【摘要】 目的建立了盐辅助分散液液微萃取(salt-assisted dispersive liquid-liquid microextraction,SADLLME),稳定同位素稀释,气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测葡萄酒中氨基甲酸乙酯(ethyl carbamate,EC)的方法。方法取30 mL葡萄酒于50 mL离心管中,加入浓度为10μg/mL的EC-d5溶液100μL和硫酸钠3 g,震荡溶解,注射针快速打入700μL二氯甲烷,震荡1 min,离心,取下层有机相,经DB-INNWAX UI色谱柱(30 m×0.25 mm,0.25μm)分离,多重反应监测方式进行质谱检测。结果方法在验证浓度范围内(5～1500 ng/mL),线性良好,r~2=0.9988,检出限为0.73μg/L,定量限为2.18μg/L,回收率为91.5%～97.8%,相对标准偏差为2.55%～5.26%。对市场上3个品牌红葡萄酒进行检测,EC含量为6.82～15.3μg/L。结论该方法样品处理简便、快速,相对绿色,定性、定量可靠,能够满足葡萄酒中EC风险监测的需要。更多还原

【Abstract】 Objective To establish a new method for determination of ethyl carbamate（EC） in wine by salt-assisted dispersion liquid-liquid microextraction（SADLLME） coupled with stable isotope dilution technique and gas chromatography-tandem mass spectrometry（GC-MS/MS）.Methods Adding 30 mL wine into a 50 mL centrifuge tube,followed by adding 100 μL of EC-d5（10 ug/mL） and 3 g of Na₂ SO₄,the sample tube was shaken untill the salt was dissolved,and then 700 μL dichloromethane was quickly injected into the sample solution.After shaking 1 min and centrifugation,the bottom organic phase of sample solution was analyzed by GC-MS/MS through separation with DB-INN WAX UI（30 m×0.25 mm,0.25 μm）chromatographic column and detection with the multiple response monitoring mode.Results This method had good linearity（r²=0.9988） in the investigated concentration range（5-1500 ng/mL）,the limit of detection and limit of quantification were 0.73 μg/L and 2.18 μg/L,respectively.The recoveries were 91.5%-97.8%with relative standard deviation ranged from 2.55%-5.26%.Totally 3 brands of red wines on the market were investigated by this method,and the content of EC was 6.82-15.3 μg/L.Conclusion This method is simple and fast,relatively green,qualitative and quantitative reliable,which can meet the needs of EC risk monitoring in wine.更多还原