[ Objective ] The research aimed to establish a new determination method of chlorpyrifos-methyl. [Method] In NaOH media, the chemiluminescence reaction between luminol and H_2O_2 was strengthened by chlorpyrifos-methyl. And the light intensity had better linear relationship with the concentration of chlorpyrifos-methyl. Based on its properties,chlorpyrifos-methyl could be determined by using H_2O_2 luminol flow injection chemiluminescence method. [ Result ] Under the determined optimized conditions, the linear range of determining chlorpyrifos-methyl was 3×10~(-7)～3×10~(-5)g/ml and the detection limit was 3.8 × 10~(-8) g/ml. The relative standard deviation (RSD) was 2. 83% (n = 11) for 1 × 10~(-6) g/ml chlorpyrifos-methyl. [Conclusion]The chemiluminescence spectrum and ultraviolet-visible spectrum of the system were studied and the possible mechanism of the chemiluminescence was proposed. The method was applied to the chlorpyrifos-methyl determination in synthetic samples, with satisfactory results.%[目的]建立测定甲基毒死蜱的新方法.[方法]在NaOH介质中,过氧化氢氧化鲁米诺产生化学发光,甲基毒死蜱对该发光反应有增强作用且发光强度与甲基毒死蜱的浓度有较好的线性关系,基于此性质,用过氧化氢-鲁米诺流动注射化学发光法测定甲基毒死蜱.[结果]在该试验确定的优化条件下,测定甲基毒死蜱的线性范围为3×10~(-7)～3×10~(-5)g/ml,检出限为3.8×对10~(-8)g/ml，对浓度1×10~(-6)g/ml的甲基毒死蜱进行11次平行测定,其RSD为2.83%.[结论]研究了体系的化学发光光谱及紫外可见光谱特性,提出了发光反应可能的机理.将该法用于合成样品中甲基毒死蜱的测定,获得满意结果.
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