Abstract:A rapid and accurate method was established for determining the content of ethyl carbamate in a large number of Baijiu samples based on liquid chromatography-tandem mass spectrometry. An Accucore aQ chromatographic column （150 mm×2.1 mm， 2.6 μm） was used for gradient elution， which was carried out with methanol and 0.1% （volume ratio） formic acid aqueous solution as mobile phases at the flow rate of 0.3 mL/min.In the positive ion mode of electrospray ionization （ESI）， selected reaction monitoring （SRM） was used for detection. The results showed that the content of ethyl carbamate determined by the established method presented a linear relationship （R2=0.999 6）， and the limits of detection and quantitation were 0.114 μg/L and 0.380 μg/L，respectively. The recovery range was 103.06%-106.34%， and the relative standard deviation （RSD） was 1.19%-2.05%. The RSD （n=6） of ethyl carbamate determined by the established method for 5 brands of Baijiu purchased from the market was 1.84%-3.49%.