摘要
采用液液萃取及氘代同位素方法,优化了基于气相色谱-质谱(GC-MS)联用的葡萄酒中氨基甲酸乙酯的分析检测方法。结果表明,5 mL供试样品采用15 mL二氯甲烷并配合1.2 g NaCl操作时,可获得最佳的萃取效果,且溶剂量消耗较少。同时,试验所得检测方法在5~200μg·L^-1时具有良好的相关性(R^2>0.998 5),其回收率(82.38%~112.4%)、灵敏度(LOD 0.8μg·L^-1,LOQ 3μg·L^-1)、精密度(日内1.78%~3.78%和日间0.99%~2.70%)均满足测定分析需要。采用本方法对市售的80款河西走廊葡萄酒样品检测表明,有18个样品高于国际限量标准(>20μg·L^-1),但其储存时间多数已超过10 a,且这些葡萄酒的氨基甲酸乙酯含量与其贮存时间存在明显的正相关。
The liquid-liquid extraction and deuterated isotope methods were used to optimize the analytical detection of ethyl carbamate in wines based on gas chromatography-mass spectrometry.The results showed that 5 mL of the test sample was treated with 15 mL of dichloromethane and worked with 1.2 g of NaCl to obtain the best extraction effect,with less solvent consumption.At the same time,the test results obtained in the range of 5~200μg·L^-1 had a good correlation(R^2>0.998 5),and the recovery rate(82.38%~112.4%),sensitivity(LOD 0.8μg·L^-1,LOQ 3μg·L^-1)and precision(intra-day 1.78~3.78%,inter-day 0.99%~2.70%)could all meet the needs of measurement and analysis.Using this method,the test results of 80 samples of commercially available wine samples from the Hexi Corridor showed that 18 samples of them were above the international limit(>20μg·L^-1),but most of them had been stored for more than 10 years;indicating that there existed a significant positive correlation between ethyl carbamate content and its storage time.
作者
郝兰兰
张波
雷春妮
何佳
马腾臻
李宁宁
韩舜愈
HAO Lanlan;ZHANG Bo;LEI Chunni;HE Jia;MA Tengzhen;LI Ningning;HAN Shunyu(College of Food Science and Engineering,Gansu Agricultural University,Lanzhou 730070,China;Lanzhou Customs Integrated Technology Center,Lanzhou 730030,China)
出处
《河南农业大学学报》
CAS
CSCD
北大核心
2019年第3期406-414,共9页
Journal of Henan Agricultural University
基金
甘肃省葡萄酒产业发展项目([2017]466号-09)
关键词
气质联用法
葡萄酒
氨基甲酸乙酯
定量分析
gas chromatography-mass spectrometry(GC-MS)
wine
ethyl carbamate
quantitative analysis
