Residue levels of ethyl carbamate in wines and spirits by gas chromatography and mass spectrometry/mass spectrometry

Cairns, Thomas; Siegmund, Emil G.; Luke, Milton A.; Doose, Gregory M.

doi:10.1021/ac00144a010

Cited by 26 publications

(16 citation statements)

References 6 publications

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“…The limits of detection and quantitation were 0.01 and 0.04 mg/L, respectively, being over 10 times lower than the limits of the corresponding GC/MS SIM procedure. The limit of detection attained by GC/MS/MS was comparable with that of the method of Cairns et al 36. The sensitivity of the method is, therefore, adequate to check the upper limit of 0.4 mg/L in stone‐fruit spirits.…”

Section: Resultsmentioning

confidence: 99%

“…As a result of the use of a deuterated internal standard in combination with MRM, the precision never exceeded 7.8% relative standard deviation (RSD) (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. No lack of accuracy in the CID of ethyl carbamate, as reported in early GC/MS/MS experiments,36 was observed during our study.…”

Section: Resultsmentioning

confidence: 99%

“…For a long time this technology was restricted to expensive instruments, and only used to provide structural confirmation of samples that were positive in conventional GC/MS. In the analysis of spirit drinks, a lack of accuracy and precision in the collision‐induced dissociation (CID) of ethyl carbamate was reported 36. Recently, the introduction of low‐cost benchtop triple‐quadrupole mass spectrometers made it possible to adopt these techniques in routine analysis, e.g.…”

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confidence: 99%

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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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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

mentioning

confidence: 99%

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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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“…(Conacher et al 1987, Cairns et al 1987, nitrogen-phosphorus thermionic (Bailey et al 1986, Baumann and, flame ionization (Andrey 1987, Van Ingen et al 1987, chemiluminescence (Dennis et al 1986) and mass spectrometry (Aylott et al 1987, Cairns et al 1987, Mildau et al 1987. Application of these methods has resulted in a growing body of data on ethyl carbamate levels in alcoholic beverages.…”

Section: Introductionmentioning

confidence: 99%

Investigation of ethyl carbamate levels in some fermented foods and alcoholic beverages

Dennis

Howarth

Key

et al. 1989

Food Additives and Contaminants

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An analytical procedure has been developed for the determination of trace amounts of ethyl carbamate in fermented foodstuffs and alcoholic beverages. Concentrations were generally below the 1-5 micrograms/kg detection limit in bread, cheese, yoghurt, beer, gin and vodka. Higher concentrations were found in the other alcoholic beverages examined, which included whisky, fruit brandy, liqueur, wine, sherry and port.

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“…Some methods still include an additional extraction cleanup step 4,15 . Ethyl carbamate detection is usually performed by mass spectrometry [1][2][3][4]7,8,15 , either on electron or chemical ionization 23,24 . Other detection techniques such as Hall electrolytic conductivity detection and thermal energy analyzer in nitrogen detection have also been applied 25,26 .…”

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confidence: 99%

Ultra-Trace Determination of Methyl Carbamate and Ethyl Carbamate in Local Wines by GC-FID Following Pre concentration with C18-SPE

Sarawan

Chanthai²

2014

Orient. J. Chem

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Residue levels of ethyl carbamate in wines and spirits by gas chromatography and mass spectrometry/mass spectrometry

Cited by 26 publications

References 6 publications

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

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

Investigation of ethyl carbamate levels in some fermented foods and alcoholic beverages

Ultra-Trace Determination of Methyl Carbamate and Ethyl Carbamate in Local Wines by GC-FID Following Pre concentration with C18-SPE

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