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
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10 μg/mL的EC-d5溶液100 μL和硫酸钠3 g, 震荡溶解, 注射针快速打入700 μL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, 0.25 μm)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, r2 = 0.9988, 检出限为0.73 μg/L, 定量限为2.18 μg/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6.82~15.3 μg/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 100 μL of EC-d5 (10 μg/mL) and 3 g of Na2SO4, 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 (51500 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 6.8215.3 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.
标题：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
英文标题：Determination of ethyl carbamate in wine by salt-assisted dispersive liquid-liquid microextraction-gas chromatography-tandem mass spectrometry
作者：
王雅楠 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
郭欣然 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
王宗义 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
魏朝俊 北京农学院,生物与资源环境学院
李瑞英 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
中文关键词: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,
英文关键词:salt-assisted dispersion liquid-liquid microextraction,wine,ethyl carbamate,gas chromatography-tandem mass spectrometry,stable isotope dilution,
发表日期：2019-12-12
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