Guangzhou Quality Supervision and Testing Institute, Guangzhou 511447, China; Research Center of Risk Dynamic Detection and Early Warning for Food Safety of Guangzhou City, Guangzhou 511447, China; Key Laboratory of Detection Technology for Food Safety of Guangzhou City, Guangzhou 511447, China.
College of Light Industry and Food Sciences, Zhongkai University of Agriculture and Engineering, Guangzhou 510225, China.
Food Chem. 2019 Dec 1;300:125200. doi: 10.1016/j.foodchem.2019.125200. Epub 2019 Jul 17.
Ethyl carbamate (EC) and N-nitrosoamines (NAs) are toxic contaminants which can be typically formed in fermented alcoholic beverages. In the present work, a novel approach for simultaneous analysis of EC and NAs in beer and yellow rice wine based on ice-bath assisted sodiumhydroxide purification and GC-MS/MS was firstly established. Samples were extracted with acetonitrile-ethyl acetate after addition of internal standards. The extraction solution system was purified by sodiumhydroxide solid under ice-bath. After concentration, target analytes were separated on a HP-INNOWAX quartz capillary column and determined under dynamic multiple reactions monitoring mode of MS/MS. The limits of detection and quantification (LOD and LOQ), matrix effect, recovery and precision of the method were evaluated. Results were linear in the concentration range 2-200 μg/L for all analytes of interest, with regression coefficients higher than 0.999. LODs and LOQs were in the ranges of 0.1-0.5 μg/kg and 0.5-1.5 μg/kg, respectively. The mean recoveries at three spiked levels were between 81.5% and 121.0%. The intra- and inter-day precisions were in the ranges of 2.2-9.4% and 1.6-7.9%, respectively. The validated method was successfully applied to determine thirteen targets in commercial beer and yellow rice wine. EC was detected in all beers and yellow rice wines with the concentrations ranging from 1.18 to 22.90 μg/L. Results indicated wide EC contamination and confirmed its urgency for monitoring EC in fermented alcoholic beverages.
氨基甲酸乙酯（EC）和亚硝胺（NAs）是有毒污染物，通常在发酵酒精饮料中形成。本工作首次建立了基于冰浴辅助氢氧化钠净化和 GC-MS/MS 用于同时分析啤酒和黄酒中 EC 和 NAs 的新方法。样品用乙腈-乙酸乙酯提取，加入内标。在冰浴下用氢氧化钠固体净化提取溶液体系。浓缩后，目标分析物在 HP-INNOWAX 石英毛细管柱上分离，并在 MS/MS 的动态多反应监测模式下测定。评价了方法的检出限和定量限（LOD 和 LOQ）、基质效应、回收率和精密度。所有感兴趣的分析物在 2-200μg/L 浓度范围内均呈线性，相关系数均高于 0.999。LOD 和 LOQ 分别为 0.1-0.5μg/kg 和 0.5-1.5μg/kg。三个加标水平的平均回收率在 81.5%-121.0%之间。日内和日间精密度分别在 2.2%-9.4%和 1.6%-7.9%范围内。验证后的方法成功应用于测定商业啤酒和黄酒中的 13 种目标物。所有啤酒和黄酒中均检出 EC，浓度范围为 1.18-22.90μg/L。结果表明 EC 污染广泛，证实了监测发酵酒精饮料中 EC 的紧迫性。
