A simple and sensitive liquid chromatography-mass spectrometric technique coupled with solid-phase microextraction (SPE) method was describéd for the determination of fluoroacetamide in a poison case. The experimental conditions of SPE and the probe of SPE were discussed, recovery rate and precision were investigated. The results showed that the detection limit of fluoroacetamide is 0. 1mg/L, the average recovery is 99.2%.
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