凝胶渗透色谱气相色谱质谱法检测猪肝中三氟氯氰菊酯农药残留

Determination of pesticide residue cyhalothrin in pig liver by gel permeation chromatography-gas chromatography-mass spectrometry

目的 建立猪肝中三氯氰菊酯农药残留的凝胶渗透色谱净化气相色谱负化学离子源质谱的检测方法.方法 样品经乙酸乙酯为溶剂超声波提取后,凝胶渗透色谱净化处理,采用HP-5MS色谱柱分离,气相色谱-负化学离子源质谱选择离子检测技术检测.结果 0.001、0.005、0.020 mg/kg3个浓度添加回收率在75.3％～]07.6％间,相对标准偏差（RSDs）≤7.1％,最低检出限为0.001 mg/kg.结论 建立的检测方法能够消除油脂类干扰,灵敏度高,选择性好,稳定可靠,适用于猪肝中的三氟氯氰菊酯农药残留的检测.

Objective To establish an assay to determine pesticide residue cyhalothrin in pig liver by gel permeation chroma- tography-gas chromatography-mass spectrometry in negative chemical ionization （GC-MS/NCI） mode. Methods Specimens were subjected to ultrasonic-assistant extraction in ethyl acetate solvent, followed by clean-up treatment by gel permeation chromatography （GPC） . The exact was then separated on HP-5MS column Cyhalothrin was analyzed by gas chromatogra- phy-mass spectrometry operated by negative-ion chemical-ionization（GC-MS/NCI） in selected ion monitoring （SIM） mode. Re- sults Recovery efficiency was 75.3%- 107.6% at three spiked levels （0. 001,0. 005,0. 020 mg/kg） , relative standard devia- tion（RSDs） was all ≤ 7.1%. Limit of detection was 0. 001mg/kg. Conclusion The established method was capable to elimi- nate fatty matrix interference, with high sensitivity, excellent selectivity, stability and reliability, and is applicable for analysis of cyhalothrin residue in pig liver.