An Optimized Solid-Phase Microextraction and Gas Chromatography–Mass Spectrometry Assay for the Determination of Ethyl Palmitate in Hair

2020 ◽  
Vol 44 (4) ◽  
pp. 402-409 ◽  
Author(s):  
M F Bastiani ◽  
L L F Lizot ◽  
A C C Da Silva ◽  
R Z Hahn ◽  
S S Dries ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Incubation Temperature ◽  
Solid Phase ◽  
Drinking Behavior ◽  
Extraction Yield ◽  
Linear Range ◽  
Ethyl Esters ◽  
Gas Chromatography Mass Spectrometry ◽  
Ethyl Palmitate ◽  
Ethanol Drinking

Abstract The use of hair as a matrix for the evaluation of chronic ethanol drinking behavior presents the advantage of a longer window of detection and higher specificity when compared to classical biochemical markers. The most recent recommendations the Society of Hair Testing (SOHT) indicate that ethyl palmitate (EtP) hair levels can be used to estimate the ethanol drinking behavior, alternatively to the combined measurement of four main fatty acid ethyl esters. In this study, solid-phase microextraction (SPME) conditions for the extraction of EtP from hair were optimized using response surface analysis, after a Box–Behnken experiment. Analyses were performed by GC-MS. The optimized HS-SPME conditions, using a PDMS-DVB (65 μm) fiber, were pre-adsorption time of 6 min, extraction time of 60 min and incubation temperature of 94°C. The linear range was 0.05 to 3 ng mg−1, with accuracy within 95.15–109.91%. Between-assay and within-assay precision were 8.58–12.53 and 6.12–6.82%, respectively. The extraction yield was 61.3–71.9%. The assay was applied to hair specimens obtained from 46 volunteers, all presenting EtP levels within the linear range of the assay. Using a statistically designed experiment, a sensitive SPME-GC-MS assay for the measurement of EtP in hair was developed and validated, requiring only 20 mg of hair.

Variations in Main Flavor Compounds of Freshly Distilled Brandy during the Second Distillation

2014 ◽  
Vol 10 (4) ◽  
pp. 809-820 ◽  
Author(s):  
Yuping Zhao ◽  
Tiantian Tian ◽  
Jiming Li ◽  
Baochun Zhang ◽  
Ying Yu ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Ethyl Esters ◽  
Flavor Compounds ◽  
Gas Chromatography Mass Spectrometry ◽  
Benzene Derivatives ◽  
Distillation Process ◽  
Ethyl Hexanoate ◽  
Diethyl Succinate ◽  
Ethyl Octanoate

Abstract The present study investigated the variations in main flavor compounds of a Chinese brandy during the second distillation process using headspace–solid-phase microextraction coupled with gas chromatography-mass spectrometry. A total of 97 volatile compounds involving esters, alcohols, aldehydes, ketones, furans, benzene derivatives and terpenes were quantified, and 28 components were identified as key ingredients. By monitoring the second distillation process, it was found that most ethyl esters (ethyl hexanoate, ethyl octanoate, etc.), alcohols (3-methylbutanol, etc.), terpenes (linalool, etc.), acetaldehyde and ionone all had higher values at the beginning of the distillation, but declined gradually or sharply along with the distillation process. However, two esters (ethyl lactate and diethyl succinate), acids (acetic acid, hexanoic acid), benzene derivatives (2-phenylethanol, etc.) and furan (furfural) showed lower levels when the distillation was just started, and gradually increased, accumulating as a large quantity at the end of the distillation.

scholarly journals Processing of Flavor-Enhanced Oils: Optimization and Validation of Multiple Headspace Solid-Phase Microextraction-Arrow to Quantify Pyrazines in the Oils

Life ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 390
Author(s):  
Ziyan Xu ◽  
Chuan Zhou ◽  
Haiming Shi ◽  
Hong Zhang ◽  
Yanlan Bi ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Incubation Temperature ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Headspace Solid Phase Microextraction ◽  
Flavor Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

An efficient and effective multiple headspace-solid phase microextraction-arrow-gas chromatography-mass spectrometry (MHS-SPME-arrow-GCMS) analytical protocol is established and used to quantify the flavor compounds in oils. SPME conditions, such as fiber coating, pre-incubation temperature, extraction temperature, and time were studied. The feasibility was compared between SPME-arrow and the traditional fiber by loading different sample amounts. It was found that the SPME-arrow was more suitable for the MHS-SPME. The limit of detection (LODs) and limit of quantitation (LOQs) of pyrazines were in the range of 2–60 ng and 6–180 ng/g oil, respectively. The relative standard deviation (RSD) of both intra- and inter-day were lower than 16%. The mean recoveries for spiked pyrazines in rapeseed oil were in the range of 91.6–109.2%. Furthermore, this newly established method of MHS-SPME-arrow was compared with stable isotopes dilution analysis (SIDA) by using [2H6]-2-methyl-pyrazine. The results are comparable and indicate this method can be used for edible oil flavor analysis.

scholarly journals Study on Honey Quality Evaluation and Detection of Adulteration by Analysis of Volatile Compounds

2017 ◽  
Vol 61 (1) ◽  
pp. 17-27 ◽  
Author(s):  
Vojtěch Kružík ◽  
Adéla Grégrová ◽  
Aleš Rajchl ◽  
Helena Čížková
Keyword(s):  
Solid Phase Microextraction ◽  
Quality Evaluation ◽  
Phenylacetic Acid ◽  
Solid Phase ◽  
Quality Parameters ◽  
Ethyl Esters ◽  
Gas Chromatography Mass Spectrometry ◽  
Fast Evaluation ◽  
Three Samples

Abstract Fast evaluation of honey quality is a topical and significant problem of the food industry, bee keepers and consumers. In this work, 22 samples of commercially available honey aromas (with methyl and ethyl esters of phenylacetic acid predominated), 13 samples of authentic honey collected directly from bee keepers (characterised by high content of benzaldehyde, 2-phenylethanol, hotrienol and 2-phenylacetaldehyde) and 63 honeys purchased from an outdoor market were evaluated based on volatiles profiles determined through solid-phase microextraction coupled with gas chromatography-mass spectrometry (SPME-GC/MS) and then suspicious samples were identified. The results were statistically processed and compared with results of a sensory analysis. Six honeys, which differed significantly in volatiles profiles (outliers detected by Factor Analysis), selected volatile substance representation (furan-2-carbaldehyde, 1,4-dimethylpyrazole, benzaldehyde, 2-phenylacetaldehyde) and honey aroma intensity and pleasantness were subjected to targeted analyses (i.e. determination of 5-(hydroxymethyl)-2-furaldehyde, diastase activity, unauthorized additive presence). Four of these suspicious samples were found to have high content of 5-(hydroxymethyl)-2-furaldehyde (more than 40 mg/kg), three honeys had low values for diastase activity (less than 8) and three samples positive for triacetin addition. The fact that all these samples revealed a breach of least one of the selected quality parameters defined by the Codex Alimentarius standard proved the proposed methodology to be a useful tool for fast quality evaluation of honey.

scholarly journals Saccharomyces bayanus Enhances Volatile Profile of Apple Brandies

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3127
Author(s):  
Magdalena Januszek ◽  
Paweł Satora ◽  
Łukasz Wajda ◽  
Tomasz Tarko
Keyword(s):  
Gas Chromatography ◽  
Sensory Analysis ◽  
Solid Phase ◽  
Ethyl Esters ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Volatile Profile ◽  
Ethyl Palmitate ◽  
Saccharomyces Bayanus ◽  
The Impact

Qualitative and quantitative profiles of volatiles in alcoholic beverages depend mainly on the quality of raw materials, yeasts used for fermentation, and processing technique. Saccharomyces bayanus is a yeast species which is not commonly used for the production of alcoholic beverages, but it is able to produce volatiles that add desirable aroma. Since there is little information regarding the application of that microorganism for the production of apple brandies and how it affects volatile profile of finished products, we decided to address that issue. The aim of the study was to determine the impact of S. bayanus on the profile of volatile compounds and sensory properties of apple spirits obtained from three apple cultivars (Topaz, Rubin, and Elise) in comparison to spirits obtained from fermentation carried out spontaneously or with Saccharomyces cerevisiae. Obtained brandies were analysed using gas chromatography–flame ionization detector (GC–FID), solid phase microextraction–gas chromatography–mass spectrometry (SPME–GC–MS) and sensorially. In our study, brandies produced from musts fermented by S. bayanus demonstrated the highest concentration of ethyl esters and increased concentrations of isoamyl acetate, 2-phenylethyl acetate, ethyl palmitate and hexanol. Moreover, our results support the hypothesis that non-Saccharomyces yeasts which are present during spontaneous fermentation and demonstrate higher β-glucosidase activities enhance aroma of alcoholic beverages through releasing aroma compounds from glycosidic forms, e.g., α-phellandrene, (E)-β-fanesene, (Z,E)-α-farnesene, α-farnesene, and farnesol. Considering results obtained in sensory analysis, we proved that S. bayanus is suitable for the production of apple brandies, improving their flavour. Brandies obtained from musts fermented by S. bayanus obtained the highest average range for “overall note” parameter in sensory analysis.

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