Alberts Philippus, Stander Maria A, De Villiers André
a Department of Chemistry and Polymer Science , University of Stellenbosch , Private Bag X1 , Matieland 7602 , South Africa.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2011;28(7):826-39. doi: 10.1080/19440049.2011.568010. Epub 2011 May 13.
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.
氨基甲酸乙酯（EC）是一种已知的遗传毒性致癌物，经常存在于酒精饮料中，因此受到公众健康关注。因此，多个国家都对这些商品中的EC最高浓度水平进行了立法。所以，定量分析方法对于监测饮料中的EC水平至关重要。大多数已发表的测定酒精饮料中EC的分析方法都采用复杂的样品预处理程序来获得可进样的样品，或者灵敏度较低，例如直接进样的情况。此外，这些程序通常需要大量有毒溶剂，并且一般不适用于多种酒精饮料。本文描述了一种测定葡萄酒、加烈葡萄酒和烈酒中EC的新方法。该方法基于反相固相萃取（SPE）样品净化，结合正相液相色谱-大气压化学电离串联质谱（NP-LC-APCI-MS/MS）分析。此方法提供了一种快速、稳健且简单的分析程序，适用于分析多种酒精饮料。该方法的准确度（以不同基质中的平均回收率表示）为94.5%，不同基质的检测限（LOD）在0.25至0.63μg l⁻¹之间。简化样品制备、低检测限、低溶剂消耗和良好的选择性等优点使该方法非常适合研究不同商品中EC的存在情况。该方法被应用于研究南非葡萄酒、加烈葡萄酒和烈酒中EC的存在情况。1至9年陈酿的南非葡萄酒中EC含量为1.8至31μg l⁻¹（相对标准偏差RSD = 69%，n = 106），2至34年陈酿的加烈葡萄酒中EC含量为2.8至79μg l⁻¹（RSD = 89%，n = 21），3至20年陈酿的白兰地中EC含量为4.4至95μg l⁻¹（RSD = 105%，n = 26）。研究了影响这些商品中EC形成的因素，发现储存温度、酒精含量和pH会影响EC的形成速率。在这些变量中，储存温度的影响最为显著。
