谷物及土壤中氟虫腈残留分析方法研究

A Method for Determination of Fipronil Residue in Cereal and Soil

氟虫腈是一种苯基吡唑类高效杀虫剂,用于防治多种害虫。为有效监测农产品中氟虫腈残留,建立了稻米、小麦、玉米等谷物及水稻秸秆和土壤中氟虫腈残留量检测方法。样品采用乙腈为提取溶剂,超声波振荡提取,谷物及秸秆提取液经柱层析净化,采用气相色谱电子俘获检测器检测。研究结果表明,在0.01～0.5mg/kg的添加浓度范围内,氟虫腈的平均回收率在80.60%～99.66%之间,相对标准偏差低于9%,最小检测浓度为0.01mg/kg。本文作者所建立的氟虫腈残留分析方法具有简便、快速的特点,方法的灵敏度与准确度均符合农药残留分析要求。

A method was developed to analysis residue of fipronil in cereal and soil. After acetonitrile was added, the samples were sonicated in an ultrasonic water bath and then centrifuged, filtered, and cleaned up by a column containing neutral alumina and active carbon, successive eluted by ethyl acetate/n-hexane （3：5, V/V）. The pesticide residues were determined by gas chromatography with electron-capture detection. Recoveries at spiked concentrations between 0.01 to 0.5 mg/kg were 80.60%-99.66% with RSDs less than 9%. The limit of detection was 0.01 mg/kg. The sensitivity and accuracy of the proposed method were fit for analysis of pesticide residue in cereal and soil.