A coupled column system was developed for the simultaneous determination of both rodenticides fluoroacetamide and tetramine in this paper by gas chromatography/mass spectrometry (GC/MS). A short length of strong polar column (1.5 m of Innowax) was coupled to the top of a 30 m of DB-5 ms with a quartz capillary column connector. Peak width at half height (W(h)) was used to evaluate the band broadening of the coupled column system. The length of the short couple column and oven temperature program were discussed according to W(h). The precisions of the coupled column were analyzed with peak area and retention time. Good linear correlations were found for both rodenticides. Typical samples were discussed for each rodenticide and some poisoning cases were presented.
