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

1987 ◽  
Vol 70 (4) ◽  
pp. 749-751 ◽  
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.

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

1987 ◽  
Vol 70 (4) ◽  
pp. 749-751
Author(s):  
Henry B.S. Conacher ◽  
B.Denis 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.

scholarly journals Comparison of Methods for Extraction of Ethyl Carbamate from Alcoholic Beverages in Gas Chromatography/Mass Spectrometry Analysis

2006 ◽  
Vol 89 (4) ◽  
pp. 1048-1051 ◽  
Author(s):  
Armen Mirzoian ◽  
Md. Abdul Mabud
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Ethyl Carbamate ◽  
Alcoholic Beverages ◽  
Mass Spectrometry Analysis ◽  
Gas Chromatography Mass Spectrometry ◽  
Official Method ◽  
Chromatography Mass Spectrometry ◽  
Limit Of Quantitation

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.

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.

scholarly journals IDENTIFICATION OF CANNABIMIMETIC MDMB(N)-073F METABOLITES IN URINE BY METHOD OF GAS CHROMATOGRAPHY WITH MASS SPECTROMETRIC DETECTION

2019 ◽  
Vol 7 (2) ◽  
pp. 70-83 ◽  
Author(s):  
S. S. Kataev ◽  
O. N. Dvorskaya ◽  
M. A. Gofenberg
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Acute Poisoning ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Urine Samples ◽  
Instrumental Method ◽  
Phase Extraction

Background. At the beginning of 2019, the use of a new representative of synthetic cannabimimetics of the methylbutanoate indazole carboxamides group, MDMB(N)-073F, was recorded in a number of regions in the Russian Federation. Characteristic features of the pharmacological effect, the clinical picture of MDMB(N)-073F poisoning have not been studied, the psychoactive effects produced by MDMB(N)-073F remain unexplored. In this regard, the study of the new cannabimimetic metabolism is an important aspect in establishing the fact of taking MDMB(N)-073F during expert studies of biological objects.The aim of the research is identifying metabolites of synthetic MDMB(N)-73F cannabimimetics in real urine samples using solid-phase extraction (SPE) and gas chromatography (GC) with mass spectrometric detection (GC-MS).Materials and methods. 10 urine samples were collected from March 15 to March 29, 2019. 8 urine samples were taken from the medical examination offices of the city of Yekaterinburg and the Sverdlovsk region from the persons examined for intoxication; 2 urine samples were obtained from the patients of the Sverdlovsk regional center of acute poisoning upon enrolment to the toxic-intensive care unit with a preliminary diagnosis of “acute poisoning by synthetic cannabimimetics”. In the research, SampliQ EVIDEX-200 mg – 3 ml (Agilent, USA) cartridges were used for the sample preparation; β-glucuronidase Type HP-2, From Helix Pomatia, 100000 U/ml (Sigma-ALDRICH CHEMI, Germany) was used for enzymatic hydrolysis. Gas chromatography – mass spectrometry with the use of Agilent 7820 gas chromatograph with Agilent 5975 mass selective detector (Agilent, USA) was used as an instrumental method of the analysis.Results. The metabolites that make it possible to establish the fact of taking MDMB(N)-073F cannabimimetics via urine screening procedure to detect the presence of narcotic and medicinal substances with the use of solid-phase extraction and gas chromatography methods with mass spectrometry, have been described. The major metabolites MDMB(N)-073F in the urine of smoking mixtures consumers have been identified. The metabolism of MDMB(N)-073F has been found to be mainly due to hydrolysis of the ester group, hydroxylation, oxidative defluorination and N-dealkylation. Most of the resulting metabolites are excreted in the urine in the conjugated form.Conclusion. Gas chromatographic and mass spectrometric characteristics of some derivatives of the main metabolites of the new synthetic MDMB(N)-073F cannabimimetic have been obtained. This data can be used in the practice of forensic chemical and chemical toxicological analysis.

scholarly journals Development, Optimization and Validation of a Sustainable and Quantifiable Methodology for the Determination of 2,4,6-Trichloroanisole, 2,3,4,6-Tetrachloroanisole, 2,4,6-Tribromoanisole, Pentachloroanisole, 2-Methylisoborneole and Geosmin in Air

Processes ◽  
2021 ◽  
Vol 9 (9) ◽  
pp. 1571
Author(s):  
Patricia Jové ◽  
Marina Vives-Mestres ◽  
Raquel De Nadal ◽  
Maria Verdum
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
High Temperature ◽  
Thermal Desorption ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Air Analysis ◽  
Good Linearity ◽  
Repeatability And Reproducibility

Compounds 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA), 2-methylisoborneol (2MIB) and geosmin (GSM) have been reported as being responsible for cork and wine taint. A sustainable method based on thermal desorption-gas chromatography–mass spectrometry (TD-GC/MS) has been developed and optimized, taking into account desorption parameters and chromatographic and mass spectrometric conditions. The combination of parameters that jointly maximized the compound detection was as follows: desorption temperature at 300 °C, desorption time at 30 min, cryo-temperature at 20 °C and trap high temperature at 305 °C. The proposed methodology showed a good linearity (R ≤ 0.994) within the tested range (from 0.1 to 2 ng) for all target compounds. The precision expressed as repeatability and reproducibility was RSD < 10% in both. The limits of quantification ranged from 0.05 to 0.1 ng. The developed methodology and the sampling rates (R-values) of all targeted compounds (from 0.013 to 0.071 m3 h−1) were applied to the air analysis of two wineries. The results showed that the developed methodology is a sustainable and useful tool for the determination of these compounds in air.

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%

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