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 LIST OF PUBLICATIONS ON the PHASER (GC-O)
- Evaluation of Leaf-Derived Extracts as an Environmentally Sustainable Source of Essential
Oils by Using Gas Chromatography-Mass Spectrometry and Enantioselective Gas Chromatography-Olfactometry
Barbara d’Acampora Zellner, Maria Lo Presti, Lauro Euclides Soares Barata, Paola Dugo,
Giovanni Dugo and Luigi Mondello. Anal. Chem. 2006, 78, 883-890
<< Read Abstract >>
In consideration of the world's present environmental situation and the threat of species extinction, investigations concerning alternative sustainable sources of natural substances represent an extremely important issue. In this respect, the present research is focused on the analytical evaluation of Brazilian rosewood (Aniba rosaeodora Ducke) leaves, as an alternative source (with respect to wood) of rosewood essential oil and, as such, of natural linalool, which is extensively used in perfumery. Enantioselective-gas chromatography-olfactometry (Es-GC-O) was used as a tool for the simultaneous stereodifferentiation and olfactive evaluation of the volatile optically active components present in the analyzed samples. In addition to Es-GC-O analyses, direct olfactive analyses were also performed, enabling the evaluation of the global aroma exerted by each sample and the influence of each linalool antipode, as also other minor compounds. The samples were also submitted to gas chromatography-mass spectrometric analysis, thus establishing their chemical profiles. The assessment of enantiopure chiral compounds through Es-GC-O, along with direct olfactive analyses, confirmed that the leaves are a potential substituent for wood in the extraction of Brazilian rosewood essential oil, representing a sustainable nonwood source of natural linalool.
- Odour fingerprint acquisition by means of comprehensive two-dimensional gas chromatography-olfactometry and comprehensive two-dimensional
gas chromatography/mass spectrometry
Barbara d’Acampor Zellner, Paola Dugo, Giovanni Dugo, Luigi Mondello. Journal of Chromatography A, 1141 (2007) 279–286
<< Read Abstract >>
The analysis of complex matrices, such as perfumes, by means of gas chromatography-olfactometry (GC-O) can be rather imprecise due
to the co-elutions, leading to a possible masking of odour-active trace-level compounds by major interferences or agglomeration of olfactive
impressions resulting in unreliable olfactive characterization. To overcome these limits an innovative technique, comprehensive two-dimensional
gas chromatography-olfactometry (GC×GC-O), was applied, revealing several relevant co-elutions, as in the linalool and linalyl acetate zones. A
total of 177 compounds, out of these 135 odour-active, were detected by GC-O, while about 481 out of 818 compounds presented odour-activity
through GC×GC-O analyses. In addition, GC/mass spectrometry (GC/MS) and GC×GC/MS analyses were also performed. Peak assignment
was achieved by means of different information sources, such as GC/MS, GC×GC/MS, LRI, injection of standards and olfactive impressions.
- Identification of New, Odor-Active Thiocarbamates in Cress Extracts and Structure-Activity Studies on Synthesized Homologues
Katharina Breme, Xavier Fernandez, Uwe J. Meierhenrich, Hugues Brevard, and Daniel Joulain. J. Agric. Food Chem. 2007, 55, 1932-1938
<< Read Abstract >>
New, odorant nitrogen- and sulfur-containing compounds are identified in cress extracts. Cress belongs
to the botanical order Brassicales and produces glucosinolates, which are important precursors of nitrogen- and sulfur-containing compounds. Those compounds often present low perception thresholds and various olfactive notes and are thus of interest to the flavor and fragrance chemistry. When the study of organonitrogen and organosulfur compounds is undertaken, Brassicale extracts are one of the matrices of choice. Cress extracts were studied by analytical (GC-MS, GC-FPD) and chemical
(fractionation) means to identify new interesting odorant compounds. Two compounds that have never
been reported in cress extracts, containing both nitrogen and sulfur, were discovered: N-benzylO-ethyl
thiocarbamate and N-phenethyl O-ethyl thiocarbamate. These two molecules being of organoleptic
interest, their homologues were synthesized and submitted to organoleptic tests (static and GCsniffing).
Their odors evolve from garlic and onion over green, mushroom- and cress-like to fresh,
spearmint-like. This paper presents the origin, chemical synthesis, and organoleptic properties of a
series of O-alkyl thiocarbamates.
- Gas chromatography–olfactometry in food flavour analysis
Barbara d’Acampor Zellner, Paola Dugo, Giovanni Dugo, Luigi Mondello. Journal of Chromatography A, 1186 (2008) 123–143
<< Read Abstract >>
The application of gas chromatography–olfactometry (GC–O) in food flavour analysis represents to be a valuable technique to characterise odour-active, as well as character impact compounds, responsible for the characterizing odour of a food sample. The present article briefly reviews
the use of GC–O in the flavour investigation of dairy products (milk and cheese), coffee, meat and fruits. Particular attention has been devoted to
extraction techniques, GC–O hardware commonly utilised and olfactometric assessment methods, which can be applied to food analysis.
- Influence of decomposed chemical emissions from PVC flooring on perceived air quality
Satoko Chino1, Shinsuke Kato, Janghoo Seo and Yuji Ataka1. Indoor Air 2008, August 17-23, 2008, Copenhagen, Denmark
<< Read Abstract >>
2-Ethyl-1-hexanol (2E1H) is sometimes detected indoors in relatively high concentrations
because ester compounds in building materials hydrolyze. This study addresses 2E1H
emission from flooring, and its influence on perceived air quality. Some PVC floorings are
attached on top of moisture-containing SL materials with adhesive, and it is these 2E1H
emission rates that are measured. In addition, odorous compounds from PVC floorings
attached to SL materials are identified and characterized using gas chromatography–flame
ionization detection-olfactometry (GC-FID-O). 2E1H emission rates also change, depending
on the type of flooring material. The diffusion coefficients of the chemical substances in the
material are affected by the material’s characteristics. The quantity and character of odorous
chemical compounds from building materials differs. It is considered that the perceived air
quality and emission rate are affected by the chemical reaction in the building materials and
moisture content of the floor slabs.
- Successful application of Thermal Desorption-Gas Chromatography/Olfactometry/Mass Spectrometry
(TD-GC/O/MS) technique to the identification of main odorants in complex mixtures of volatile compounds
Maurizio Benzo, Gianluca Gilardoni
<< Read Abstract >>
A GC/MS system equipped with a thermal desorber and a sniffing port has been set up
and used for identification of main odorants in complex mixtures of volatile
compounds. Emissions were sampled from the soil in a former refinery plant in
LaSpezia during remediation, and have been analyzed with TD-GC/O/MS technique;
headspace samples of the soil have been tested in the same way. Samples had a strong
disturbing odour but their chromatograms were covered by a great number of peaks of
saturated, branched and cyclic hydrocarbons.
Aromagrams allowed to individuate as main odorants (garlic-like odour) small peaks of
linear and cyclic olefins; their identification has been confirmed by peak disappearance
after oxidation of the emission bubbling through a permanganate solution.
Other trace odorants were found analyzing the water after scrubbing of the emission
through a Drechsel bottle; water was extracted using SBSE technique, and aromagram
showed very small peaks identified as cyclic thioeters (broccoli-like odour): their
presence was confirmed by peak disappearance after addition of hydrogen peroxide and
oxidation to sulfoxide.
Aromagram allowed to individuate also a few aromatic hydrocarbons (grass-like,
gasoline-like odour) as responsible of the whole odour of the emission.
- Characterization of olive paste volatiles to predict the sensory quality of virgin olive oil
Diego L. García-González, Noelia Tena, Ramón Aparicio. Eur. J. Lipid Sci. Technol. 109 (2007) 663–672
<< Read Abstract >>
One of the main challenges that virgin olive oil producers face today is an accurate
prediction of the sensory quality of the final product prior to the milling of the olives. The
possibility that olive paste aroma can be used as a predictive measurement of virgin
olive oil quality is studied in this paper. The study was centered on distinguishing the
aroma of olive pastes that produced virgin olive oils without sensory defects from the
aroma of olive pastes the virgin olive oils of which showed sensory defects. Olive
pastes were analyzed by solid-phase microextraction-gas chromatography and a
sensor system based on metal oxide sensors. Forty-four volatile compounds were
identified in olive pastes, all of them being also present in virgin olive oil. Six volatile
compounds – acetic acid, octane, methyl benzene, (E)-2-hexenal, hexyl acetate and 3-
methyl-1-butanol – distinguished both kinds of pastes with only five misclassified
samples. Five metal oxide sensors were able to classify the olive pastes with only two
erroneous classifications.
- First Identification of O,S-Diethyl Thiocarbonate in Indian Cress Absolute and Odor Evaluation of Its
Synthesized Homologues by GC-Sniffing
KATHARINA BREME, NADINE GUILLAMON, XAVIER FERNANDEZ,PASCAL TOURNAYRE, HUGUES BREVARD, DANIEL JOULAIN, JEAN LOUIS BERDAGU´ E, AND UWE J. MEIERHENRICH
J. Agric. Food Chem. 2009, 57, 2503–2507
<< Read Abstract >>
Indian cress (Tropaeolum majus L.) absolute was studied by GC-olfactometry (VIDEO-Sniff method)
in order to identify odor-active aroma compounds. Because of its fruity-sulfury odor note, a compound
that has never been identified in plant extracts before stood out: O,S-diethyl thiocarbonate, present
at 0.1% (percentage of the total GC/FID area) in the extract. GC×GC-TOFMS allowed for a clean
mass spectrum to be obtained, and isolation by preparative GC followed by NMR studies allowed its
identification. Here, we report on the first detection of O,S-diethyl thiocarbonate in Indian cress absolute
by GC-olfactometry/VIDEO-Sniff and on its isolation and identification. The synthesis and odor
evaluation of its homologues are presented.
- GC–MS, GC–O and enantio–GC investigation of the essential oil of Tarchonanthus camphoratus L.
Rosaria Costa, Barbara d’Acampora Zellner, Maria L. Crupi, Maria R. De Fina, Maria R. Valentino, Paola Dugo, Giovanni Dugo and Luigi Mondello
J. Agric. Food Chem. 2009, 57, 2503–2507
<< Read Abstract >>
The volatile fraction of Tarchonanthus camphoratus L. has been studied by means of gas chromatography–
mass spectrometry (GC–MS) and GC–FID, leading to the determination of 90 components whose major were á -pinene
(14.7 g/100 g), eucalyptol (14.8 g/100 g) and fenchyl alcohol (12.2 g/100 g). Gas chromatography–olfactometry (GC–O) has
been applied to the evaluation of the olfactive notes and their intensity. Also, the enantiomeric distribution of some
relevant constituents has been assessed by enantio-GC through the use of a chiral cyclodextrin-based stationary phase.
- Gas chromatography-olfactometry
Conor M. Delahunty, Graham Eyres, Jean-Pierre Dufour. J. Sep. Sci. 2006, 29, 2107 – 2125
<< Read Abstract >>
GC-olfactometry (GC-O) refers to the use of human assessors as a sensitive and selective
detector for odour-active compounds. The aim of this technique is to determine
the odour activity of volatile compounds in a sample extract, and assign a relative
importance to each compound. Methods can be classified into three types: detection
frequency, dilution to threshold and direct intensity. Dilution to threshold methods
measure the potency of odour-active compounds by using a series of extract dilutions,
whereas detection frequency and direct-intensity methods measure odouractive
compound intensity, or relative importance, in a single concentrated extract.
Factors that should be considered to improve the value of GC-O analysis are the
extraction method, GC instrument conditions, including the design and operation
of the odour port, methods of recording GC-O data and controlling the potential for
human assessor bias using experimental design and a trained panel. Considerable
emphasis is placed on the requirement for multidimensional GC analysis, and on
best practice when using human assessors.
- Character impact odorants from Brassicaceae by aroma extract dilution analysis (AEDA): Brassica cretica and Brassica insularis
Katharina Breme, Stéphane Langle, Xavier Fernandez, Uwe J. Meierhenrich, Hugues Brevard, Daniel Joulain Flavour Frag. J. 2009, 24, 88-93
<< Read Abstract >>
Volatile extracts of two wild cabbages, Brassica cretica and Brassica insularis, were studied by GC-MS, GC/FID, and
GC-olfactometry/aroma extract dilution analysis (GC-O/AEDA). Major compounds were 3-butenyl cyanide (70% of the total GC/FID area)
and 3-butenyl isothiocyanate (29%) in B. cretica and 2-phenylethyl cyanide (53%) and 2-phenylethyl isothiocyanate (21%) in B. insularis.
AEDA revealed the impact of five heteroatomic trace compounds (diacetyl, methional, furfuryl thiol, 1-octen-3-one and skatole)
with moderate to high flavour dilution (FD) factors that were detected only due to GC-O analyses
- Identification of Odor Impact Compounds of Tagetes minuta L. Essential Oil: Comparison of Two GC-Olfactometry Methods
Katharina Breme, Pascal Tournayre, Xavier Fernandez, Uwe J. Meierhenrich, Hugues Brevard, Daniel Joulain and Jean Louis Berdagué J. Agric. Food Chem., 2009, 57 (18), pp 8572–8580
<< Read Abstract >>
Odor impact compounds of Tagetes minuta L. essential oil were studied by gas chromatography (GC)-olfactometry using aroma extract
dilution analysis (AEDA) and vocabulary-intensity-duration of elementary odors by sniffing (VIDEO-Sniff). AEDA was conducted by
direct injection and revealed the presence of 43 odorant zones. Highest flavor dilution (FD) values were obtained for ethyl 2-methylpropanoate,
ethyl 3-methylbutanoate, (E)-ocimenone, two tentatively identified thiols, and two yet unknown compounds. VIDEO-Sniff was realized by dynamic
headspace sampling (D-HS) combined with 8W-GC-olfactometry where eight sniffers simultaneously detect volatile compounds obtained from a single
chromatographic separation and revealed the presence of 42 odorant zones. Odorant trace compounds detected by GC-O that were present in
quantities inferior to the GC-qMS system’s detection limit and those subject to coelutions were identified by GC×GC-time-of-flight mass
spectrometry (TOFMS). A total amount of 37 odorant components could be identified by VIDEO-Sniff, and the strong influence of the fruity
notes of numerous esters stood out. Highest olfactory signals were obtained for ethyl 2-methylpropanoate, ethyl 2- and 3-methylbutanoate,
and oct-1-en-3-one. Both methods hence come to the conclusion that ethyl 2-methylpropanoate and ethyl 2- and 3-methylbutanoate are among the
main odorants in Tagetes minuta L. essential oil. Differences, advantages, and drawbacks of both GC-O methods are discussed.
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