scholarly journals Safety Evaluation of the Grape Marc Spirit by GC-FID Analysis

Author(s):  
Teodora Coldea ◽  
Elena Mudura ◽  
Nicoleta Ranta ◽  
Darius Hadarean

There were investigated grape marc spirits regarding their safety on consumers. Major volatile compounds which present risk to human health (such as methanol, furfural, and acetaldehyde) and ethyl alcohol content were compared to European Union Regulation and other values found in previous studies.  The aim of our study was to evaluate the safety of grape marc spirits considering their content in major volatile compounds by comparison with the requirements of European Union Regulation. We investigated the ethyl alcohol content by electronic densimetry and 10 major volatile compounds (acetaldehyde, ethyl acetate, methanol, 1-propanol, 1-butanol, 2-butanol, isobutyl alcohol, isoamyl alcohol, amyl active alcohol and furfural) by Gas Chromatography coupled with Flame Ionization Detector. We used reference chemicals to identify these compounds and 3-pentanol as internal standard to quantify the volatiles. Results were compared with the requirements of European Union Regulation. All major volatile compounds registered values in accordance to EU Regulation and the grape pomace spirits samples do not present any kind of risk for consumption.

OENO One ◽  
2004 ◽  
Vol 38 (4) ◽  
pp. 225 ◽  
Author(s):  
Maria Gerogiannaki-Christopoulou ◽  
Nikolaos V. Kyriakidis ◽  
Panagiotis E. Athanasopoulos

<p style="text-align: justify;">Agrape pomace distillate was produced from 4 Greek white grape varieties (<em>Vitis vinifera</em> L.). Pomace was fermented with and without addition of citric acid, acting as an antibacterial agent, during fermentation. Fermented grape pomace was distilled in a traditional copper distillation apparatus.. Five major volatile compounds, including methanol, were measured. Pentanol-3 was used as an internal standard. Flame ionization detector (FID) coupled to capillary gas chromatography was used for determination of five volatile distillate components. The addition of citric acid resulted in the reduction of methanol content by about 15%. All the other components studied did not affect in any appreciable degree.</p>


1971 ◽  
Vol 17 (2) ◽  
pp. 82-85 ◽  
Author(s):  
Naresh C Jain

Abstract An extremely simple, rapid method is described for simultaneously determining methanol, ethanol, acetone, isopropanol, and low-boiling hydrocarbons associated with glue sniffing. Less than 1 µl of blood, mixed with an internal standard, is injected directly into a low-cost gas chromatograph equipped with a flame-ionization detector. No extraction, distillation, and (or) sample preparation is required, and the method is sensitive to less than 10 µg of alcohol per ml.


Author(s):  
Manda V. ◽  
Popescu M. ◽  
Baniceru M.

Two simple, sensitive and specific gas and liquid chromatographic methods are developed and validated for quantification of articaine in human whole blood. Liquid-liquid extraction with n-hexane-isoamyl alcohol 90:10 (v/v) is used for sample preparation in both methods. GC-FID (gas chromatographic-flame ionization detection) analysis is performed with a gas chromatograph equipped with a split-splitless injector, flame-ionization detector and HP INNOwax capillary column. Reverse phase LC-PDA (liquid chromatographic-photo diode array detection) analysis is carried out using a C18 Hypersil GOLD column with two mobile phases: acetonitrile-water 10 mM ammonium acetate 50:50 (v/v), pH 7, and acetonitrile-buffer solution sodium acetate 10 mM and acetic acid 10 mM 50:50 (v/v), pH 4.7, respectively. A comparison between GC-FID and LC-PDA is performed, as well as between internal and external standard as quantification methods in LC. The best results in terms of accuracy (as recovery) and precision (as relative standard deviation) are obtained in GC (95-98% and 5.5-8.2%, respectively) with lidocaine internal standard and in LC (96-102% and 4.2-6.1%, respectively) with external standard and mobile phase pH 4.7. This method is applied in a preliminary pharmacokinetic study to three healthy volunteers to whom anesthesia with articaine is performed.


Analytica ◽  
2021 ◽  
Vol 2 (3) ◽  
pp. 84-92
Author(s):  
Silvia Arduini ◽  
Alessandro Zappi ◽  
Marcello Locatelli ◽  
Salvatore Sgrò ◽  
Dora Melucci

An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of “grappa”, a product which has peculiar tradition and production in its country of origin. Therefore, the evaluation of its authenticity plays an important role for its consumption in Italy, as well as for its exportation all around the world. For the present work, 123 samples of grappa and several kinds of spirits were analyzed in their alcohol content by electronic densimetry, and in their volatile fraction by gas-chromatography with a flame-ionization detector. Part of these samples (94) was employed as a training set to compute a chemometric model (by linear discriminant analysis, LDA) and the other part (29 samples) was used as a test set to validate it. Finally, two grappa samples seized from the market by the Italian Customs and Monopolies Agency and considered suspicious due to their aroma reported as non-compliant were projected onto the LDA model to evaluate the compliance with the “grappa” class. A further one-class classification method by principal component analysis (PCA) was carried out to evaluate the compliance with other classes. Results showed that the suspicious samples were not recognized as belonging to any of the analyzed spirit classes, confirming the starting hypothesis that they could be grappa samples adulterated in some way.


Author(s):  
Teodora Emilia COLDEA ◽  
Carmen SOCACIU ◽  
Maria TOFANÄ‚ ◽  
Elena Vá‰KONY ◽  
Nicoleta RANTA

There were analyzed samples of fruit distillates from the two stages of distillation process, first distillate and the second distillate, as apple brandy originating from Bistriţa-Năsăud County, Transylvania provenience and were collected directly from the producer soon after the process ended. We investigated 10 major volatile compounds (acetaldehyde, ethyl acetate, methanol, 1-propanol, 1butanol, 2-butanol, isobutylic alcohol, isoamylic alcohol, amyl active alcohol and furfural) by gas chromatography coupled with flame ionization detector (GC-FID). We used reference chemicals to identify these compounds and 3-pentanol as internal standard to quantify the volatiles. This analysis permitted to observe the differences between the two distillates. Acetaldehyde, ethyl acetate and methanol have smaller amounts in the second distillation step. Furfural and higher alcohols registered different evolution in the last distillation step. They were higher then in the first distillate. The factors which differentiate the two samples can be separation of fractions (heads, hearts and tails), temperature, quality of raw material and the fermentation process. 


1983 ◽  
Vol 48 (3) ◽  
pp. 722-734
Author(s):  
Martin Koval

The flame ionisation detector response to C6-C11 aliphatic hydrocarbon solutions in carbon disulphide in the concentration range between 1.3-9.5 mg ml-1 retained lineary despite the excess of solvent entering the detector simultaneously with the analyte. Pure carbon disulphide exhibited a small positive detector response which did not interfere in calibration procedure and which, under certain GC conditions, inverted to negative values. This response was not proportional to the injected volume and was strongly influenced by the column temperature and/or bleed. On the basis of these findings, a method compatible with the widely used charcoal tube carbon disulphide desorption procedure was developed and evaluated. It consists of static desorption of the sum of aliphatic alkanes and cycloalkanes from the activated charcoal after which an internal standard is added to the supernatant eluate. The resulting carbon disulphide solution is analysed on a highly polar stationary phase 1,2,3-tris(2-cyanoethoxy)propane where the solvent and the analyte coelute in a single peak, the height of which is practically proportional to the sum of alkanes and cycloalkanes present. This also makes determinations of other substances present in the sample more simple. The field test of the proposed method yielded values comparable in precision and accuracy with a control infrared spectrophotometric method.


2019 ◽  
Vol 11 (1) ◽  
pp. 1-10
Author(s):  
Olawale Paul Olatidoye ◽  
Taofik Akinyemi Shittu ◽  
Samuel Olusegun Awonorin ◽  
Emmanuel Sunday Akin Ajisegiri

The use of inappropriate temperature-time combinations during the roasting of nuts could lead to quality defects, such as burnt taste, short shelf-life, rancidity, and poor flavour. In this study, cashew kernels were roasted in a forced airflow-drying oven for 20, 40,and 60 min at 100, 120, 140, and 160°C. The productswere evaluated for volatile flavour compounds and the sensory evaluation of the roasted cashew kernelsat different roasting conditions. The volatile fraction was isolated using the combined steam distillation–extraction procedure and identified by gas chromatography–flame-ionization detection (GC-FID). The consumer acceptability test was carried out by 100 panellists using nine point hedonic scales to assess preferences for like or dislike, colour, taste, texture, flavour,and overall acceptability. It was found that there were significant differences in flavour compounds between the different conditions of roasting. Twenty-nine volatile compounds were identified in both fresh and roasted cashew kernelscomprising five main classes,which consist of 12 hydrocarbons, eight aldehydes, four ketones, three alcohols,and one acid. The volatile compounds(mg/100g) ranged from 5.03x10-2to 1.20 (2-butanone), 7.46x10-6to 1.85 (hexanal), 8.91x10-6to 1.94 (acetone), 6.74x10-1to 2.24 (benzaldehyde). The amount of generated volatile compounds increased astheroasting temperature and time increased. The consumer acceptability test revealed that samples roasted for 40 or 60 min at 140°C produced the most acceptable product in terms of all the measured attributes. The study showed that the roasting conditions produced acceptable cashew kernelsof desirable colour and superior flavour quality that enhance direct and commercial utilization.


1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).


1983 ◽  
Vol 29 (7) ◽  
pp. 1404-1407 ◽  
Author(s):  
F A Muskiet ◽  
G Jansen ◽  
B G Wolthers ◽  
A Marinkovic-Ilsen ◽  
P C van Voorst Vader

Abstract We describe a rapid method for determining cholesterol sulfate in plasma and erythrocytes. After its single-step isolation by means of anion-exchange chromatography cholesterol sulfate is hydrolyzed, trimethylsilylated, and determined by gas chromatography with flame ionization detection. 5 beta-Cholestan-3 alpha-ol sulfate is used as internal standard. The method enables simultaneous determination of dehydroepiandrosterone sulfate in plasma. We applied it for the diagnosis of seven patients with recessive X-linked ichthyosis. Concentrations are given for plasma and erythrocytes from four unaffected relatives of patients with X-linked ichthyosis, a patient with placental sulfatase deficiency, two patients with other types of ichthyoses, and 20 controls. The method may also be of use for the rapid isolation of other organic sulfates from biological material, as illustrated by a comparison of gas chromatograms of urine from a normal pregnant woman and that from a patient with placental sulfatase deficiency.


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