建立了气相色谱-串联质谱测定土壤中有机氯农药的方法,同时测定了上海郊区的20个农业土壤.样品前处理包括加速溶剂萃取(弗罗里硅土池内净化)和凝胶渗透色谱净化在线浓缩.采用多反应监测模式的气相色谱-串联质谱分析有机氯农药,降低了背景干扰,提高了分析的灵敏度.在0.001~2 mg/L的质量浓度范围内,各种农药标准溶液的线性相关系数均大于0.995.分别向3种实际土壤样品中添加农药的混合标准溶液,所测定的有机氯农药的平均回收率为65.9%~140.0%,相对标准偏差为1.5%~20.3%(n=5).有机氯农药的检出限(S/N=3)为0.1~3.0 μg/kg,定量限(S/N=10)为0.3~8.0 μg/kg.实际土壤样品的测定结果表明:六六六(1.82~3.70 μg/kg)和六氯苯(0.94~9.8 μg/kg)有少量检出,滴滴涕的检出率高达100%,其含量范围较宽(1.08~308.76 μg/kg),平均值为53.28 μg/kg,其中85%的样品中滴滴涕含量/(滴滴伊+滴滴滴)含量的比值小于1,表明滴滴涕主要来自于早期的使用.
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