Biomedical subjects

Vicente Ferreira

Publications and source records attributed to Vicente Ferreira.

At least 19 recordsLinked to original sources

PubMed2006

Optimization of a procedure for the selective isolation of some powerful aroma thiols. Development and validation of a quantitative method for their determination in wine.

This paper deals with the isolation properties of four relevant wine mercaptans in two different separation systems and with the subsequent development, optimization and validation of an analytical procedure for their quantitative determination. 4-Methyl-4-mercaptopentanone (4M4MP), 2-furanmethanethiol (FFT), 3-mercaptohexanol (3MH) and 3-mercaptohexyl acetate (AMH) can be quantitatively extracted from 200 ml of wine in a bed packed with 1 g of LiChrolut EN resins. Fatty acids and diverse interfering compounds are removed by rinsing with an aqueous solution with a 40% of methanol and buffered at pH 7.2 with alpha,alpha,alpha-tris-(hydroxymethyl)-aminomethane (TRIS) 0.2 M. Mercaptans can be further isolated by extraction with an aqueous solution of 1 mM p-hydroxymercury benzoate. Best results were achieved with an extraction with a solution at pH 10.7 with 0.2 M 4-(2-hydroxyethyl)piperazine-1-ethanesulfonic acid (HEPES), further acidification to pH 7.5, release of thiols by the addition of dithioerythritol and extraction with 2 x 0.75 ml dichloromethane. The extract is concentrated to 200 and 20 microl are finally injected in a gas chromatograph-ion trap mass spectrometric system. Method detection limits are 0.8, 6, 15 and 5 ng l(-1) for 4M4MP, FFT, MH and AMH, respectively. The recovery in the sample pre-treatment was 76, 45, 75 and 95%, respectively. Repeatability and linearity are also satisfactory. Different critical aspects, such as the effect of air or the evaporation of the extract were also studied.

Gas Chromatography-Mass Spectrometry↗

PubMed2006

Quantitative determination of wine highly volatile sulfur compounds by using automated headspace solid-phase microextraction and gas chromatography-pulsed flame photometric detection. Critical study and optimization of a new procedure.

The quantitative determination of wine volatile sulfur compounds by automated headspace solid-phase microextraction (HS-SPME) with a carboxen-polydimethylsiloxane (CAR-PDMS) fiber and subsequent gas chromatography-pulsed flame photometric detection (GC-PFPD) has been evaluated. The direct extraction of the sulfur compounds in 5 ml of wine has been found to suffer from matrix effects and short linear ranges, problems which could not be solved by the use of different internal standards or by multiple headspace SPME. These problems were attributed to saturation of the fiber and to competitive effects between analytes, internal standards and other wine volatiles. Another problem was the oxidation of analytes during the procedure. The reduction in sample volume by a factor 50 (0.1 ml diluted with water or brine) brought about a reduction in the amount of sulfur compounds taken in the fiber by a factor just 3.3. Consequently, a new procedure has been proposed. In a sealed vial containing 4.9 ml of saturated NaCl brine, the air is thoroughly displaced with nitrogen, and the wine (0.1 ml) and the internal standards (0.02 ml) are further introduced with a syringe through the vial septum. This sample is extracted at 35 degrees C for 20 min. This procedure makes a satisfactory determination possible of hydrogen sulfide, methanethiol, ethanethiol, dimethyl sulfide, diethyl sulfide and dimethyl disulfide. The linear dynamic ranges cover the normal ranges of occurrence of these analytes in wine with typical r2 between 0.9823 and 0.9980. Reproducibility in real samples ranges from 10 to 20% and repeatability is better than 10% in most cases. The method accuracy is satisfactory, with errors below 20% for hydrogen sulfide and mostly below 10% for the other compounds. The proposed method has been applied to the analysis of 34 Spanish wines.

Automation↗

PubMed2006

Solid phase extraction, multidimensional gas chromatography mass spectrometry determination of four novel aroma powerful ethyl esters. Assessment of their occurrence and importance in wine and other alcoholic beverages.

A method for the quantitative determination of four powerful aromatic ethyl esters recently identified in some wines has been developed, validated and applied to the determination of these compounds in different samples of wine, whisky and brandy. Ethyl 2-, 3-, and 4-methylpentanoate and ethyl cyclohexanoate are extracted from 100ml of sample by solid phase extraction (SPE) on a 200mg LiChrolut EN bed. Major compounds are eliminated by rinsing with a water-methanol (50:50) solution containing 1% sodium bicarbonate, and analytes are eluted with 1.5ml of dichloromethane. Fifty microlitres of this extract are then injected in a multidimensional gas chromatography-mass spectromety (GC-GC-MS) system. Recoveries in the SPE are quantitative. Method repeatability is satisfactory (5-12% for a 5-10ngl(-1) level, and less than 7% for 25-50ngl(-1) level), the method linearity holds along the whole range of occurrence of analytes (2-2700ngl(-1)), and the signal is independent on the matrix. Method detection limits are below 1ngl(-1) in all cases. Results suggest that these compounds are formed by the slow esterification with ethanol of the corresponding acids formed by different microorganisms. The levels of these compounds are above the corresponding thresholds in most samples of aged wines or distillates, but are particularly high in some sweet wines, whiskeys and brandies where they may constitute the most important contributors to the sweet-fruity notes reaching concentrations up to 85-350 times higher than the corresponding odor thresholds.

Alcoholic Beverages↗

PubMed2006

Use of new generation poly(styrene-divinylbenzene) resins for gas-phase trapping-thermal desorption. Application to the retention of seven volatile organic compounds.

Two new generation polymeric resins, Bond Elut ENV (styrene-divinylbenzene) from Varian and LiChrolut EN (ethylvinylbenzene-divinylbenzene) from Merck, commonly used in liquid--solid-phase extraction (SPE) were evaluated as sorbents for gas-phase sampling followed by thermal desorption and compared to Tenax TA, a reference sorbent in this kind of applications. The three resins were tested against seven volatile organic compounds (VOCs): 1-octene, ethylbenzene, (p-, m-, o-)xylenes, styrene and 1,4-dichlorobenzene. Elution curves for all compounds were determined at temperatures from 120 to 180 degrees C, and from such curves, different parameters, such as retention factor (k), distribution coefficient (K), height equivalent to a theoretical plate (H), asymmetry factor (Fa) and breakthrough volume (VB) were calculated and extrapolated at room (25 degrees C) and desorption (220 degrees C) temperatures in order to estimate breakthrough and elution volumes. In average, retention in LiChrolut EN is 10 and 200 times stronger than in Bond Elut ENV and Tenax TA, respectively, but its chromatographic behavior is rather poor giving quite asymmetric elution profiles (Fa >1.8 at 120 degrees C). Bond Elut ENV exhibited the best chromatographic behavior, with H values two or five times lower than those of LiChrolut EN or Tenax TA. An additional advantage of the new sorbents is that retention decreases with T much faster than it does in Tenax (8 or 20 times for Bond Elut ENV or LiChrolut EN). Modeling has finally shown that beds with 60-80 (for Bond Elut ENV) or 300-400 (for LiChrolut EN) times less of sorbent have the same retention properties than standard Tenax TA tubes and similar (LiChrolut EN) or five to six times smaller (Bond Elut ENV) elution volumes. These predictions have been experimentally confirmed.

Organic Chemicals↗

PubMed2006

Determination of the biogenic amines in musts and wines before and after malolactic fermentation using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate as the derivatizing agent.

An accurate, rapid and sensitive high-performance liquid chromatographic (HPLC) method is reported for the determination of four biogenic amines in red and white wine samples. The method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) followed by liquid chromatography gradient elution analysis without any other sample pretreatment. The procedure developed permitted the determination of the four amines in 40 min. The relative standard deviation (RSD) values ranged from 3.1% to 6.1% in peak areas and the response was linear (R2>0.994) in a range from 0.1 to 4 mg/l. Leaving aside putrescine in Tempranillo wines, the malolactic fermentation did not exert any effect on the concentration of these compounds. On the contrary, the influence of the grape variety was important, and Tempranillo wines showed higher levels of tyramine and histamine and lesser of putrescine and cadaverine (p<0.05) than wines made with Cabernet Sauvignon.

Aminoquinolines↗

PubMed2006

Critical aspects of the determination of pentafluorobenzyl derivatives of aldehydes by gas chromatography with electron-capture or mass spectrometric detection: Validation of an optimized strategy for the determination of oxygen-related odor-active aldehydes in wine.

This work presents a thorough study of some aspects critical to the quantitative performance of methods for the determination of volatile aldehydes previously derivatized to pentafluorobenzyl hydroxylamine oximes. The conclusions of the study are further applied to the validation of an optimized procedure for the determination of oxidation-related aldehydes from wine. Aspects studied include the chromatographic injection, the analytical performance of electron-capture detection (ECD) or MS detection, and the way in which the derivatization is carried out. Different injection techniques have been optimized and compared (classical splitless-hot injection; cold splitless; and large volume solvent split injection). All of them were carried out in a programmed temperature vaporization (PTV) injector, with a 350 microL internal volume liner (3.4 mm internal diameter). Classical splitless injection of hexane extracts is troublesome and requires large carrier gas flows (>10 mL min(-1)). Cold splitless injection was clearly superior. Large volume solvent split injection has been also optimized. ECD has been found to lack the necessary selectivity for the determination of unsaturated aldehydes in wine, although the quantitation of several minor aldehydes is possible. MS detection has proven to be superior for the determination of these compounds in wine. The way in which the reagent is applied is also critical and for the case of wine is important to ensure that the reagent is applied after some of the major wine aldehydes have been eliminated. The finally proposed method is extremely sensitive. Method detection limits ranged from 0.002 microg L(-1) (for unsaturated aldehydes) to 0.73 microg L(-1) (for phenylacetaldehyde) and precision (measured as relative standard deviation) is < or =6% in all cases. The method makes it possible to determine quantitatively in a single run the wine aldehydes with sensory significance (isobutyraldehyde, 2-methylbutanal, isovaleraldehyde, (E)-2-hexenal, (E)-2-heptenal, (E)-2-octenal, (E)-2-nonenal, methional and phenylacetaldehyde).

Aldehydes↗

PubMed2006

Identification of three novel compounds in wine by means of a laboratory-constructed multidimensional gas chromatographic system.

A laboratory-made off-line multidimensional GC-GC system has been optimized and applied to the isolation and identification of three novel aroma compounds in wine. The system comprises two independent chromatographs equipped with four-port manually actuated valves and fast capillary connectors that make it possible to quickly transfer a capillary trapping loop from the first to the second system. The first system includes a split/splitless injector, a thick phase semi-capillary column, the valve and both a flame ionization detection (FID) system and a sniffing port. The trapping loop lies outside the chromatograph and it is immersed in a Dewar with liquid nitrogen. The second system includes a programmable temperature vaporization (PTV) injector, the valve, the analytical column and two parallel detectors (a MS system and a sniffing port). The injection of large sample volumes (90 microl) in the first GC system and the general operation of the system have been optimized. The extract was obtained by purging the wine at 37 degrees C with a stream of nitrogen and trapping the volatiles in a bed containing 1g LiChrolut EN. Fatty acids and alcohols were removed by washing the resins with a water/methanol solution containing 1% NaHCO3, and volatiles were recovered with dichloromethane. The GC-MS analysis of the cuts obtained in the first GC system made it possible to identify by first time in wine the strong smelling compounds ethyl 2-, 3- and 4-methylpentanoate.

Chromatography, Gas↗

PubMed2006

Automated analysis of 2-methyl-3-furanthiol and 3-mercaptohexyl acetate at ng L(-1) level by headspace solid-phase microextracion with on-fibre derivatisation and gas chromatography-negative chemical ionization mass spectrometric determination.

A fast and automated method for the analysis at ng L(-1) level of aroma-powerful polyfunctional thiols has been developed and applied to wine. The sample is just poured in a 20 mL vial and its vapour extracted with a poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) solid-phase microextraction fibre (65 microm thickness) previously exposed to vapours of the reactive (pentafluorobenzyl bromide) and of an alkali (tributylamine). The derivatised compounds are subsequently desorbed in the GC system and determined by negative chemical ionization mass spectrometry. The method is fully automated by using a Combi-Pal autosampler conveniently programmed. The analysis takes 50 min, which contrasts to the long and tedious methods previously proposed. The development of an optimal procedure is constrained by the aggressive character of the reagent (towards the fibre and the chromatographic column), its volatility and the quality of the blanks that can be obtained. Therefore, a critical step was fixing in the fibre a "safe" and repetitive amount of reagent. This was achieved by exposing the fibre (5 min) to the vapours of a water:acetone (9:1) solution containing 200mg L(-1) of reagent. Under these conditions, the extraction-derivatisation of analytes improves with time and temperature, and the best working conditions are dictated by a compromise between sensitivity, speed and chromatographic performance. Although analytes studied were 2-methyl-3-furanthiol, 4-mercapto-4-methyl-2-pentanone, 3-mercaptohexanol, 2-furanmethanethiol and 3-mercaptohexyl acetate, a good analytical performance could be achieved only for these two last compounds. Both of them can be repetitively (10%<RSD<20%) determined in wine at concentrations below 0.1 ng L(-1). Other aspects considered in the method setup were the oxidation of analytes during the process, and the electron-capture detection (ECD) and MS properties of the pentafluorobenzyl derivatives of different polyfunctional thiols.

Acetates↗

PubMed2006

Physicochemical model to interpret the kinetics of aroma extraction during wine aging in wood. Model limitations suggest the necessary existence of biochemical processes.

A model based on physicochemical parameters has been developed and applied to the study of the kinetics of extraction of aroma compounds from oak casks having been used a variable number of times. Two major deviations from the model can be observed: a strong seasonal dependence of extraction (unexpected in a thermostated cellar); and higher yields with a smaller number of longer extractions. 4-Propylguaiacol follows both behaviors, and its levels have been found to be closely related to those of 4-ethylguaiacol and to the number of uses of the barrel, which suggests that this compound may be formed by the same microorganisms forming ethylphenols from a precursor found in wood. Although the extraction kinetics of all aroma compounds appear to be more or less mediated by the action of microorganisms, those of whiskeylactones, eugenol, and 4-allyl-2,6-dimethoxyphenol are more in accordance with the physicochemical model, whereas those of vanillin, syringaldehyde, furfuryl alcohol, and, of course, 4-propylguaiacol are much more coherent with a microbiological extraction/formation.

Chemical Phenomena↗

PubMed2006

Optimization and evaluation of a procedure for the gas chromatographic-mass spectrometric analysis of the aromas generated by fast acid hydrolysis of flavor precursors extracted from grapes.

A procedure has been developed for the GC-MS analysis of the aromas released in fast acid hydrolysis of precursor fractions from grape musts and skins. Different sorbents for the extraction of the precursors were compared. The best results were obtained with LiChrolut EN polymeric resins which displayed two and six-fold more extraction capacity than Amberlite XAD-2 resins and C18 sorbents, respectively. C18 sorbents are more suitable for selective extraction of less polar precursors. The initial version of the method was imprecise and so the imprecision of the different steps was assessed. The maceration of the solid parts and the liquid-liquid extraction of the aromas released in the acid hydrolysis proved to be the critical steps. Greater crushing of the solid parts and solid-phase extraction (SPE) instead of liquid-liquid extraction (LLE) improved reproducibility. In the method finally proposed about 100 aromatic components belonging to four large groups (lipid derivatives, shikimic acid derivatives, norisoprenoids and terpenes) were determined with good reproducibility. Important aroma compounds, such as cis-rose oxide or wine lactone were detected in non-Muscat grapes.

Acids↗

PubMed2006

Sensory and chemical characterization of the aroma of a white wine made with Devín grapes.

The aroma profile of a Slovak white wine made with Devín grapes was evaluated by 13 expert judges. The panel evaluated the orthonasal and retronasal aroma profiles, as well as the profile of residual wine aroma found in the empty glass after the consumption. For the majority of attributes, the orthonasal perception was the most intense, followed by retronasal, and finally by the residual odor. Varietal wine Devín possessed primarily a "Muscat" odor by nose, together with intense fruity, sweet, and herbaceous notes. Data were analyzed by generalized procrustes analysis. Two primary clusters separated orthonasal ratings from both retronasal and residual odor ratings. Similar results were obtained by analysis of variance. The relative proportion of "heavy" aroma notes, likely related to polar odorants, increased in retronasal and residual odor profiles. The gas chromatography-olfactometry profile revealed a great complexity and showed that the characteristic aroma of this variety seems to be a mixture of Muscat, Gewürztraminer, and Sauvignon-Blanc, being rich in linalool, cis-rose oxide, and 4-methyl-4-mercaptopentanone.

Chromatography, Gas↗

PubMed2006

Intensity and persistence profiles of flavor compounds in synthetic solutions. Simple model for explaining the intensity and persistence of their aftersmell.

Hydroalcoholic solutions containing a single aroma-active compound were evaluated by a sensory panel to determine the difference between ortho and retronasal odor intensities (DeltaI(ro)), buccal savoring, and aftersmell duration. Eight compounds were used. Buccal perception seems to be just a physiologically restricted form of retronasal perception. DeltaI(ro) values were dependent on the panel, although results from the two panels were significantly correlated. Such differences and the aftersmell persistence were also significantly correlated with different physicochemical parameters related to volatility. A simple model to explain such dependence is proposed. The model considers the mouth-throat system as a perfect mixing tank with a finite amount of odorants being progressively diluted by swallowing and purging (both taken as continuous processes). Retronasal intensity is modeled from the odor properties of the liquid in such a tank calculated from orthonasal odor intensity versus concentration (I/log C) curves. The model explains successfully experimental results and has also been successfully applied to instrumental data from other authors.

Alcohols↗

PubMed2005

Prediction of the wine sensory properties related to grape variety from dynamic-headspace gas chromatography-olfactometry data.

Wine extracts obtained by a dynamic headspace sampling technique were studied by quantitative gas chromatography-olfactometry (GC-O) to determine the aroma profiles of six young monovarietal Spanish white wines. A partial least-square regression study was carried out to look for models relating wine aroma properties with GC-O scores. Models were validated by sensory analysis. Four out of the five most important sensory descriptors were satisfactorily described by a model, and sensory tests confirmed most of the predictions. The main aroma differences between these wines are due to the ratio linalool/3-mercaptohexyl acetate. Floral, sweet, and muscat are positively related to the concentration of linalool and negatively to that of 3-mercaptohexyl acetate. Tropical fruit is related to the wine content in this last odorant. 2-Phenyl acetate, reinforced by other acetates, can also contribute to floral and sweet notes. Alkyl-methoxypyrazines lessen the tropical fruit note, and acetic acid lessens the muscat nuance.

Acyclic Monoterpenes↗

PubMed2005

Concurrent phenomena contributing to the formation of the aroma of wine during aging in oak wood: an analytical study.

Red wine was stored in different oak barrels or in stainless steel, and samples were taken for two years to determine 79 aroma compounds. Aging in oak affects 41 compounds. The type of wood affects 11 compounds. At least seven different processes seem to take place concurrently in aroma evolution, and five such processes, affecting 37 compounds, are linked to the oak cask. These are extraction from the wood, oxidation of wine alcohols and amino acids, microbiological formation of ethyl phenols, sorption processes, and condensation of acetaldehyde with polyphenols. The wood can release linear gamma- and delta-lactones, beta-damascenone, and ionones. Some compounds are released very fast from wood, which suggests they lie in the external part of the wood. Some extraction profiles are too complex to be explained by physical processes. Finally, the levels of 2,5-dimethyl-4-hydroxy-3(2H)-furanone and 2-ethyl-5-methyl-4-hydroxy-3(2H)-furanone increase even in the reference wine, which suggests the presence of a precursor.

Food Handling↗

PubMed2004

Gas chromatography-olfactometry and chemical quantitative study of the aroma of six premium quality spanish aged red wines.

The aroma of six premium quality Spanish red wines has been studied by quantitative gas chromatography-olfactometry (GC-O) and techniques of quantitative chemical analysis. The GC-O study revealed the presence of 85 aromatic notes in which 78 odorants were identified, two of which-1-nonen-3-one (temptatively) and 2-acetylpyrazine-are reported in wine for the first time. Forty out of the 82 quantified odorants may be present at concentrations above their odor threshold. The components with the greatest capacity to introduce differences between these wines are ethyl phenols produced by Brettanomyces yeasts (4-ethylphenol, 4-ethyl-2-methoxyphenol, and 4-propyl-2-methoxyphenol), 2,5-dimethyl-4-hydroxy-3(2H)-furanone (furaneol), (Z)-3-hexenol, thiols derived from cysteinic precursors (4-methyl-4-mercaptopentan-2-one, 3-mercaptohexyl acetate, and 3-mercaptohexanol), some components yielded by the wood [(E)-isoeugenol, 4-allyl-2-methoxyphenol, vanillin, 2-methoxyphenol (guaiacol), and (Z)-whiskylactone], and compounds related to the metabolism (2-phenylethanol, ethyl esters of isoacids, 3-methylbutyl acetate) or oxidative degradation of amino acids [phenylacetaldehyde and 4,5-dimethyl-3-hydroxy-2(5H)-furanone (sotolon)]. The correlation between the olfactometric intensities and the quantitative data is, in general, satisfactory if olfactometric differences between the samples are high. However, GC-O fails in detecting quantitative differences in those cases in which the olfactive intensity is very high or if odors elute in areas in which the odor chromatogram is too complex.

Chromatography, Gas↗

PubMed2004

Determination of important odor-active aldehydes of wine through gas chromatography-mass spectrometry of their O-(2,3,4,5,6-pentafluorobenzyl)oximes formed directly in the solid phase extraction cartridge used for selective isolation.

A method for the quantitative determination of octanal, nonanal, decanal, (E)-2-nonenal and (E, Z)-2,6-nonadienal in wine has been developed. In the proposed method, 200 ml of wine percolate through a solid phase extraction (SPE) cartridge packed with 200 mg of LiChrolut EN resins. The interferences are eluted with 60 ml of an aqueous solution containing 40% of methanol and 1% of NaHCO3. In the same SPE cartridge, the corresponding O-(2,3,4,5,6-pentafluorobenzyl)oximes are formed by letting percolate 2 ml of the reagent solution (5 mg ml(-1)). At room temperature the derivatization goes to completion in 15 min. The derivatives are eluted with 2 ml of dichloromethane, and the extract is concentrated and then analyzed by gas chromatography-mass spectrometry (GC-MS). The percentage of recovery in the isolation process is better than 90% in all cases with the exception of octanal, and is independent of the wine studied. In the cases of octanal, nonanal and decanal, the detection limits of the method are determined by the contamination levels of the reagent itself, and vary between 160 and 380 ng l(-1). For (E)-2-nonenal and (E, Z)-2,6-nonadienal, the detection limits were 12 and 20 and ng l(-1), respectively. The linearity of the method upheld until 10 microg l(-1) and was satisfactory in all cases. The reproducibility of the method is independent of the concentration and ranges from 30 to 190 ng (l(-1). The method has been applied to the analysis of these components in several wine samples. With the exception of (E, Z)-2,6-nonadienal, all the components can reach concentrations above their corresponding odor threshold values.

Aldehydes↗

PubMed2004

Simple strategy for the optimization of solid-phase extraction procedures through the use of solid-liquid distribution coefficients application to the determination of aliphatic lactones in wine.

A practical strategy for the optimization of solid-phase extraction (SPE) systems is presented. Critical SPE volumes (sample loaded, rinsing and elution solvent) are calculated from solid-liquid extraction coefficients and from basic bed parameters determined in simple experiments, using the Lövkist Jonsson model and other expressions derived from the general theory of chromatography. The agreement between calculated and measured volumes is satisfactory, which makes it possible to consider different sorbents and rinsing and elution solvents in the SPE optimization with a relatively low experimental effort. The strategy has been successfully applied to the optimization of a SPE method directed to the selective extraction of aliphatic lactones from wine. Six different reversed-phase sorbents were studied and the one showing maximum extraction selectivity was selected. Wine (50 ml) is extracted in a 200 mg cartridge filled with Bond Elut-ENV resins. Interferences are removed with 20 ml of methanol-water (40:60) with 1% NaHCO3. Elution is carried out with 1.8 ml of dichloromethane. The extract is concentrated to 0.15 ml and analyzed by GC-ion trap MS. Eight odor-active aliphatic gamma and delta lactones (with 8-12 C atoms) from wine are recovered (R > 75%) in an extract free from wine major volatiles. Detection limits are in the 40-300 ng/l range, well below the odor detection threshold of these compounds. Linearity (r2 > 0.996) and precision (average R.S.D. 3.5%) are satisfactory in all cases. The levels in wine of some of these lactones (gamma-octa, undeca and dodecalactones) are reported by first time and results demonstrate that can be present at concentrations above or close to their corresponding odor thresholds.

Chromatography, Liquid↗

PubMed2003

Fast fractionation of complex organic extracts by normal-phase chromatography on a solid-phase extraction polymeric sorbent. Optimization of a method to fractionate wine flavor extracts.

Some properties of LiChrolut-EN resins as normal-phase sorbent have been studied. Retention factors using pentane as solvent range from less than 2 (ethyl esters) to more than 56 (fatty acids and vanillin). All retention factors were smaller than 2 with dichloromethane. The efficiency of the bed was between 4 and 13 plates per cm. A method for the fast fractionation of wine flavor extracts has been further developed. Wine (75 ml) is extracted on a 0.5 g LiChrolut-EN bed. Volatile compounds are recovered in 5 ml of dichloromethane and the extract is further concentrated to 0.1 ml. Recoveries of the extraction procedure are above 85% for all compounds less polar than isoamyl alcohol. This extract is fractionated on a bed (5.0 cm height, 0.6 cm internal diameter) packed with 0.55 g of LiChrolut-EN resins. A first fraction is collected by the elution with 4 ml of pentane. A second one with 6 ml of a mixture pentane/dichloromethane (9:1) and a final fraction with 4 ml of dichloromethane. The first fraction is enriched in ethyl esters and some other non-polar compounds. The second fraction concentrates the alcohols and some volatile phenols, while the third is enriched in fatty acids, vanillin derivatives and some lactones. The recovery in the fractionation is complete. The profile obtained in the fractionation is very stable, and becomes distorted only when the column is loaded with an extract containing 80 mg of major volatiles (coming from more than 150 ml of wine). The fractionation of extracts from different wines showed that the performance of the process does not depend on the composition of the extract. Twenty-seven out of 32 studied compounds eluted reproducibly mainly in one fraction. The results suggest that the method can be applied as an aid for qualitative or quantitative analysis to any kind of organic extract as an alternative to liquid chromatography on silica-gel.

Chromatography, Liquid↗