Improved sample preparation for GC–MS–SIM analysis of ethyl carbamate in wine

Abstract

An improved sample preparation procedure for analysis of carcinogenic ethyl carbamate (EC) in wine by GC–MS–SIM is proposed. Differences over AOAC reference procedure were: (1) use of EC-d5 as internal standard instead of less similar propyl carbamate; (2) extraction by diethyl ether instead of more toxic dichloromethane, and (3) concentration by vacuum automated parallel evaporation instead of more time and work consuming rotary evaporation. Mean recovery was 104.4%, intraday precision was 6.7% (3.4μgL−1) and 1.7% (88.5μgL−1), regression coefficient was 0.999 in the linear working range of 3–89μgL−1, and limits of detection and quantification were 0.4 and 1.2μgL−1. Applicability was demonstrated by analysis (in triplicate) of 5 wine samples. EC concentration ranged from 5.2±0.2 to 29.4±1.5μgL−1. The analytical method is selective, accurate, repeatable, linear, and has similar method performance as the reference method along with the several mentioned advantages.