盐辅助分散液液微萃取-气相色谱-串联质谱法检测葡萄酒中的氨基甲酸乙酯  

Determination of ethyl carbamate in wine by salt-assisted dispersive liquid-liquid microextraction-gas chromatography-tandem mass spectrometry

作　　者：王雅楠 郭欣然 王宗义[1] 魏朝俊[2] 李瑞英 WANG Ya-Nan;GUO Xin-Ran;WANG Zong-Yi;WEI Chao-Jun;LI Rui-Ying(Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Detection and Control of Spoilage Microorganisms and Pesticide Residues in Agricultural Products,Beijing University of Agriculture,Beijing 102206,China;College of Bioscience and Resources Environment,Beijing University of Agriculture,Beijing 101500,China)

机构地区：[1]北京农学院,食品科学与工程学院,食品质量安全北京实验室,农产品有害微生物及农残安全检测与控制北京市重点实验室,北京102206 [2]北京农学院,生物与资源环境学院,北京101500

出　　处：《食品安全质量检测学报》2020年第5期1364-1368,共5页Journal of Food Safety and Quality

基　　金：北京农学院“内涵发展定额--大学生科研训练”项目、第11届北京市大学生化学实验竞赛(2019)项目。

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。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 100μL of EC-d5(10 ug/mL)and 3 g of Na2 SO4,the sample tube was shaken untill the salt was dissolved,and then 700μL 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,0.25μm)chromatographic column and detection with the multiple response monitoring mode.Results This method had good linearity(r^2=0.9988)in the investigated concentration range(5-1500 ng/mL),the limit of detection and limit of quantification were 0.73μg/L and 2.18μg/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 6.82-15.3μg/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.

关 键 词：盐辅助分散液液微萃取 葡萄酒 氨基甲酸乙酯 气相色谱-串联质谱法 稳定同位素稀释 

分 类 号：O657.63[理学—分析化学] TS262.6[理学—化学]