毛细管色谱／质谱选择离子监测法测定酒精饮料中氨基甲酸乙酯  

Determination of Ethyl Carbamate in Alcoholic Beverages by Selected Ion Monitoring in Capillary Gas Chromatography/Mass Spectrometry

作　　者：周英田[1] 孙咏梅[1] 邓峰[1] 

机构地区：[1]军事医学科学院卫生学环境医学研究所

出　　处：《色谱》1996年第3期190-192,共3页Chinese Journal of Chromatography

摘　　要：氨基甲酸乙酯是一种致癌物质，已在多种葡萄酒中被检测到。测定时，一般取样４０ｍＬ，用二氯甲烷萃取，然后蒸发至近干。残留物用乙酸乙酯溶解，定容至５．０ｍＬ。取１μＬ进气相色谱－质谱仪（ＧＣ－ＭＳ）分析，用选择离子监测ｍ／ｚ６２定量。ＣＶ为４．１％，其平均回收率高于８０％。对８种样品的分析结果表明，氨基甲酸乙酯含量为１．０１～１．７８μｍｍｏｌ／Ｌ，与有关文献报道相近。he present paper describes a sensitive method suitable for the determination of ethyl carbamate,known as a carcinogen in various wines. A representative sample(40mL of wine) was added to a 250mL centrifuge tube contained 30g sodium chloride. Total volumes were then made up to 50mL with saturated sodium chloride and extracted with methylene chloride. Extracts were evaporated to incipient dryness. The residue was dissolved in ethyl acetate and the final volume was adjusted to 5. 0mL. Take 1μL for gas chromatography/mass spectrometry analysis. Chromatographic conditions were column, 25cm×0. 22mm i. d., 25QC2/BP20,0.25 (SGE. Serial No: 82308)coupled directly to MSD; injector, 180℃; transfer line, 200℃;detector, 168℃; column oven, initial 55℃ , hold 2min, programmed at 30℃ min-1 to 120℃, hold 0. 5min, and then 3℃min-1 to 130℃ and then 10℃min-1 to 250℃, hold 0min; helium carrier gas flow rate 0.6mL/min.The selected ion of the m/z 62 was used for quantitation. The method is proved to be suitable for the determination of trace levels of ethyl carbamate in various alcoholic beverages. The CV value was 4.1 %. The average recoveries were better than 80% for the 8 fortified samples. The results of the 8 kinds of wines showed that ethyl carbamate contents were between 1. 01-1.78μmol/L which ware similar to related reports.

关 键 词：色谱 质谱 氨基甲酸乙酯 酒 

分 类 号：TS262[轻工技术与工程—发酵工程] O657.7[轻工技术与工程—食品科学与工程]