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

卷:177

Nobrega, Ian C. C. ; Pereira, Giuliano E. ; Silva, Marileide ; Pereira, Elainy V. S. ; Medeiros, Marcelo M. ; Telles, Danuza L. ; Albuquerque, Eden C., Jr. ; Oliveira, Juliane B. ; Lachenmeier, Dirk W.

关键词: Ethyl carbamate;    Wine;    Automated parallel evaporation;    Diethyl ether extraction;    Validation;    GC-MS-SIM;   

DOI  :  10.1016/j.foodchem.2014.12.031

学科分类：食品科学和技术

【 摘 要 】

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-d(5) 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% (3.4 mu g L-1) and 1.7% (88.5 mu g L-1), regression coefficient was 0.999 in the linear working range of 3-89 mu g L-1, and limits of detection and quantification were 0.4 and 1.2 mu g L-1. Applicability was demonstrated by analysis (in triplicate) of 5 wine samples. EC concentration ranged from 5.2 +/- 0.2 to 29.4 +/- 1.5 mu g L-1. The analytical method is selective, accurate, repeatable, linear, and has similar method performance as the reference method along with the several mentioned advantages. (C) 2015 Elsevier Ltd. All rights reserved.