Derivatization followed by gas chromatography-mass spectrometry for quantification of ethyl carbamate in alcoholic beverages

Abstract A procedure to analyze ethyl carbamate (EC) by gas chromatography/mass spectrometry was optimized and validated. Deuterated EC (d5-EC) was added to the samples as an internal standard followed by extraction with polystyrene crosslinked polystyrene cartridges using minimal volumes of ethyl acetate. The EC response was measured in selective ion monitoring (SIM) mode and found to be linear in the range between the limit of quantitation (10 μg/L) and 1000 μg/L. EC recoveries varied from 92 to 112%, with the average value of 100 ± 8%. The procedure compared well (r2 = 0.9970) with the existing AOAC Official Method with the added benefits of minimal solvent usage and reduced matrix interferences.

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Analysis of Ethyl Carbamate in Wines Using Solid-Phase Extraction and Multidimensional Gas Chromatography/Mass Spectrometry

Journal of Agricultural and Food Chemistry ◽

10.1021/jf025559s ◽

2002 ◽

Vol 50 (21) ◽

pp. 5797-5802 ◽

Cited By ~ 48

Author(s):

Eshwar Jagerdeo ◽

Sumer Dugar ◽

Gregory D. Foster ◽

Hilary Schenck

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Solid Phase Extraction ◽

Solid Phase ◽

Ethyl Carbamate ◽

Gas Chromatography Mass Spectrometry ◽

Phase Extraction ◽

Multidimensional Gas Chromatography ◽

Chromatography Mass Spectrometry

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Quantification ethyl carbamate in wines using reaction-assisted-extraction with 9-xanthydrol and detection by heart-cutting multidimensional gas chromatography-mass spectrometry

Analytica Chimica Acta ◽

10.1016/j.aca.2017.11.022 ◽

2018 ◽

Vol 1001 ◽

pp. 86-92 ◽

Cited By ~ 4

Author(s):

Qiqi Tu ◽

Wanshu Qi ◽

Junbo Zhao ◽

Li Zhang ◽

Yinlong Guo

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Ethyl Carbamate ◽

Gas Chromatography Mass Spectrometry ◽

Multidimensional Gas Chromatography ◽

Chromatography Mass Spectrometry ◽

Assisted Extraction

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Capillary Column Gas Chromatographic Determination of Ethyl Carbamate in Alcoholic Beverages with Confirmation by Gas Chromatography/Mass Spectrometry

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/70.4.749 ◽

1987 ◽

Vol 70 (4) ◽

pp. 749-751 ◽

Cited By ~ 1

Author(s):

Henry B S Conacher ◽

Denis B Page ◽

Benjamin P Y Lau ◽

James F Lawrence ◽

Ruth Bailey ◽

...

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Capillary Column ◽

Methylene Chloride ◽

Ethyl Carbamate ◽

Mass Spectrometric ◽

Mass Spectrometric Detection ◽

Alcoholic Beverages ◽

Gas Chromatography Mass Spectrometry ◽

Acetate Solution

Abstract A method is described for determining ethyl carbamate at low \i%l kg levels in several types of alcoholic beverages by capillary column gas chromatography with Hall electrolytic conductivity detection and confirmation by mass spectrometry. Samples are diluted to obtain a uniform concentration of ethanol (ca 10%) then saturated with NaCl and extracted with methylene chloride. Extracts are evaporated to a small volume and injected in ethyl acetate solution for chromatographic analysis. The method was evaluated by 5 laboratories, 4 employing the Hall detector and one using mass spectrometric detection. Overall between-laboratory mean percent recoveries were: wine, 85.3 ± 21.0% coefficient of variation (CV) (spiking level 20- 45 μg/kg); sherry, 83.8 ± 16.1% CV (spiking level, 81-142 μg/kg);whiskey, 79.5 ± 13.9% CV (spiking level 127-190 Mg/kg); and brandy, 85.0 ± 12.5% CV (spiking level 297-446 μg/kg). Mass spectrometric results agreed well with the Hall results for all commodities. Detection limits were about 5 μg/kg for the Hall detector and about 0.5 μg/kg for mass spectrometric detection.

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