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

Machado, Ana Maria de Resende; Cardoso, María das Graças; Emídio, Elissandro Soares; Prata, Vanessa de Menezes; Dórea, Haroldo Silveira; Anjos, Jeancarlo Pereira dos; Magriotis, Zuy M.; Nelson, David Lee

doi:10.1080/00032719.2012.673101

Cited by 6 publications

(9 citation statements)

References 20 publications

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“…and amburana ( A. cearensis ) casks and obtained recoveries in the range of 87–108%. In addition to the studies cited, the values are close to those observed in other studies using GC–MS . The results obtained for the quantification of EC in the samples of cane juice, fermented must and in the head, heart and tail fractions are represented in Table .…”

Section: Resultssupporting

confidence: 87%

“…Therefore, other factors and stages of the production process that may influence the formation of EC in beverages should be investigated because the presence of copper has not been shown to be relevant to the formation of EC. Machado et al worked with nitrogen fertilization of the cane in the expectation that the nitrogen supplied to the sugarcane could influence the composition of the nitrogen compounds. The authors concluded that the different doses of urea and ammonium nitrate did not lead to an increase in the concentration of EC.…”

Section: Resultsmentioning

confidence: 99%

“…Instrumentally, the determination of EC in beverages and foods is limited because of the low concentrations of this analyte and because of possible interference from other compounds in the matrix. Thus, EC can be determined directly or after pre‐treatment (clean‐up and concentration) via solvent extraction, solid‐phase extraction or solid phase micro‐extraction .…”

Section: Introductionmentioning

confidence: 99%

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Determination of ethyl carbamate in cachaça stored in newly made oak, amburana, jatobá, balsa and peroba vats and in glass containers

et al. 2017

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Ethyl carbamate was quantified in cachaça using high‐performance liquid chromatography with fluorescence detection during the production process and during storage in different types of wooden casks and glass containers, with and without the presence of light. According to the physicochemical analysis, the head and tail fractions are unacceptable for consumption. Ethyl carbamate was detected in sugarcane juice and during fermentation. During distillation, ethyl carbamate levels ranged from the limit of detection to 17.1 μg L−1. Ethyl carbamate increased during storage in wooden casks. The presence (or absence) of light did not affect the formation of ethyl carbamate in cachaça stored in glass containers. Copyright © 2017 The Institute of Brewing & Distilling

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Section: Resultssupporting

confidence: 87%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Determination of ethyl carbamate in cachaça stored in newly made oak, amburana, jatobá, balsa and peroba vats and in glass containers

et al. 2017

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“…Machado et al . , in an effort to clarify the formation of ethyl carbamate, worked with the effect of the application of nitrogen fertilizer on sugarcane in the expectation that the nitrogen supplied to the sugarcane would influence the composition of nitrogenous compounds. The authors concluded that the different doses of urea and ammonium nitrate did not cause an increase in the concentration of ethyl carbamate, there being no formation of ethyl carbamate during the planting and growing of the sugarcane.…”

Section: Resultsmentioning

confidence: 99%

“…In addition, other nitrogen-containing compounds have been studied as potential precursors for the formation of ethyl carbamate before and after the distillation process, such as carbamyl phosphate and the cyanide ion (22). Machado et al (23), in an effort to clarify the formation of ethyl carbamate, worked with the effect of the application of nitrogen fertilizer on sugarcane in the expectation that the nitrogen supplied to the sugarcane would influence the composition of To better demonstrate the results of this research, the following chromatograms (Figs. 2, 3 and 4) of sugarcane juice and cachaça aged for 12 months in oak and amburana barrels are presented.…”

Section: Resultsmentioning

confidence: 99%

Ethyl carbamate in the production and aging of cachaça in oak (Quercussp.) and amburana (Amburana cearensis) barrels

et al. 2014

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There are residual organic and inorganic contaminants in the cachaça production chain. Among the organic contaminants, ethyl carbamate has been widely studied. It is formed naturally during the fermentation processes and can be found in many foods and beverages such as bread, yoghurt, wine, beer and especially in fermented-distilled beverages such as whiskey, rum, vodka, grappa, cachaça and tiquira. The objective of this study was to identify and quantify ethyl carbamate during the steps of the production process and aging of cachaça in oak (Quercus sp) and amburana (Amburana cearensis) barrels. The cane used for cachaça production, as well as the process for obtaining the fermentation broth, did not affect the formation of ethyl carbamate, as it was not detected. Carbamate was detected in low concentrations, but was not quantified, in the fermentation, distillation and aging steps.

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A Sensitive Method for the Rapid Determination of Underivatized Ethyl Carbamate in Fortified Wine by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Leça

Pereira

et al. 2017

Food Anal. Methods

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This work presents the optimization of a miniaturized liquid-liquid extraction (mLLE) followed by reversed-phase liquid chromatography-electrospray tandem mass spectrometry (RP-HPLC-MS/MS) for the determination of ethyl carbamate (EC) in fortified wine, without using derivatizing agents. The mLLE was optimized by an experimental design. Thus, 15 mL of wine and 8 mL of ethyl acetate were used for the extraction. After concentration, each extract was injected into the HPLC-MS/MS equipment and the characteristic secondary ion transition of EC (m/z = 90.10 → 62.05) was used for the quantification purposes. The proposed method presented a good linearity (R 2 = 0.9999) and a high sensitivity with low limits of detection (LOD) and quantification (LOQ), 0.17 and 0.52 μg L −1 , respectively. The precision (repeatability and reproducibility) never exceeded 8% of variation, and the recoveries varied between 93 and 114%. The applicability of the method was checked through the analysis of 24 fortified wines, with EC values ranging between 23 ± 1 and 194 ± 5 μg L −1 . All chromatograms revealed good peak resolutions. This new method is efficient for the simple, fast, and reliable determination of EC in fortified wines, providing great sensitivity without using derivatizing agents or large volumes of organic solvents.

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

Cited by 6 publications

References 20 publications

Determination of ethyl carbamate in cachaça stored in newly made oak, amburana, jatobá, balsa and peroba vats and in glass containers

Determination of ethyl carbamate in cachaça stored in newly made oak, amburana, jatobá, balsa and peroba vats and in glass containers

Ethyl carbamate in the production and aging of cachaça in oak (Quercussp.) and amburana (Amburana cearensis) barrels

A Sensitive Method for the Rapid Determination of Underivatized Ethyl Carbamate in Fortified Wine by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

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