2%~13.8%。

关键词: 固相萃取, 农药多残留, 气相色谱-质谱法, 水产品 , 样品前处理

Abstract:

Two sample pretreatment methods were developed and applied to determine 111 residues of pesticides in aquatic products. For Method Ⅰ, the residues were extracted from homogenized tissue with acetone-ethylacetate-n-hexane (1∶1∶1, v/v/v), and then were redissolved in acetonitrile; for Method Ⅱ, the residues were extracted from homogenized tissue with acetonitrile-water under ultrasonication, and then were separated by liquid-liquid partition. The supernatants were purified using solid phase extraction (Envi-18 and PSA columns) prior to the GC-MS analysis. The determination was performed in selected ion monitoring (SIM) mode with the external calibration for quantitative analysis. Under the optimal conditions, the detection limits (S/N=3) for residues of pesticides were in the ranges of 0.001-0.026 mg/kg. The recoveries of Method Ⅰ for the spiked standards at concentration of 0.25 mg/kg were 72%-113% with the relative standard deviations (RSDs) of 3.4%-12.1%. The recoveries of Method Ⅱ were 51%-127%, among which the recoveries for 94% pesticides were between 70% and 120% with the RSDs of 3.2%-13.8%.

Key words: aquatic products , gas chromatography-mass spectrometry (GC-MS), multiresidual pesticides, sample pretreatment, solid phase extraction (SPE)