麦田土壤啶虫脒的残留分析方法

确立乙腈振荡提取、弗罗里硅土SPE小柱净化麦田土壤中啶虫脒残留样本的前处理方法,建立柱程序升温、NPD检测的气相色谱残留样品检测方法。结果表明,在优化的色谱条件下,啶虫脒的色谱保留时间为9.93min,在0.5～200mg/L时,啶虫脒质量浓度与其色谱峰面积在GC-NPD上线性响应良好,回归方程为y=-3 678.37x+3 595.04(r2=0.999 8)。啶虫脒在麦田土壤0.01、0.05、0.1和1.0mg/kg的4个水平的加标回收率均大于75%,各添加水平5次平行测定值的相对标准偏差均小于5%。其准确度和精密度均符合农药残留分析的要求。该色谱条件下仪器的最低检出量为0.62ng,所建立的残留分析方法的最低检测量为0.014mg/kg,可以满足麦田土壤残留的定量检测要求。

Residue Analysis Method of Acetamiprid in Wheat Field Soil

A method for determination acetamiprid residue in wheat field soil has been developed by extraction with acetonitrile,purification with SPE cartridge and determination with GC-NPD.The results showed that under the optimal conditions,the retention time of acetamiprid was 9.93 minutes,the calibration curves showed good linearity(y=-3 678.37x+3 595.04,r2=0.999 8)from 0.5-200 mg/L mass concentration of acetamiprid.The recovery rates were determined in wheat field soil blank spiked at 0.01 mg/kg,0.05 mg/kg,0.1 mg/kg and 1 mg/kg and the overall recovery rates were over 75%,with a relative standard deviation(RSD) less than 5%.The detection limit of acetamiprid was 0.62 ng and the limit of quantification was 0.014 mg/kg in wheat field soil.The results indicated that the method is simple,efficient and reliable,and it’s suitable for the determination of acetamiprid residues in wheat field soil.