The method for separation of monomethylamine, dimethylamine and trimethylamine by Gas Chromatography (GC) at the same time is studied in this paper. They are detected with Nitrogen phosphorus Detector (NPD). The good separate efficiency and high sensitivities can be got. Their lowest detection limits can reach 0.025mg/L. By the way, their sensitivities on NPD and FID are compared, and the sensitivities on NPD is higher than their on FID. Hence, the former is quite suitable to monitor methal amines with low content in environmental samples.