Determination of ethyl carbamate in wine by GC‐SIM‐MS after continuous extraction with diethyl ether

Fauhl, C.; Wittkowski, R.

doi:10.1002/jhrc.1240150315

Cited by 16 publications

(13 citation statements)

References 11 publications

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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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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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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“…Gas chromatography coupled with mass spectrometry (GC/MS) seems to be the method of choice for the analysis of ethyl carbamate in alcoholic beverages 3, 6, 12, 19–28. The overwhelming majority of these procedures involves a quadrupole mass spectrometer operating in selected ion monitoring (SIM) mode.…”

mentioning

confidence: 99%

“…Gas chromatography coupled with mass spectrometry (GC/MS) seems to be the method of choice for the analysis of ethyl carbamate in alcoholic beverages. 3,6,12,[19][20][21][22][23][24][25][26][27][28] The overwhelming majority of these procedures involves a quadrupole mass spectrometer operating in selected ion monitoring (SIM) mode. However, the analysis of minor organic compounds in complex matrices like spirit drinks is difficult because of interferences by matrix components, even when extensive cleanup procedures are applied to the sample, e.g.…”

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confidence: 99%

Application of tandem mass spectrometry combined with gas chromatography to the routine analysis of ethyl carbamate in stone‐fruit spirits

Lachenmeier

Frank

Kuballa

2004

Rapid Comm Mass Spectrometry

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Gas chromatography (GC) coupled to mass spectrometry (MS) operated in selected ion monitoring (SIM) mode is currently the method of choice for the determination of the toxic contaminant ethyl carbamate in alcoholic beverages. However, even after extensive sample cleanup over diatomaceous earth columns, the identity of ethyl carbamate often cannot be ascertained with confidence, due to inconsistent ratios of the SIM ions m/z 62, 74 and 44 because the qualifier ions are highly susceptible to interferences. Therefore, a new method combining GC and tandem MS using a triple-quadrupole instrument is introduced to determine ethyl carbamate in stone-fruit spirits. For quantitative analysis the characteristic transitions of m/z 74 --> 44 and m/z 62 --> 44 for ethyl carbamate as well as m/z 64 --> 44 for the deuterated internal standard ethyl carbamate-d5 were monitored in the multiple reaction monitoring (MRM) mode. In the validation studies, ethyl carbamate exhibited good linearity with a regression coefficient of 1.000. The limits of detection and quantitation were 0.01 and 0.04 mg/L. The recovery of the method was 100.4 +/- 9.4%. The precision never exceeded 7.8% (intraday) and 10.1% (interday) and the trueness never exceeded 11.3% (intraday) and 12.2% (interday) at any of the concentrations examined, indicating good assay accuracy. A good agreement of analytical results between a previously developed GC/MS SIM method and the GC/MS/MS MRM procedure was found (R=0.987). Regarding the validation data, the procedure is sensitive, selective and reproducible. The applicability of the developed method was demonstrated by the investigation of 70 stone-fruit spirits from commercial trade. The ethyl carbamate concentration of the samples ranged between 0.07 and 7.70 mg/L (mean 1.21 mg/L). The main advantage of the developed GC/MS/MS method is the reliability of the results without the need for time-consuming confirmatory analyses.

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Compounds Responsible for Wine Defects

Flamini

Traldi

2009

Mass Spectrometry in Grape and Wine Chemistry

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Determination of ethyl carbamate in wine by GC‐SIM‐MS after continuous extraction with diethyl ether

Cited by 16 publications

References 11 publications

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

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

Application of tandem mass spectrometry combined with gas chromatography to the routine analysis of ethyl carbamate in stone‐fruit spirits

Compounds Responsible for Wine Defects

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