Jeancarlo Pereira dos Anjos

Determination of ethyl carbamate in cachaça produced from copper stills by HPLC

Ethyl carbamate (EC) is a common substance in fermented foods and drinks, and its quantification is important because of its carcinogenic nature and its usually presence in alcoholic beverages. The present work involved the development and validation of an analytical method for the evaluation of EC in cachaça by HPLC-FLD after previous derivatization with xanthydrol. The method presented a mean recovery of 94.88%, an intra-day precision of 4.19% (30.0 μgL(-1)) and 3.32% (75.0 μgL(-1)), a coefficient of determination (r(2)) equal to 0.9985, and limits of detection and quantification equal to 6.39 and 21.32 μgL(-1), respectively. The results show that the analytical method is accurate, reproducible and linear over the concentration range from 5.0 to 160 μg of EC per litre. The method was applied to the analysis of EC in cachaça, the analyses being rapid and efficient.

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 cachaca 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.

Determinação das composições físico-químicas de cachaças do sul de minas gerais e de suas misturas

Este trabalho teve por objetivo a determinacao da composicao fisico-quimica de cachacas artesanais produzidas no sul do Estado de Minas Gerais e suas misturas. Foram analisados os teores de etanol, acidez volatil, aldeidos, cobre, esteres, alcoois superiores totais e metanol, alem dos alcoois propanol-1, isobutanol e 3-metil-butanol-1. Os resultados apresentam o perfil peculiar desta bebida, que apresentou teores satisfatorios de alcoois superiores, esteres e aldeidos. O teor de cobre apresenta-se como preocupante ja que algumas amostras excederam o limite de 5 mg.L-1. A producao de misturas foi estudada e esta apresenta-se como uma alternativa viavel ao produtor e cooperativas.

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.

Evolution of the concentration of phenolic compounds in cachaça during aging in an oak (Quercus sp.) barrel

A cachaca, tradicional e popular bebida brasileira, e obtida por meio da destilacao do mosto fermentado de cana de acucar. Dentre as etapas do processo de producao da bebida, o envelhecimento natural consiste em armazena-la em recipientes de madeira apropriados por um tempo determinado, onde ocorrem alteracoes na composicao quimica, aroma, sabor e cor da bebida. Este trabalho teve como objetivo realizar um acompanhamento da composicao fenolica em diferentes periodos de envelhecimento da cachaca em tonel de carvalho (Quercus sp.). Foram realizadas coletas periodicas durante o periodo de envelhecimento da cachaca em tonel de carvalho e realizaram-se analise de treze compostos fenolicos utilizando a tecnica de cromatografia liquida de alta eficiencia com detector de arranjo de diodos (HPLC-DAD). Foi constatado um aumento progressivo na concentracao dos compostos analisados ao longo do periodo analisado, sendo que os compostos encontrados em maior concentracao foram siringaldeido e acido galico.

Parâmetros físico-químicos e cromatográficos em aguardentes de cana queimada e não queimada

Este trabalho teve por objetivo avaliar as concentracoes de furfural, alcoois superiores, esteres, aldeidos, cobre, acidez volatil, metanol e grau alcoolico de aguardentes obtidas de cana, com e sem queima previa. Foram utilizadas amostras de aguardente artesanal de cana queimada e nao queimada, fermentadas com a mesma levedura e destiladas no mesmo destilador; amostras de produtor de aguardente industrial de cana queimada e amostras obtidas de outro produtor artesanal de cana nao queimada. As analises fisico-quimicas e cromatograficas (CG) foram realizadas no Laboratorio de Analise Fisico-Quimica de Aguardente - LAFQA/DQI na Universidade Federal de Lavras. As concentracoes de furfural apresentaram diferenca significativa (P<0,01), entre os grupos de aguardentes artesanais, obtidas de cana-de-acucar com e sem queima previa, oriundas de um mesmo processo de producao, com medias de 1,48 mg.100mL-¹ etanol e 0,63 mg.100mL-¹ etanol, respectivamente, embora tenham estado abaixo do limite maximo (5,0 mg.100mL-¹ etanol) permitido. Os demais componentes das aguardentes estudadas nao foram afetados significativamente pela queima previa da cana-de-acucar.

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 cachaca samples varied from <LD to 17.46 µg L-1, for the period during which the cachaca was stored in an oak barrel, and <LQ to 18.51 µg L-1 for the cachaca stored in a glass recipient. The storage of the beverage in both the oak barrel and the glass vessel resulted in a significant increase in the concentration of this contaminant.

Contamination of cachaça by PAHs from storage containers.

Cachaça is a distiled beverage obtained from the fermentation of sugar cane syrup that, depending on the production procedures, may be susceptible to contamination by polycyclic aromatic hydrocarbons (PAHs). These compounds present carcinogenic and/or mutagenic properties and offer a risk to human health. Sixteen PAHs were determined in cachaças that had been stored in glass bottles and in polyethylene tank by gas chromatography coupled with mass spectrometry. The quantification of the PAHs utilised an internal standard. The limits of detection and quantification varied from 0.05 to 0.10μgL(-)(1) and 0.20 to 0.30μgL(-)(1), respectively. A total PAH concentration of 51.57μgL(-)(1) was found in the beverages that were stored in the tank, while the concentration in the cachaça stored in glass jugs was 6.07μgL(-)(1). These results indicate that the polyethylene tank is a source for PAHs in cachaça.

Determination of Phenolic Compounds and Coumarins in Sugar Cane Spirit Aged in Different Species of Wood

The identities and quantities of the phenolic compounds and coumarins in twelve samples of sugar cane spirit aged in Quercus sp., Amburana cearensis, Cariniana legalis, Castanea sativa Mill, Ocotea sp., Cotyledon orbiculata L., and Hymenaea sp. casks were determined. These compounds have a direct influence on the sensory characteristics of aged beverages; some of them are considered to be markers for the aging process. The analysis of phenolic compounds was performed by HPLC. Solid phase extraction (SPE) was also used for the determination of coumarins. The concentrations of the principal compounds extracted varied according to the species of wood. The concentrations of total phenolic compounds ranged from 0.08 for a sample stored in a 4000-L jatobá barrel for a period of six months to 40.9 mg · L−1 for a sample aged in a 50000-L oak barrel for a period of 48 months. The use of the SPE technique removed interfering compounds from the samples, thereby improving the detection of coumarin.

Experimental Design Methodology to Optimize the Solid Phase Microextraction Procedure Prior to GC/MS Determination of Ethyl Carbamate in Samples of Homemade Cachaça

Seeking to improve the quality of cachaça, the Ministério da Agricultura, Pecuária e Abastecimento (Ministry of Agriculture, Livestock and Supply - MAPA), the body responsible for setting and approving regulations governing the Identity and Quality Standards (PIQs) for distilled sugar cane spirits and cachaça, through the Normative Instruction No. 13 of 2005 included some contaminants such as ethyl carbamate (EC), acrolein, lead, and arsenic that must be evaluated in these drinks. Studies on EC, as well as the methods for its determination, are required to evaluate and determine which factors contribute to the formation of this compound in the beverage. An analytical method using gas chromatography/mass spectrometry (GC/MS) with prior sample treatment by solid phase microextraction (SPME) was developed along with the assessment of the principal validation parameters. These two developments lead to the determination of EC with analytical reliability. The optimization of the extraction step was performed via a factorial design involving the selection of parameters such as extraction time, extraction temperature, salt concentration, desorption time, pH, and the method of extraction. The linear range was 5.0 to 200.0 µg L−1 (R2 = 0.9965) with limits of detection and quantification of 1.5 and 5.0 µg L−1, respectively. The recoveries for samples of cachaça containing 10.0 and 80.0 µg L−1 concentrations of EC were 89% and 93%, respectively. The concentrations of EC in the samples of cachaça examined were well below the limits required by Brazilian law.