提出了动物组织中沙蚕毒素类农药残留的快速分析方法.用快速溶剂萃取仪以环己烷、丙酮及二氯甲烷(1∶1∶1体积混合)的混合溶剂,将血液、肝等动物组织样品中沙蚕毒素类农药萃取入有机相,提取液在水浴中于40 ℃蒸干后用甲醇定容至2 mL,用气相色谱-质谱/质谱法测定.结果表明:杀虫双在2.4~7.2 mg·L-1范围内呈线性,检出限(3S/N)为48 μg·L-1:杀虫脒在1.2~7.2 mg·L-1范围呈线性,检出限(3S/N)为8 μg·L-1.对上述2种沙蚕毒素农药分别在血液及肝脏样品用标准加入法对方法作回收及精密度试验,结果为:血样中的平均回收率依次为92.0%,93.0%,相对标准偏差为2.1%,3.5%,肝脏样品中平均回收率依次为90.0%,92.7%,相对标准偏差为4.5%,6.9%.

A rapid method for determination of nereistoxin pesticides in animal tissues by GC-MS/MS with accelerated solvent extracted was proposed.The animal tissue sample (e.g.blood,liver and etc.) was extracted with a mixture of cyclohexane,acetone and dichloromethan (mixed in the ratio of 1 to 1 to 1 by vol.) to transfer the pesticides into the organic phase.On-line purification with aluminum oxide was used to remove impurities from the extract.The extract was evaporated to dryness in a water bath at 40 ℃,and the residue was taken up with 2.0 mL of methanol,which was used for GC-MS/MS determination.Two pesticides,i.e.,bisultap and chlordimeform,were determined by the proposed method,giving linearity ranges between 2.4-7.2 mg·L-1 and 1.2-7.2 mg·L-1 respectively.Detection limits (3S/N) of 48 μg·L-1 (for bisultap) and 8 μg·L-1 (for chlordimeform) were obtained.Recovery and precision were tested by the standrad addition method and the results obtained were as follows:values of average recovery:92.0% and 90.0% for bisultap in blood and liver samples,93.0% and 92.7% for chlordimeform in blood and liver samples respectively;values of RSD′s (n=6):2.1% and 4.5% in the former case;3.5% and 6.9% in the latter case.