scholarly journals Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters

Foods ◽  
2021 ◽  
Vol 10 (10) ◽  
pp. 2487
Author(s):  
Marinos Xagoraris ◽  
Foteini Chrysoulaki ◽  
Panagiota-Kyriaki Revelou ◽  
Eleftherios Alissandrakis ◽  
Petros A. Tarantilis ◽  
...  

For long heather honey has been a special variety due to its unique organoleptic characteristics. This study aimed to characterize and optimize the isolation of the dominant volatile fraction of Greek autumn heather honey using solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS). The described approach pointed out 13 main volatile components more closely related to honey botanical origin, in terms of occurrence and relative abundance. These volatiles include phenolic compounds and norisoprenoids, with benzaldehyde, safranal and p-anisaldehyde present in higher amounts, while ethyl 4-methoxybenzoate is reported for the first time in honey. Then, an experimental design was developed based on five numeric factors and one categorical factor and evaluated the optimum conditions (temperature: 60 °C, equilibration time: 30 min extraction time: 15 min magnetic stirrer velocity: 100 rpm sample volume: 6 mL water: honey ratio: 1:3 (v/w)). Additionally, a validation test set reinforces the above methodology investigation. Honey is very complex and variable with respect to its volatile components given the high diversity of the floral source. As a result, customizing the isolation parameters for each honey is a good approach for streamlining the isolation volatile compounds. This study could provide a good basis for future recognition of monofloral autumn heather honey.

Molecules ◽  
2021 ◽  
Vol 26 (12) ◽  
pp. 3612
Author(s):  
Marinos Xagoraris ◽  
Alexandra Skouria ◽  
Panagiota-Kyriaki Revelou ◽  
Eleftherios Alissandrakis ◽  
Petros A. Tarantilis ◽  
...  

This study aimed at an experimental design of response surface methodology (RSM) in the optimization of the dominant volatile fraction of Greek thyme honey using solid-phase microextraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS). For this purpose, a multiple response optimization was employed using desirability functions, which demand a search for optimal conditions for a set of responses simultaneously. A test set of eighty thyme honey samples were analyzed under the optimum conditions for validation of the proposed model. The optimized combination of isolation conditions was the temperature (60 °C), equilibration time (15 min), extraction time (30 min), magnetic stirrer speed (700 rpm), sample volume (6 mL), water: honey ratio (1:3 v/w) with total desirability over 0.50. It was found that the magnetic stirrer speed, which has not been evaluated before, had a positive effect, especially in combination with other factors. The above-developed methodology proved to be effective in the optimization of isolation of specific volatile compounds from a difficult matrix, like honey. This study could be a good basis for the development of novel RSM for other monofloral honey samples.


Biomolecules ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 896
Author(s):  
Emili Besalú ◽  
Chantal Prat ◽  
Enriqueta Anticó

This study describes a new chemometric tool for the identification of relevant volatile compounds in cork by untargeted headspace solid phase microextraction and gas chromatography mass spectrometry (HS-SPME/GC-MS) analysis. The production process in cork industries commonly includes a washing procedure based on water and temperature cycles in order to reduce off-flavors and decrease the amount of trichloroanisole (TCA) in cork samples. The treatment has been demonstrated to be effective for the designed purpose, but chemical changes in the volatile fraction of the cork sample are produced, which need to be further investigated through the chemometric examination of data obtained from the headspace. Ordinary principal component analysis (PCA) based on the numerical description provided by the chromatographic area of several target compounds was inconclusive. This led us to consider a new tool, which is presented here for the first time for an application in the chromatographic field. The superposing significant interaction rules (SSIR) method is a variable selector which directly analyses the raw internal data coming from the spectrophotometer software and, combined with PCA and discriminant analysis, has been able to separate a group of 56 cork samples into two groups: treated and non-treated. This procedure revealed the presence of two compounds, furfural and 5-methylfurfural, which are increased in the case of treated samples. These compounds explain the sweet notes found in the sensory evaluation of the treated corks. The model that is obtained is robust; the overall sensitivity and specificity are 96% and 100%, respectively. Furthermore, a leave-one-out cross-validation calculation revealed that all of the samples can be correctly classified one at a time if three or more PCA descriptors are considered.


2018 ◽  
Vol 13 (8) ◽  
pp. 1934578X1801300 ◽  
Author(s):  
Armando A. Durant-Archibold ◽  
Noris Salazar Allen ◽  
Anette Garrido ◽  
Jose Gudiño Ledezma ◽  
Mahabir P. Gupta

We report for the first time the chemical composition of volatile components (VOCs) of two subspecies, D. hirsuta subsp. hirsuta and D. hirsuta subsp. nepalensis, of the liverwort Dumortiera hirsuta from Panama by using headspace-solid phase microextraction-gas chromatography-mass spectrometry in order to assess distinguishing markers between the two species. Forty VOCs were identified in total for both subspecies. Of these, 34 are reported for the first time in D. hirsuta. Furthermore, both subspecies showed clear differences in the type and amount of VOCs. The major compounds in D. hirsuta subsp. hirsuta were α-gurjunene, β-selinene, α-guaiene, α-humulene and β-caryophyllene; while in D. hirsuta subsp. nepalensis were ledene, α-gurjunene, β-caryophyllene and α-guaiene, respectively. Two oxygenated sesquiterpenes, globulol and nerolidol, could be considered as possible distinguishing chemical markers between these two subspecies. We conclude that both morphotypes of D. hirsuta are chemically different.


2013 ◽  
Vol 9 (2) ◽  
pp. 227-232 ◽  
Author(s):  
Abdul Ghani Liew Abdullah ◽  
Nik Meriam Sulaiman ◽  
Mohamed Kheireddine Aroua ◽  
Che Rosmani Che Hassan

AbstractVolatiles are important flavor compounds of fruit juices and beverages. In this study, a headspace Solid-phase microextraction (SPME) gas chromatography-mass spectrometry (GC-MS) was used to analyze the volatile components in starfruit juices. Several experimental parameters (e.g. adsorption temperature, adsorption time, and sample volume) were optimized to improve sampling efficiency in two aspects; maximum adsorption and selective adsorption of volatile components onto SPME fiber. The following conditions were found to be optimal for selectivity and sensitivity: adsorption temperature of 50°C for 30 min, with a 65 μm divinylbenzene /polydimethylsiloxane (DVB/PDMS)-coated fiber with a sample volume of 15 g in a 30-ml vial. The proposed technique could be applied for the analysis of volatile compounds that contribute to starfruit juices flavor in different cultivars, and also their ripening stages.


2019 ◽  
Vol 14 (8) ◽  
pp. 1934578X1986887
Author(s):  
Anette Garrido ◽  
Jose Gudiño Ledezma ◽  
Armando A. Durant-Archibold ◽  
Noris Salazar Allen ◽  
Juan Carlos Villarreal A ◽  
...  

We report for the first time the chemical profiling of volatile organic compounds (VOCs) of gametophyte and sporophyte life stages of Leiosporoceros dussii, from Panama by using headspace-solid phase microextraction-gas chromatography-mass spectrometry in order to assess distinguishing chemical markers between the male and female gametophytes, and sporophytes of this hornwort. A total of 27 VOCs were identified in L. dussii. Furthermore, the gametophyte and sporophyte showed clear differences in the type and amount of VOCs. The main constituents of L. dussii female thalli were menthacamphor (17.8%), hexanol (12.3%), and menthyl acetate (12.3%), while the major compounds of the male thalli were hexanol (25.3%), β-ionone (21.1%), benzeneacetaldehyde (17.6%), and β-cyclocitral (14.0%). The main VOCs of the sporophytes were hexanal (19.3%), β-cyclocitral (17.6%), 2-nonenal (15.8%), hexanol (12.5%), and β-ionone (10.2%). Unique compounds found in the female thalli were 3-pentanone, 3-octenol, nonanol, estragole, and menthyl acetate, and in the male thalli were methyl heptenone, nonanal, neoisomenthol, and bornyl acetate. Isomenthol, thymol, isomenthol acetate, and β-methylnaphthalene were only found in the sporophyte. The characteristic VOCs identified in L. dussii suggest a difference between the chemical constituents of L. dussii and other hornworts species. The presence of simple VOCs when compared with compounds previously characterized in another hornwort genera may support the distinct genetic nature of this species.


2011 ◽  
Vol 74 (4) ◽  
pp. 651-657 ◽  
Author(s):  
E. J. YANG ◽  
Y.-S. KIM ◽  
H. C. CHANG

The aim of this study was to purify and identify an antifungal compound from Lactobacillus plantarum AF1, which was isolated from kimchi. The antifungal compound was purified by solid-phase extraction and recycling preparative high-performance liquid chromatography, and its structure was elucidated by using gas chromatography–mass spectrometry (GC-MS). The active compound from L. plantarum AF1 was confirmed to be δ-dodecalactone (molecular weight, 198.3) by comparison of its gas chromatographic retention time with the mass spectrum of standard δ-dodecalactone. The MICs of δ-dodecalactone against various fungi and bacteria ranged from 350 to 6,250 μg/ml. δ-Dodecalactone showed strong antifungal activity against molds Aspergillus flavus, A. fumigatus, A. petrakii, A. ochraceus, A. nidulans, and Penicillium roqueforti. The three tested yeast strains of Candida albicans were more resistant than the molds. Antibacterial activity was evident but less potent than the antifungal activity. δ-Dodecalactone produced pleasurable (fruity) organoleptic characteristics. The results indicate the potential of the δ-dodecalactone produced by L. plantarum AF1 as a biopreservative and flavoring compound, as well as a biosafe remedy for candidiasis.


Proceedings ◽  
2020 ◽  
Vol 70 (1) ◽  
pp. 75
Author(s):  
Alexandra Nanou ◽  
Athanasios Mallouchos ◽  
Efstathios Z. Panagou

Olives are characterized by a wide variety of volatile compounds, which are primarily products of microbial metabolism that contribute to the organoleptic characteristics of the final product and especially to its flavor. The volatilome in Spanish-style processed green olives of Conservolea and Halkidiki cultivars were analytically characterized. A solid phase micro-extraction (SPME) technique was used for the extraction of volatile components from the olive samples that were further identified and quantified by gas chromatography coupled to mass spectrometry (GC–MS). Eighty-eight (88) compounds were identified, including several aldehydes, ketones, acids, terpenes, but mainly esters and alcohols. Results showed that there were no significant differences in the qualitative composition of the volatile profiles between the two varieties. Acetic and propanoic acids, thymol, ethanol, 2-butanol, 1-propanol, ethyl acetate as well as ethyl propanoate were the most dominant compounds found in both cultivars. However, some quantitative differences were spotted between the two varieties regarding some of the identified volatile compounds. The quantity of 2-butanol was higher in the Halkidiki variety, while propanoic acid ethyl ester was found in higher amounts in the Conservolea variety. Furthermore, differences in the quantities of some volatile compounds over time were observed. Most of the identified compounds presented an increasing trend during storage.


Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3842
Author(s):  
Alessandro D’Alessandro ◽  
Daniele Ballestrieri ◽  
Lorenzo Strani ◽  
Marina Cocchi ◽  
Caterina Durante

Basil is a plant known worldwide for its culinary and health attributes. It counts more than a hundred and fifty species and many more chemo-types due to its easy cross-breeds. Each species and each chemo-type have a typical aroma pattern and selecting the proper one is crucial for the food industry. Twelve basil varieties have been studied over three years (2018–2020), as have four different cuts. To characterize the aroma profile, nine typical basil flavour molecules have been selected using a gas chromatography–mass spectrometry coupled with an olfactometer (GC–MS/O). The concentrations of the nine selected molecules were measured by an ultra-fast CG e-nose and Principal Component Analysis (PCA) was applied to detect possible differences among the samples. The PCA results highlighted differences between harvesting years, mainly for 2018, whereas no observable clusters were found concerning varieties and cuts, probably due to the combined effects of the investigated factors. For this reason, the ANOVA Simultaneous Component Analysis (ASCA) methodology was applied on a balanced a posteriori designed dataset. All the considered factors and interactions were statistically significant (p < 0.05) in explaining differences between the basil aroma profiles, with more relevant effects of variety and year.


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