GC-MS/MS法分析常用食品和卷烟烟气中的氨基甲酸乙酯  

Determination of ethyl carbamate in daily foods and cigarette smoke by gas chromatography coupled tandem mass spectrometry

作　　者：廖惠云[1] 张华[1] 秦艳华[1] 庄亚东[1] 熊晓敏[1] 尤晓娟[1] 朱莹[1] 张媛[1] 王晨辉[1] LIAO Huiyun;ZHANG Hua;QIN Yanhua;ZHUANG Yadong＊;XIONG Xiaomin;YOU Xiaojuan;ZHU Ying;ZHANG Yuan;WANG Chenhui(Technology Center, China Tobacco Jiangsu Industrial Co., Ltd., Nanjing 210019, China)

机构地区：[1]江苏中烟工业有限责任公司技术中心,南京市梦都路28号210019

出　　处：《烟草科技》2018年第4期53-59,80,共8页Tobacco Science & Technology

基　　金：国家烟草专卖局资助项目"卷烟主流烟气中氨基甲酸乙酯的测定"(2013QB001)

摘　　要：为分析常用食品和卷烟烟气中的痕量氨基甲酸乙酯(EC),使用脉冲不分流进样方式,建立了反相固相萃取净化-固相反萃取-气相色谱/串联质谱分析方法。采用水为溶剂振荡萃取样品中的目标物,使用C_(18)反相固相萃取柱净化萃取液,再用二氯甲烷通过硅藻土固相萃取柱对净化液进行反萃取,得到的洗脱溶液经浓缩后进行GC-MS/MS分析,以氘代氨基甲酸乙酯为内标进行定量。结果表明:(1)在优化条件下,目标物在0.75~48.00μg/L浓度范围内线性良好(R^2为0.999 9),检出限和定量限分别为0.025 9和0.086 3μg/kg,不同水平下的加标回收率为91.56%~112.22%,RSD为4.24%~7.97%。(2)样品普查显示,酒精类饮料(黄酒、白酒、啤酒和红酒)、料酒、酱油、酸奶和腐乳等日常食品中EC的质量分数为5.17~523.66μg/kg,EC在卷烟烟气中的释放量为0.33~1.20 ng/支。该方法灵敏度高、适用性强,可用于日常食品和卷烟烟气中痕量EC的定量分析。For quantifying trace levels of ethyl carbamate （EC） in daily foods and cigarette smoke, a reverse-phase solid phase extraction cleanup method coupled with solid phase reverse extraction and gas chromatography/tandem mass spectrometry was developed by adopting pulse splitless injection mode. After extracting EC from samples by using water as a solvent, the extract was cleaned up by C18 reverse-phase solid phase extraction column, then was reversely extracted by diatomite solid phase extraction column with dichloromethane. The eluent was detected with gas chromatography-tandem mass spectrometry after concentration with deuterium-labeled EC as internal standard for quantitation. The results showed that：1） Under optimal condition, the calibration curve was linear （R2=0.999 9） when the concentration of EC was in the range of 0.75-48.00 μg/L, the limits of detection and quantitation were 0.025 9 and 0.086 3 μg/kg, respectively. The recoveries of different sample matrix ranged from 91.56% to 112.22% with relative standard deviations of 4.24%-7.97%. 2） The results from surveyed samples indicated that the contents of EC in several daily foods, including alcoholic beverage （yellow rice wine, white spirit, beer and red wine）, cooking wine, soy sauce, yoghourt and fermented bean curd ranged from 5.17-523.66 μg/kg, and the release of EC in cigarette smoke ranged from 0.33 to 1.20 ng/cig. With higher sensitivity and better applicability, this method could be used to detect trace EC in other daily foods and cigarette smoke.

关 键 词：反相固相萃取净化 固相反萃取 气相色谱/串联质谱(GC-MS/MS) 日常食品 卷烟 烟气 氨基甲酸乙酯 

分 类 号：TS411.2[农业科学—烟草工业]