Brazilian vodkas have undetectable levels of ethyl carbamate

While in Europe vodka is mainly derived from potatoes or cereals, a large proportion of Brazilian vodka is likely obtained from sugarcane, which contains ethyl carbamate (EC) precursors. EC, in addition to several other contaminants and congeners, were investigated in 32 samples of Brazilian vodka. All samples complied with the Brazilian regulations for congeners and contaminants, having EC content below 0.01 mg/L (detection limit). These results are probably related to the processing of vodka, in particular the use of extractive and rectifying stainless steel distillation columns, which allow the production of high strength spirits with low levels of congeners and contaminants.

Carbamato de etila em bebidas alcoólicas (cachaça, tiquira, uísque e grapa)

The presence of ethyl carbamate in cachaças, tiquiras, whiskies and grapes was investigated by GC-MS, monitoring the m/z 62 ion. The external standard method was used for quantitation in 188 samples (126 cachaças, 37 tiquiras, 6 grappas and 19 whiskies). The results of the study for cachaça were analysed considering the geographic origin, distillation type (still or column), bottle coloration (amber or transparent) and ageing. The average contents of ethyl carbamate in cachaças and tiquiras were 0.77 and 2.4 mg L-1, respectively. These values were higher than the mean concentration found in grapes (0.045 mg L-1) and whiskies (0.14 mg L-1). On average the cachaças distilled in column tend to present higher values of ethyl carbamate than those from still. In the sampling studied it was not possible to define a correlation between content of ethyl carbamate, bottle coloration and ageing time.

Teores de carbamato de etila e outros componentes secundários em diferentes cachaças produzidas em três regiões do estado de Minas Gerais: Zona da mata, sul de minas e vale do jequitinhonha

Minas Gerais is the highest producer of handmade spirits. Research has been carried out aiming to contribute to progress. Thus, the goal of this work is to evaluate the quality of spirits in three different regions of Minas Gerais state. We analyzed ethyl carbamate, alcoholic grade, volatile acidity, higher alcohols, aldehyde, esters, methanol, furfural and copper. The values obtained for ethyl carbamate varied from undetectable to 643.5 µg L-1, with only one region not following the legislation (150 µg L-1). Most of the compounds in the spirits were present within the limits estabilished by the legislation.

Determinação de carbamato de etila em aguardentes de cana por CG-EM

A simple, specific and sensitive GC-MS procedure with ion m/z 62 was validated for the determination of ethyl carbamate (EC) in spirits. It exhibited linearity over the concentration of 30 to 600 μg/L with 30 μg/L limit of quantification. EC was detected in 70 of the 71 samples analyzed with levels from 33 to 2609 μg/L (mean level = 893 μg/L). 35% of the samples contained 500 to 1000 μg/L and 23% contained 150 to 500 and 1000 to 1500 μg/L. No significant correlation was found between EC and the levels of copper, pH and alcohol content of the samples.

Teores de carbamato de etila em aguardentes de cana e mandioca: parte II

Herein, we report the concentration of ethyl carbamate (EC) and copper in 380 samples of sugar-cane spirit and 45 samples of manioc spirit as determined by GC-MS and FAAS respectively. The cyanide content determined spectrophotometrically is reported for the manioc spirit. Sugar cane spirit produced by alembic distillation (70,0 µg L-1) shown a lower content of EC than samples produced by column distillation (270 µg L-1). No simple correlation between the content of EC and copper for sugar cane spirit as well among the concentration of EC, copper, and cyanide for manioc spirit could be observed.

Distinção entre cachaças destiladas em alambiques e em colunas usando quimiometria

One hundred fifteen cachaça samples derived from distillation in copper stills (73) or in stainless steels (42) were analyzed for thirty five itens by chromatography and inductively coupled plasma optical emission spectrometry. The analytical data were treated through Factor Analysis (FA), Partial Least Square Discriminant Analysis (PLS-DA) and Quadratic Discriminant Analysis (QDA). The FA explained 66.0% of the database variance. PLS-DA showed that it is possible to distinguish between the two groups of cachaças with 52.8% of the database variance. QDA was used to build up a classification model using acetaldehyde, ethyl carbamate, isobutyl alcohol, benzaldehyde, acetic acid and formaldehyde as chemical descriptors. The model presented 91.7% of accuracy on predicting the apparatus in which unknown samples were distilled.

Estimativa da incerteza de medição em análise cromatográfica: abordagem sobre a quantificação de carbamato de etila em cachaça

The measurement uncertainty is useful to estimate the confidence of analytical results. Nowadays, a result without the uncertainty statement cannot be considered reliable, but the scientific literature still lacks examples of the estimate of the measurement uncertainty. This paper presents a practical and reliable description of the measurement uncertainty estimation of the analytical determination of ethyl carbamate in cachaça by GC-IDMS. The isotope dilution technique (ID) associated with GC-MS was used to improve the accuracy. The uncertainty estimated corresponds to 10% of the mass fraction of ethyl carbamate (115 ± 11) ng/g, which is in agreement with ppb level.

Benzo(a)pireno, carbamato de etila e metanol em cachaças

The objective of this work was to evaluate the presence of benzo(a)pyrene (BaP), ethyl carbamate (EC) and methanol in 61 samples of cachaça. The quantification of BaP was carried out using HPLC with fluorescence detection, EC concentrations was determined by GC/MS and that of methanol, by GC/FID. In all samples, the concentration of methanol remained below 5 mg 100 mL-1 absolute alcohol. The results of BaP varied from <0.03 to 0.86 μg L-1; the values of EC exceeded the limit established by Brazilian legislation (150 μg L-1) in 53% of the samples.

Caracterização e quantificação de contaminantes em aguardentes de cana

The objective of the present study was the evaluation of the presence of organic and inorganic contaminants in samples of aged cachaça from the South of the state of Minas Gerais. Furfural, methanol and copper were determined by colorimetric reactions, while the analyses of ethyl carbamate and acrolein were performed by GC/MS and HPLC, respectively. High levels of furfural and copper were obtained. All samples showed concentrations below the established by legislation for the ethyl carbamate, and for acrolein, only one sample showed higher levels. Methanol was not detected in the samples.

Identificação do carbamato de etila durante o armazenamento da cachaça em tonel de carvalho (quercus sp) e recipiente de vidro

The objective of the present study was the identification and quantification of ethyl carbamate (EC), by HPLC-FLD, after different periods of storage in an oak (Quercus sp) barrel and a glass vessel. The concentration of EC in the cachaça samples varied from

Formação de carbamato de etila em aguardentes recém-destiladas: proposta para seu controle

The commercial sugar cane spits redistillation decreased up to 92,5% their ethyl carbamate (EC) original content. Quantitative analysis of EC in 15 samples of sugar cane spirit (alembic and column), fresh distilled and collected in situ demonstrated that the urethane is formed mostly after distillation. The average time to achieve the complete EC formation is independent of the diffuse light presence and of the distillation apparatus used. The k obs for urethane formation at 25 ºC was calculate as (3,3 ± 0,5) x 10-5/s and the activation parameters are: ΔH‡ 34 kcal/mol; ΔS‡ - 69 cal/mol K; and ΔG‡ 54 kcal/mol.

Decaimento de íons cianato e a formação de carbamato de etila

Cyanate ion stability was studied in aqueous/ethanolic solutions, pH = 4.5 (CH3COOH/NaCH3COO), at different temperatures. Following the decay [(OCN)-] versus time, in the presence of excess C2H5OH, the rate constant for this reaction (k1) was calculated as (2.5 ± 0.3) x 10-4 s-1 at 25 ºC, for 0 < [C2H5OH] < 13.7 x 10-1 mol L-1. For [C2H5OH] > 2.0 mol L-1 a decrease in the numerical value of k1 was observed, reaching 5.2 x 10-5 s-1 when [CH3CH2OH] = 13.7 mol L-1. Variations in the kinetic parameter values ΔH1‡, ΔS1‡ and ΔG1‡ for the cyanate ion decay reaction were observed for solutions at different ethanol concentrations.

Biomorphological Alterations Induced by an Anti-juvenile Hormonal Compound, 2-(2-EthoxyEthoxy)Ethyl Furfuryl Ether, on Three Species of Triatominae Larvae (Hemiptera, Reduviidae)

Applied topically to larvae of Rhodnius prolixus Stal, Triatoma infestans (Klug) and Panstrongylus herreri Wygodzinsky, vectors of Trypanosoma cruzi, the causative agent of Chagas'disease, a synthetic, furan-containing anti-juvenile hormonal compound, 2-(2-ethoxyethoxy)ethyl furfuryl ether induced a variety of biomorphological alterations, including precocious metamorphosis into small adultoids with adult abdominal cuticle, ocelli, as well as rudimentary adultoid wings. Some adultoids died during ecdysis and were confined within the old cuticle. The extension of these biomorphological responses is discussed in terms of the complexity of the action of anti-juvenile hormonal compounds during the development of triatomines

Optimization of chromatographic conditions and comparison of extraction efficiencies of four different methods for determination and quantification of pesticide content in bovine milk by UFLC-MS/MS

This paper describes the optimization of a multiresidue chromatographic analysis for the identification and quantification of 20 pesticides in bovine milk, including three carbamates, a carbamate oxime, six organophosphates, two strobilurins, a pyrethroid, an oxazolidinedione, an aryloxyphenoxypropionate acid/ester, a neonicotinoid, a dicarboximide, and three triazoles. The influences of different chromatographic columns and gradients were evaluated. Furthermore, four different extraction methods were evaluated; each utilized both different solvents, including ethyl acetate, methanol, and acetonitrile, and different workup steps. The best results were obtained by a modified QuEChERS method that lacked a workup step, and that included freezing the sample for 2 hours at -20 ºC. The results were satisfactory, yielding coefficients of variation of less than 20%, with the exception of the 50 µg L-1 sample of famoxadone, and recoveries between 70 and 120%, with the exception of acephate and bifenthrin; however, both analytes exhibited coefficients of variation of less than 20%.

Injúria potencial de herbicidas de solo ao girassol: II - chlorimuron-ethyl

Conduziu-se um ensaio de campo na Estação Experimental Agronômica da Universidade Federal do Rio Grande do Sul, em Eldorado do Sul, RS em 1989/90. O objetivo do trabalho foi determinar o efeito residual potencial do herbicida chlorimuron-ethyl aplicado em três doses à superficie do solo (PRE) ou incorporado no mesmo (PPI), sobre a cultura de girassol. A atividade de chlorimuron-ethyl (etil 2-((((4-cloro-6-metoxipirimidina-2 il)amino)carbonil)amino)sulfonil)benzoato) não foi dependente de sua posição no solo. Chlorimuron-ethyl promoveu injúria inicial acentuada, constatando-se pouca ou nenhuma resposta ao aumento da dose para matéria seca da parte aérea do girassol, área foliar e estatura das plântulas. Contudo, avaliação de estatura das plantas, realizada na maturação fisiológica, indicou que os danos promovidos pelo herbicida reduziram-se com o decorrer do tempo. Concluiu-se que, aparentemente, num sistema de sucessão soja-girassol, o efeito residual potencial de chlorimuron-ethyl ao girassol é pequeno.