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% (3.4 μg L(-)(1)) and 1.7% (88.5 μg L(-)(1)), regression coefficient was 0.999 in the linear working range of 3-89 μg L(-)(1), and limits of detection and quantification were 0.4 and 1.2 μg 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 μg 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.

A facile synthesis of molecularly imprinted polymers and their properties as electrochemical sensors for ethyl carbamate analysis

“…The procedure and the analytical instrument condition were as reported in the literature. [35][36][37] A standard curve was prepared.…”

SERS-active Ag Nanostars Substrates for Sensitive Detection of Ethyl Carbamate in Wine

“…The development of a simple, fast and sensitive analytical method for EC quantification is thus urgently needed. Currently, a number of instrumental approaches are available for the detection of EC, including gas chromatography (GC)/mass spectrometry (MS), [3][4][5][6] high-performance liquid chromatography (HPLC) tandem MS, 7 HPLC with fluorescence detection (FLD), [8][9][10][11][12] and solid phase microextraction tandem GC-MS. 13 Although these methods can accurately and sensitively detect EC at low concentrations, the requirement of a complex instrument and prolonged sample pretreatments have often limited their wide applications. Hence, the development of new approaches for fast and accurately determinations of EC are of great importance.…”

Determination of Ethyl Carbamate in Alcoholic Beverages and Fermented Foods Sold in Korea

“…It could lead to the difference in the recoveries between EC and internal standard. Therefore, the deuterated EC (d 5 -EC) is recently used to provide more precise recovery correction (12 , 22 - 24) . The most traditional extraction method is a liquid-liquid extraction.…”

“…The MS is the most useful and authoritative method for the quantification of EC. Recently, GC-MS-MS has been adopted to improve selectivity, sensitivity, and repeatability for EC determination (10 , 24 , 32) . High performance liquid chromatography (HPLC) coupled with a fluorescence detector was employed after the derivatization with 9-xanthydrol (33) .…”