Quantitation of ethyl carbamate in whiskey, sherry, port, and wine by gas chromatography/tandem mass spectrometry using a triple quadrupole mass spectrometer

Brumley, William C.; Canas, Benjamin J; Perfetti, Gracia A; Mossoba, Magdi M.; Sphon, James A.; Corneliussen, Paul E

doi:10.1021/ac00161a006

Cited by 34 publications

(29 citation statements)

References 18 publications

(19 reference statements)

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“…Therefore, in the last decade GC-MS-MS has been widely used in various fields (e.g., food, medicine, agriculture and environment; Brumley et al, 1988;Ternes et al, 2002;Frenich et al, 2005Frenich et al, , 2007Hernandez et al, 2005;Isaacson et al, 2006;Tripp et al, 2009;Parr et al, 2011). In organic geochemistry at present, GC-MS-MS is predominantly used to investigate terpenoids and steroids (Peters et al, 2005).…”

Section: Introductionmentioning

confidence: 99%

Quantitative analysis of diamondoids in crude oils using gas chromatography–triple quadrupole mass spectrometry

Liang

Xiong

Fang

et al. 2012

Organic Geochemistry

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Section: Introductionmentioning

confidence: 99%

Quantitative analysis of diamondoids in crude oils using gas chromatography–triple quadrupole mass spectrometry

Liang

Xiong

Fang

et al. 2012

Organic Geochemistry

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“…Under these conditions, many reactions can occur leading to significant changes in wine, some are crucial to the final remarkable characteristics of Madeira wine, however it may also cause production of ethyl carbamate (EC). According to Stevens and Ough [2], under fairly normal storage temperatures (13)(14)(15)(16)(17)(18)(19)(20)(21)(22)(23)(24) • C), and not uncommon concentrations of urea (1-10 mg/L), a significant amount of EC will accumulate in wine.…”

Section: Introductionmentioning

confidence: 99%

“…Several extraction methodologies have been used, such as continuous liquid-liquid extraction [13], and solid phase extraction [7,14,15], combined with one-dimensional gas chromatography coupled with mass spectrometry detection (GC-MS). EC has been determined in fortified Madeira wines by SPE followed by GC-MS [15,16], and by derivatization with 9-xanthydrol, followed by high performance liquid chromatography (HPLC) [17].…”

Section: Introductionmentioning

confidence: 99%

“…The extraction step is followed mainly by GC-MS analysis [7,13,15,16]. To achieve the adequate sensitivity for EC detection, an injector equipped with a unit for large volume injection [7], or MS-SIM (selected ion monitoring) [13,19] or MS-MS acquisition modes (GC-MS-MS) [9,14,21] were used. Onedimensional chromatographic processes are widely applied in the analysis of food products.…”

Section: Introductionmentioning

confidence: 99%

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Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

Perestrelo

Petronilho

Câmara

et al. 2010

Journal of Chromatography A

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a b s t r a c tAn analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r 2 ) higher than 0.981. A good precision was attained (R.S.D. <20%) and low detection limits (LOD) were achieved for dry (4.31 g/L) and sweet (2.75 g/L) model wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 g/L and 88.6%, whereas for sweet wines were 9.16 g/L and 99.4%, respectively. The higher performance was attainted with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 g/L (medium dry) to 162.5 g/L (medium sweet).

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“…Muitas metodologias analíticas vêm sendo propostas para a determinação de carbamato de etila em alimentos, todas empregando a cromatografia a gás com diferentes dispositivos de detecção [12][13][14][15][16][17][18][19] . Em função das baixas concentrações em que se encontra o carbamato de etila nas bebidas alcoólicas e da baixa sensibilidade que alguns detectores apresentam, faz-se necessário além da concentração das amostras uma etapa de desidratação dos extratos, geralmente com Na 2 SO 4 anidro 14,15,20 , tornando estes procedimentos morosos e mais susceptíveis a erros. …”

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

et al. 2002

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ETHYL CARBAMATE IN ALCOHOLIC BEVERAGES (CACHAÇA, TIQUIRA, WHISKY AND GRAPE). 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.Keywords: GC-MS; ethyl carbamate; alcoholic beverages; spirits. . A comparação entre os teores de carbamato de etila em bebidas alcoólicas brasileiras com os limites estabelecidos pelo Canadá é inevitável, em função de este ser, até o momento, o único país a possuir legislação específica sobre o assunto, sendo um referencial para os EUA e para a Comunidade Européia. Em março de 1990, o FDA ("U. S. Food and Drug Administration") publicou nota 11 na qual os produtores de uísques americanos se comprometeram, a partir daquela data, a limitar o teor de carbamato de etila em 0,125 mg L -1 . Muitas metodologias analíticas vêm sendo propostas para a determinação de carbamato de etila em alimentos, todas empregando a cromatografia a gás com diferentes dispositivos de detecção [12][13][14][15][16][17][18][19] . Em função das baixas concentrações em que se encontra o carbamato de etila nas bebidas alcoólicas e da baixa sensibilidade que alguns detectores apresentam, faz-se necessário além da concentração das amostras uma etapa de desidratação dos extratos, geralmente com Na 2 SO 4 anidro 14,15,20 , tornando estes procedimentos morosos e mais susceptíveis a erros. INTRODUÇÃOA cromatografia a gás acoplada à espectrometria de massas (GC-MS) torna-se muito conveniente para a determinação de carbamato de etila em bebidas destiladas, pois além da elevada sensibilidade 5,18 quando se opera no modo SIM, não há a necessidade de se desidratar as amostras 5 . No presente trabalho aplicou-se a cromatografia a gás acoplada à espectrometria de massas, na determinação de carbamato de etila em bebidas fermento-destiladas. Também efetuou-se a comparação dos teores deste contaminante entre os destilados nacionais e os destilados estrangeiros. Os resultados foram analisados considerandose fatores ligados à região, tipo de destilação, coloração da embalagem e tempo de envelhecimento. PARTE EXPERIMENTAL ReagentesTodos os reagentes utilizados foram de grau analítico. O carbamato de etila foi adquirido da Sigma-Aldrich. Utilizou-se etanol Mallinckrodt e água destilada desionizad...

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Quantitation of ethyl carbamate in whiskey, sherry, port, and wine by gas chromatography/tandem mass spectrometry using a triple quadrupole mass spectrometer

Cited by 34 publications

References 18 publications

Quantitative analysis of diamondoids in crude oils using gas chromatography–triple quadrupole mass spectrometry

Quantitative analysis of diamondoids in crude oils using gas chromatography–triple quadrupole mass spectrometry

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

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

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