Ethyl Carbamate Levels in Selected Fermented Foods and Beverages

1989 ◽  
Vol 72 (6) ◽  
pp. 873-876 ◽  
Author(s):  
Benamin J Canas ◽  
Donald C Havery ◽  
Louis R Robinson ◽  
Michael P Sullivan ◽  
frank L Joe ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Gas Chromatography Mass Spectrometry ◽  
Fermented Foods ◽  
Energy Analyzer ◽  
Gas Chromatograph ◽  
Distilled Spirits ◽  
Mass Spectrometry Mass Spectrometry

Abstract Ethyl carbamate (EC), also known as urethane, is an animal carcinogen and a by-product of fermentation. Because EC has been found in distilled spirits and wines, a variety of fermented foods and beverages were analyzed to assess its occurrence in other products. Previously described methods using a gas chromatograph-thermal energy analyzer with a nitrogen converter were modified for each matrix and gave recoveries of >80%, with a limit of detection in the 1-2 μg/kg(ppb) range. A total of 152 test samples were analyzed; EC levels ranged from none found to 3 ppb in 15 cheeses, 6 teas, 12 yogurts, and 8 ciders; from none found to 13 ppb in 30 breads and 69 malt beverages; and from none found to 84 ppb in 12 soy sauces. Gas chromatography/mass spectrometry/mass spectrometry was used to confirm EC identity and to quantitate EC in selected food extracts

Rapid Gas Chromatographic Method for Determining Ethyl Carbamate in Alcoholic Beverages with Thermal Energy Analyzer Detection

1988 ◽  
Vol 71 (3) ◽  
pp. 509-511
Author(s):  
Canas Benjamin J ◽  
Donald C HaVery ◽  
Frank L Joe
Keyword(s):  
Mass Spectrometry ◽  
Thermal Energy ◽  
Methylene Chloride ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Energy Analyzer ◽  
Elution Method ◽  
Gas Chromatographic Method

Abstract A rapid column elution method has been developed for the determination of ethyl carbamate (EC) in alcoholic beverages. The beverage is mixed with Celite and packed in a column containing deactivated alumina capped with a layer of sodium sulfate. EC is then eluted with methylene chloride. The method, using a gas chromatograph- thermal energy analyzer with a nitrogen converter for detection and quantitation of EC, has been applied to a variety of alcoholic beverages. Recoveries ± standard deviations of EC in wine and whisky fortified at the 20 and 133 µg/kg (ppb) levels averaged 87.3 ± 5.3 and 88.7 ± 3.6%, respectively. The method has a limit of detection of 1.5 ppb. Gas chromatography/mass spectrometry/ mass spectrometry was used to confirm the identity and quantitation of EC in selected beverage extracts.

Determination and Confirmation of N-Nitrosodimethylamine in Beer

1981 ◽  
Vol 64 (6) ◽  
pp. 1457-1461
Author(s):  
Denis Andrzejewski ◽  
Donald C Havery ◽  
Thomas Fazio
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Lower Limit ◽  
Thermal Energy ◽  
Capillary Gas Chromatography ◽  
Qualitative Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Energy Analyzer ◽  
Gas Chromatograph ◽  
Chromatography Mass Spectrometry

Abstract A qualitative method has been developed for the confirmation of N-nitrosodimethylamine (NDMA) in beer by capillary gas chromatography-mass spectrometry (GC/MS) from full mass scans after quantitation, using a gas chromatograph interfaced to a thermal energy analyzer (GC/TEA). The GC/MS method has a lower limit of confirmation of 5 ppb. In a survey of 22 imported and 42 domestic beers, NDMA was found in 60 samples by GC/TEA at levels up to 7.7 ppb, and was confirmed by GC/MS in 5 samples.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

Determination of Phytosterols in Butter Samples by Using Capillary Column Gas Chromatography

1987 ◽  
Vol 70 (5) ◽  
pp. 912-915 ◽  
Author(s):  
Randall L Smith ◽  
Darryl M Sullivan ◽  
Earl F Richter
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Packed Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Positive Bias ◽  
Capillary Column Gas Chromatography

Abstract A positive bias in the gas chromatographic (GC) analysis of butter for β-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from β-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate β-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%

Separation and Characterization of Amine Drugs and Their Enantiomers by Capillary Column Gas Chromatography-Mass Spectrometry

1983 ◽  
Vol 66 (6) ◽  
pp. 1443-1446
Author(s):  
Ray H Liu ◽  
Warren W Ku ◽  
Mary P Fitzgerald
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mass Spectrometer ◽  
Capillary Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Chromatograph ◽  
Capillary Column Gas Chromatography ◽  
Spectrometer Data ◽  
Amine Drug

Abstract A gas chromatograph-mass spectrometer-data system equipped with a capillary column is used to analyze commonly abused amine drug mixtures. Enantiomeric amines are analyzed as N-trifluoroacetyl- I-prolyl chloride derivatives. The 10 compounds included in this study are amphetamine, methamphetamine, norephedrine, ephedrine, 3,-4-methylenedioxyamphetamine, N,N-dimethyltryptamine, N,N-diethyltryptamine, N,N-dimethyl-5-methoxytryptamine, mescaline, and caffeine. All compounds, including possible enantiomers, are resolved and identified by the described method.

scholarly journals Development of Sensitive and Specific Analysis of Vildagliptin in Pharmaceutical Formulation by Gas Chromatography-Mass Spectrometry

2015 ◽  
Vol 2015 ◽  
pp. 1-7
Author(s):  
Ebru Uçaktürk
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Formulation ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Validation Parameters ◽  
Diagnostic Ions

A sensitive and selective gas chromatography-mass spectrometry (GC-MS) method was developed and fully validated for the determination of vildagliptin (VIL) in pharmaceutical formulation. Prior to GC-MS analysis, VIL was efficiently derivatized with MSTFA/NH4I/β-mercaptoethanol at 60°C for 30 min. The obtained O-TMS derivative of VIL was detected by selected ion monitoring mode using the diagnostic ionsm/z223 and 252. Nandrolone was chosen as internal standard. The GC-MS method was fully validated by the following validation parameters: limit of detection (LOD) and quantitation (LOQ), linearity, precision, accuracy, specificity, stability, robustness, and ruggedness. LOD and LOQ were found to be 1.5 and 3.5 ng mL−1, respectively. The GC-MS method is linear in the range of 3.5–300 ng mL−1. The intra- and interday precision values were less than ≤3.62%. The intra- and interday accuracy values were found in the range of-0.26–2.06%. Finally, the GC-MS method was successfully applied to determine VIL in pharmaceutical formulation.

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