Determination of Ethyl Carbamate in Various Fermented Foods by Selected Ion Monitoring

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.

1988 ◽  
Vol 71 (4) ◽  
pp. 781-784 ◽  
Author(s):  
William M Pierce ◽  
Adora O Clark ◽  
Harrell E Hurst

Abstract Quantitative methods are detailed for determination of ethyl carbamate in distilled alcoholic beverages by capillary gas chromatography with flame ionization detection (GC/FID) and by packedcolumn gas chromatography/mass spectrometry (GC/MS) using selected ion monitoring. Five g samples of distillate of known ethanol concentration are diluted with water to 25% ethanol (v/v), washed with petroleum ether, and extracted with dichloromethane prior to GC/FID or GC/MS analysis. As necessary, sample extracts that exhibit GC/FID interference are passed through alumina for additional cleanup. When internal standards (ferf-butyl carbamate and n-butyl carbamate for GC/FID, or ethyl ,3C-,sN-carbamate for GC/ MS) were used for quantitation, the limit of detection for ethyl carbamate was in the range of 5-25 ppb. Coefficients of variation ranged from 3.5 to 6.0% for GC/FID determinations, and from 1.4 to 3.2% for GC/MS. Correlation between methods for 22 random distillate samples ranging in concentration from approximately 40 to 800 ppb gave a correlation coefficient (r) of 0.996.


2015 ◽  
Vol 31 (3) ◽  
pp. 289-297 ◽  
Author(s):  
Dayeon Ryu ◽  
Bogyoung Choi ◽  
Eunjoo Kim ◽  
Seri Park ◽  
Hwijin Paeng ◽  
...  

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%.


Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.


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