液相色谱串联质谱法测定白酒中氨基甲酸乙酯的方法探讨

Determination of Ethyl Carbamate in White Spirit by Liquid Chromatography-tandem Mass Spectrometry

建立了直接测定白酒中氨基甲酸乙酯的液相色谱-串联质谱（LC-MS-MS）分析方法,采用Poroshell120EC-C18色谱柱,以0.1%乙酸水溶液和乙腈为流动相（体积比9∶1）进行洗脱,流速为0.2m L/min;在电喷雾电离（ESI）正离子模式下,采用多重反应监测模式进行检测,线性范围为5~500μg/L;检出限为1μg/L,定量限为5μg/L;加标回收率为89%~106%,相对标准偏差均不大于3.9%。该法快捷、准确、重现性好。

A method for the direct determination of ethyl carbarnate in White spirit was established by liquid chromatography with tandem mass spectrometry （LC-MS-MS）.The LC separation was performed on a Poroshell 120 EC-C18 column （50mm × 3.0mm,2.7 ~ re）by using 0.1%（v/v） acetic acid aqueous solution and acetonitrile as mobile phases （v/v 9 ： 1） at a flow rate of 0.2mL/min. The analytes were detected by tandem mass spectro-metry under the positive ion mode with the electrospray ionization （ESI） source and in the multiple reaction monitoring （MRM）mode. Under the optimized conditions ,the calibration curve was linear in the ranges of 5 ~ 500 μ g/L for the ethyl carbamate with the detection limits of 1μ g/L and the limit of quantification of 5 μg/L. The recoveries of the ethyl carbamate was in the range of 89% and 106% with the relative standard deviations not more than3.9%. The developed method is simple ,rapid and accurate, and suitable for the quality control of ethyl carbamate in White spirit.