A new urea adducts method for PUFA concentration using green food grade solvents and avoiding ethyl carbamate formation.

This study aimed to selectively enrich stearidonic acid (SDA) together with γ-linolenic acid (GLA) in Echium plantagineum oil by urea complexation. The complexation process at room temperature was carried out replacing common organic solvents, such as hexane and ethanol, by alternative compounds, included in Green Solvent and Food Grade categories, adapting this process towards the principles of Green Chemistry. This substitution was also intended to avoid the generation of the toxic compound ethyl carbamate. Among all the solvents studied, the mixture propionic acid and α-pinene provided the best results, leading to a final product comprised of ∼99% of PUFA, with ∼45% SDA (∼14% in the original oil), and without apparition of ethyl carbamate. The procedure was tested on other raw materials (salmon and microalgae oils). The solvent was efficiently recuperated from the liquid phase (∼87% recovery) and reutilized once with almost identical results.

Changes of ethyl carbamate and its precursors in maesil (Prunus mume) extract during one-year fermentation.

The contents of ethyl carbamate (EC), cyanide, and ethanol were determined in maesil extracts that are liquids generated from fermentation of maesil fruit and brown sugar at 25°C or 15°C for one year. EC was detected from day 150 with a maximum value of 9.7µg/kg. The cyanide levels increased with prolonged soaking time of maesil and decreased at day 150 where EC was firstly detected, indicating that cyanide is a precursor of EC. Ethanol slowly increased at 25°C, while it fluctuated at 15°C. The contents of EC, cyanide, and ethanol were higher in the extracts fermented at 25°C compared with those at 15°C. EC contents had a higher positive correlation with cyanide contents (R=0.658) than ethanol contents (R=0.351). These results indicate that fermenting temperature gave a rise of EC precursors and consequently led to the increase of EC in the maesil extract.

Ethyl carbamate in fermented foods and beverages: dietary exposure of the Hong Kong population in 2007-2008.

To evaluate the potential public health risk of ethyl carbamate (EC), EC exposure from fermented foods and beverages for Hong Kong population was estimated. In 276 samples analysed, EC was detected (limit of detection (LOD) at 0.4 µg kg(-1)) in 202 samples (73%), with higher levels in fermented red bean curd (150-650 µg kg(-1)) and yellow wine (140-390 µg kg(-1)), while low or non-detected (ND) in preserved vegetables (ND-10 µg kg(-1)) and fermented tea (ND-15 µg kg(-1)). The estimated dietary exposure from all fermented foods and beverages was 8.27 ng kg(-1) bw day(-1), while exposure excluding alcoholic beverages was 5.42 ng kg(-1) bw day(-1), with calculated margins of exposure (MOEs) at 3.6 × 10(4) and 5.5 × 10(4) respectively. The risk of adverse health effects was low for the average population but higher (MOE of 10(3)) for high consumers of alcoholic beverages especially habitual drinkers of alcoholic types with high EC contents.

Original normal-phase high-performance liquid chromatographic separation of monoacylglycerol classes from extra virgin olive oil triacylglycerols for their stereospecific analysis.

An innovative procedure to separate the 3 isomeric sn-monoacylglycerols (MAG) classes (sn-1-, sn-2-, sn-3-MAG) is described. MAGs, obtained by chemical deacylation of triacylglycerols (TAGs), have been derivatized with (S)-(+)-1-(1-naphtyl)ethyl-isocyanate, and the resulting urethane derivatives have been separated by normal-phase high-performance liquid chromatography. This procedure allows resolution as diasteroisomers of the 2 enantiomeric classes (sn-1-MAG and sn-3-MAG), without the need of a chiral column, and to separate also the isomeric sn-2-MAG class; moreover, by introducing a chromophoric moiety, this reagent makes possible the ultraviolet detection of the analyte molecules. This procedure has been used to obtain the stereospecific analysis of the TAG fraction of extra virgin olive oil samples. The use of a nondestructive detector permitted the collection of the individual urethane classes; the fatty acid composition of each was determined by high-resolution gas chromatography, obtaining directly from the data the fatty acid distribution within each sn- position of TAGs. To validate this new method, the results have been compared with those obtained by 2 other procedures for TAG stereospecific analysis, and the obtained results were satisfactory since the proposed method gave data very similar to the other procedures.

Formación e identificación de carbamato de etilo en bebidas alcohólicas y alimentos fermentados / Ethyl carbamate formation and identification in alcoholic beverages and fermented food

La formación e identificación del carbamato de etilo ha conducido a numerosos estudios para entender mejor su formación y su posterior identificación y cuantificación. En esta revisión sintetizamos lo que ha sido aportado en la literatura que se ha publicado en este tema en las últimas décadas. Se realiza un especial interés en la formación, los precursores y los métodos analíticos de identificación y cuantificación del carbamato de etilo (AU)

Determination of ethyl carbamate in alcoholic beverages and soy sauce by gas chromatography with mass selective detection: collaborative study.

A method using gas chromatography with mass selective detection for the determination of ethyl carbamate (EC; also known as urethane) in alcoholic beverages and soy sauce was collaboratively studied by 17 laboratories including authors' laboratories. The method uses prepacked columns for extraction of liquids with methylene chloride, and n-propyl carbamate as the internal standard. A practice sample and 6 samples of distilled spirits, fortified wines, table wines, and soy sauces were analyzed by each collaborator. Each matrix included blind duplicates of incurred and fortified EC at 3 levels. Distilled spirits contained 50-330 ng EC/g (ppb), fortified wine 40-160 ppb, table wine 10-50 ppb, and soy sauce 15-70 ppb. The ranges of the repeatability relative standard deviations, excluding outliers, were 4.03-6.63% for distilled spirits, 4.01-5.05% for fortified wine, 3.94-6.73% for table wine, and 4.70-8.49% for soy sauce. The ranges of the reproducibility relative standard deviations, excluding outliers, were 8.53-9.49% for distilled spirits, 6.84-12.02% for fortified wine, 8.86-18.47% for table wine, and 13.87-27.37% for soy sauce. Recoveries of added EC ranged from 87 to 93%. Recoveries relative to reference values, labeled as the internal standard, obtained by using gas chromatography/tandem mass spectrometry with a triple quadrupole mass spectrometer ranged from 89 to 100%.