目的研究生物组织中两种混合农药(敌敌畏、克百威)的痕量确认方法； 方法采用时间编程方法和GCCIMS/MS技术，选择在共振方式下，用CI化学源在4min～6.5min以敌敌畏的分子离子(M+1)221为母离子进行MS/MS分析； 结果其碰撞诱导电压为0.5v，产生的二级质谱子离子为141，145；在6.5min～13min以克百威的分子离子(M+1)222为母离子进行MS/MS分析，其碰撞诱导电压为0.4v，产生的二级质谱子离子为165，123；结论排除背景干扰、定性快而准确。

The use of time procedure and gas chromatographyCI/tandem mass spectrometry for qualitative analysis the mixed pesticide (Dichlorvos and Carbofuran) in biological tissue has been studied. In this paper, the time of analysis is divided into two sections and the parent ion and CID voltage have been selected. Parent ion is molecular ion ,when the time is from 4min to 6.5min,Dichlorvos is studied, CID voltage is 0.5v. When the time is from 6.5min to 13min, Carbofuran is studied, CID voltage is 0.4v. It showed that time procedure and MS/MS have many advantages, such as fast, sensitively and eliminating the disturbance in the complex biological tissue.