Validation (in-house and collaboratory) of the quantification method for ethyl carbamate in alcoholic beverages and soy sauce by GC–MS

2013 ◽  
Vol 141 (4) ◽  
pp. 4161-4165 ◽  
Author(s):  
Zhu Huang ◽  
Xiao-Dong Pan ◽  
Ping-Gu Wu ◽  
Qing Chen ◽  
Jian-Long Han ◽  
...  
1994 ◽  
Vol 77 (6) ◽  
pp. 1530-1536 ◽  
Author(s):  
Benjamin J Canas ◽  
Frank L Joe ◽  
Gregory W Diachenko ◽  
Gordon Burns

Abstract A method using gas chromatography with mass selective detection for the determination of ethyl carbamate (EC; also known as urethane) in alcoholic beverages and soy sauce was collaboratively studied by 17 laboratories including authors’ laboratories. The method uses prepacked columns for extraction of liquids with methylene chloride, and n-propyl carbamate as the internal standard. A practice sample and 6 samples of distilled spirits, fortified wines, table wines, and soy sauces were analyzed by each collaborator. Each matrix included blind duplicates of incurred and fortified EC at 3 levels. Distilled spirits contained 50–330 ng EC/g (ppb), fortified wine 40–160 ppb, table wine 10–50 ppb, and soy sauce 15–70 ppb. The ranges of the repeatability relative standard deviations, excluding outliers, were 4.03–6.63% for distilled spirits, 4.01–5.05% for fortified wine, 3.94–6.73% for table wine, and 4.70–8.49% for soy sauce. The ranges of the reproducibility relative standard deviations, excluding outliers, were 8.53–9.49% for distilled spirits, 6.84–12.02% for fortified wine, 8.86–18.47% for table wine, and 13.87–27.37% for soy sauce. Recoveries of added EC ranged from 87 to 93%. Recoveries relative to reference values, labeled as the internal standard, obtained by using gas chromatography/ tandem mass spectrometry with a triple quadrupole mass spectrometer ranged from 89 to 100%.


1990 ◽  
Vol 53 (12) ◽  
pp. 1058-1061 ◽  
Author(s):  
YUKARI HASEGAWA ◽  
YUMIKO NAKAMURA ◽  
YASUHIDE TONOGAI ◽  
SHINJI TERASAWA ◽  
YOSHIO ITO ◽  
...  

A simple and sensitive method for the determination of ethyl carbamate (urethane) in various fermented foods has been developed. Twenty g of sample was homogenized and extracted with 150 ml of acetone. Twenty ml of water was added to the extract which was then evaporated to remove organic solvent. The residual aqueous solution was extracted three times with 100 ml of dichloromethane. The organic layer was concentrated by rotary evaporator and was charged on an acid-celite column. After washing the column with 100 ml of pentane and 100 ml of pentane-dichloromethane mixture (80:20), ethyl carbamate was eluted with 60 ml of dichloromethane. The eluant was concentrated to 1 ml using a rotary evaporator, and ethyl carbamate was determined by gas chromatography-mass spectrometry in the selected ion monitoring mode. For liquid samples, extraction with acetone was not necessary. The column purification step was also unnecessary for alcoholic beverages. The detection limit for this procedure was 0.5 ppb/sample, and the recovery was 70 to 105% for miso, moromi, natto, soy sauce, sake, yogurt, and bread when they were fortified with 5 to 50 ppb of ethyl carbamate. Ethyl carbamate levels in various fermented foods including yogurt, bread, mirin, or sakekasu were determined by this method. Relatively high levels of ethyl carbamate were detected in sake and soy sauce.


Food Control ◽  
2021 ◽  
Vol 124 ◽  
pp. 107867
Author(s):  
Sunghyeon Jung ◽  
Seungmin Kim ◽  
Inhwan Kim ◽  
Myung-Sub Chung ◽  
BoKyung Moon ◽  
...  

Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1474 ◽  
Author(s):  
Kai Zhou ◽  
Lorenzo Siroli ◽  
Francesca Patrignani ◽  
Yuanming Sun ◽  
Rosalba Lanciotti ◽  
...  

The aim of this work was to clarify the formation of ethyl carbamate (EC) and its influence factors throughout the production process of Cantonese soy sauce. The results showed that EC was not detected in the koji-making and early moromi fermentation stages, but started to be generated when pH of the moromi decreased to about 4.9—at the same time, the levels of ethanol, urea and citrulline increased significantly. Most EC was formed during raw soy sauce hot extraction (40.6%) and sterilization (42.9%) stages. The EC content exhibited the highest correlation with ethanol throughout the whole production process (R = 0.97). The simulation soy sauce produced in laboratory led the same conclusion—moreover, the contents of EC, ethanol and citrulline were higher in soy sauce fermented at 30 °C than in soy sauce fermented at 15 °C. Extraction of raw soy sauce by squeezing contributed little to EC formation. Further research showed that citrulline and ethanol led to significant increases in EC levels in raw soy sauce upon heating. These results indicate that ethanol and citrulline are two critical precursors of EC and that EC is mainly formed during the heat treatment stage of soy sauce.


Author(s):  
Gregory W. Diachenko ◽  
Benjamin J. Canas ◽  
Frank L. Joe ◽  
Michael DiNovi

2021 ◽  
Vol 343 ◽  
pp. 128528
Author(s):  
Kai Zhou ◽  
Francesca Patrignani ◽  
Yuan-Ming Sun ◽  
Rosalba Lanciotti ◽  
Zhen-Lin Xu

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