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Multiple headspace solid-phase microextraction (MHS-SPME) combined with gas chromatography-nitrogen phosphorus detector is proposed to determine the toxic contaminant ethyl carbamate (EC) in various alcoholic beverages after matrix modification.A novel polyethylene glycol/hydroxy-terminated silicone oil fiber was used instead of commercial ones because of its high extraction ability.Anhydrous sodium sulphate was added to modify the matrix and the extraction efficiency of EC was greatly improved.The optimum conditions for MHS-SPME were as follows: extraction time, 10 min; extraction temperature, 35 ℃; Na2SO4 addition, 4.0 mg/μL of sample; volume of sample, 20 μL.