Development of a novel solid-phase extraction, LC-MS/MS method for the analysis of ethyl carbamate in alcoholic beverages: Application to South African wine and spirits

Date
2011
Authors
Alberts P.
Stander M.A.
de Villiers A.
Journal Title
Journal ISSN
Volume Title
Publisher
Abstract
Ethyl carbamate (EC) is a known genotoxic carcinogen that is frequently present in alcoholic beverages and is therefore a public health concern. As a consequence, maximum concentration levels for EC in these commodities are legislated in several countries. Quantitative analytical methods are therefore essential to monitor EC levels in beverages. Most published analytical methods for the determination of EC in alcoholic beverages utilise elaborate sample pre-treatment procedures to obtain injectable samples, or yield low sensitivity, for example where direct injection is used. In addition, these procedures often require large volumes of toxic solvents and are not generally applicable to diverse alcoholic beverages. This paper describes a novel procedure for the determination of EC in wines, fortified wines and spirits. The procedure is based on reversed-phase solid-phase extraction (SPE) sample clean-up combined with normal-phase liquid chromatography-atmospheric pressure chemical ionisation tandem mass spectrometric (NP-LC-APCI-MS/MS) analysis. This method provides a rapid, robust and simple analytical procedure suitable for the analysis of a diverse range of alcoholic beverages. The accuracy of the method (expressed as average recovery from diverse matrices) is 94.5%, with limits of detection (LODs) ranging between 0.25 and 0.63 μg l-1 for different matrices. Benefits such as simplified sample preparation, low detection limits, low solvent consumption and good selectivity render the methodology ideally suited to study the occurrence of EC in diverse commodities. The method was applied to study the occurrence of EC in South African wines, fortified wines and spirits. South African wines, aged 1-9 years, contained 1.8-31 μg l-1 EC (RSD=69%, n=106), fortified wines aged 2-34 years contained 2.8-79 μg l-1 EC (RSD=89%, n=21), and brandies aged 3-20 years contained 4.4-95 μg l-1 EC (RSD=105%, n=26). Factors affecting the formation of EC in these commodities were investigated and storage temperature, alcohol content and pH were found to affect the rate of EC formation. Of these variables storage temperature has by far the greatest effect. © 2011 Taylor & Francis.
Description
Keywords
Beverages, Clean-up, Ethyl carbamate, Liquid chromatography/mass spectrometry, Survey, Wine, Alcohol contents, Alcoholic beverages, Analytical method, Analytical procedure, Average recovery, Clean-up, Concentration levels, Diverse matrices, Diverse range, Ethyl carbamate, Genotoxic, LC-MS/MS, Limits of detection, Liquid chromatography/mass spectrometry, Low detection limit, Low sensitivity, Public health, Reversed phase, Sample clean-up, Sample preparation, Sample pretreatment, Solid-phase extraction, Solvent consumption, Storage temperatures, Tandem mass spectrometric, Toxic solvents, Atmospheric pressure, Chemical analysis, Direct injection, Ionization of liquids, Liquid chromatography, Liquids, pH effects, Spectrometry, Wine, Extraction, alcohol, urethan, alcoholic beverage, article, chemical analysis, distilled spirit, fortified wine, limit of detection, liquid chromatography, mass spectrometry, pH, priority journal, red wine, solid phase extraction, South Africa, storage temperature, white wine, wine
Citation
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment
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