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Biomedical subjects

M P Martí

Publications and source records attributed to M P Martí.

8 recordsLinked to original sources

Fast screening method for determining 2,4,6-trichloroanisole in wines using a headspace-mass spectrometry (HS-MS) system and multivariate calibration.

The system based on coupling a headspace sampler to a mass spectrometer (HS-MS), which is considered one kind of electronic nose, is an emergent technique for ensuring and controlling quality in industry. It involves injecting the headspace of the sample into the ionization chamber of the mass spectrometer where the analytes are fragmented. The result is a complex mass spectrum for each sample analyzed. When several samples are analyzed the data matrix generated is processed with chemometric techniques to compare and classify the substances from their volatile composition, in other words, to compare and classify their flavor. So far, information from electronic nose applications has mainly been qualitative. In this paper we present a quantitative study that uses a multivariate calibration. We analyzed several white wines using HS-MS to determine 2,4,6-tricholoranisole (TCA). This is an off-flavor that is a serious problem for the wine industry. The method is simple because it does not require sample preparation, only addition of sodium chloride being necessary for sample conditioning. Also, it provides a fast screening (10 min/sample) of the quantity of TCA in wines at ultratrace (sub microg L(-1)) levels.

Anisoles↗

Determination of 4-ethylguaiacol and 4-ethylphenol in red wines using headspace-solid-phase microextraction-gas chromatography.

A method for analysing 4-ethylguaiacol and 4-ethylphenol in the aroma of red wines using headspace-solid-phase microextraction is presented. The fibres used were coated with 100 microm of polydimethylsiloxane. Parameters like ionic strength, agitation of the sample, sample volume, temperature of the sample and adsorption/desorption times were studied and optimised to obtain the best extraction results. The linearity of the response was studied in the usual concentration ranges in wines (4-ethylguaiacol, 40-400 microg/l; 4-ethylphenol, 200-1800 microg/l). Repeatability of the method was determined, and the relative standard deviation was about 10%. Limits of detection and limits of quantification were also determined, and the values found were 1 and 5 microg/l for 4-ethylguaiacol and 2 and 5 microg/l for 4-ethylphenol, respectively. All these values were under the sensory thresholds established for these volatile phenols. The presence of interferences due to the matrix composition implies the use of the standard addition technique for both compounds quantification.

Chromatography, Gas↗

Headspace solid-phase microextraction of higher fatty acid ethyl esters in white rum aroma.

Fatty acid ethyl esters are the main components of rum aroma and play an important sensorial impact in these distilled alcoholic beverages. Herein, a method for analysing these volatile compounds is described. It involves a separation and concentration step using headspace solid-phase microextraction and determination by capillary gas chromatography using flame ionisation detection. The influence of different parameters related to the isolation and concentration step, such as ethanol concentration, ionic strength, sample volume, time and temperature of extraction, was studied. The developed method enabled recoveries >91% for the analyzed compounds with limits of detection between 0.007 and 0.027 mg/l, all of them lower than the range of concentrations found in rum samples. The method was successfully applied to the analysis of fatty acid ethyl esters in different commercial white rums.

Alcoholic Beverages↗

Headspace solid-phase microextraction analysis of 3-alkyl-2-methoxypyrazines in wines.

A procedure to determine 3-alkyl-2-methoxypyrazines in wines is described. It is based on the headspace solid-phase microextraction (HS-SPME) technique after a clean-up of the sample by distillation (previously acidified to pH 0.5) to remove ethanol and other volatile compounds that can interfere in the SPME. Determination is performed by means of capillary gas chromatography using a nitrogen-phosphorus detector. The method allows quantification of 3-isobutyl-2-methoxypyrazine, 3-sec-butyl-2-methoxypyrazine and 3-isopropyl-2-methoxypyrazine at their natural concentration levels and below their sensory thresholds in Cabernet Sauvignon and Merlot wines. The method was successfully applied to experimental red wines and the evolution of their pyrazine contents during the winemaking process was monitored. Pyrazine content increased during the first maceration day but did not change significantly during alcoholic and malolactic fermentation. Final contents in wines were 12-27 ng/l of 3-isobutyl-2-methoxypyrazine and 5-10 ng/l of 3-sec-butyl-2-methoxypyrazine.

Chromatography, Gas↗

Analysis of low-volatility organic sulphur compounds in wines by solid-phase microextraction and gas chromatography.

A method for analysing low-volatility sulphur compounds using solid-phase microextraction has been developed. The analytes were extracted directly from the liquid sample using fibres coated with different stationary phases. The best extraction efficiency was obtained with Carboxen-polydimethylsiloxane coating. Ionic strength, sample volume, time and temperature of the extraction were optimised and the matrix effect studied. The method enables 15 sulphur compounds in wine to be determined at trace levels with recoveries close to 100% and limits of detection between 0.05 and 5 microg/L. The overall method was successfully applied to the determination of the sulphur compounds studied in several red, white and rosé wines.

Chromatography, Gas↗

Headspace solid-phase microextraction method for determining 3-alkyl-2-methoxypyrazines in musts by means of polydimethylsiloxane-divinylbenzene fibres.

A method for determining 2-methoxypyrazine, 3-methyl-, 3-ethyl-, 3-isopropyl-, 3-sec.-butyl- and 3-isobutyl-2-methoxypyrazine in musts is described. It involves headspace solid-phase microextraction (SPME) and determination by capillary gas chromatography using nitrogen-phosphorous detection. Pyrazines were satisfactorily separated under isothermal conditions, and quantification was carried out using 3-isopropyl-2-ethoxypyrazine as the internal standard. Ionic strength, time and temperature were studied in order to make SPME as efficient as possible. The developed method enabled detection limits at the 0.1 ng(-1) levels for some of the analytes. The method was successfully applied to identify and quantify different 3-alkyl-2-methoxypyrazines in experimental musts of Cabernet Sauvignon and Merlot. Their evolution during the ripening was also monitored.

Osmolar Concentration↗

Simultaneous analysis of thiols, sulphides and disulphides in wine aroma by headspace solid-phase microextraction-gas chromatography.

This paper deals with the improvement of a headspace solid-phase microextraction (HS-SPME) method, developed in a previous work, in order to analyse, simultaneously, thiols, sulphides and disulphides in wines. This can be achieved by applying Carboxen-polydimethylsiloxane fibres and a cryogenic trap to focus the analytes. Under optimum conditions, the HS-SPME procedure developed shows low limits of detection for the sulphides and disulphides studied (0.05-3 micrograms/l) and the thiols can also be analysed and detected at very low levels (0.5-1 microgram/l) with acceptable recoveries and repeatability.

Chromatography, Gas↗

Headspace solid-phase microextraction of sulphides and disulphides using Carboxen-polydimethylsiloxane fibers in the analysis of wine aroma.

Headspace solid-phase microextraction was applied to gas chromatography coupled to flame photometric detection to develop a method for analysing volatile sulphides and disulphides in wine. The Carboxen-polydimethylsiloxane-coated silica fiber was tested and different parameters such as presampling time, ionic strength, stirring, headspace volume, ethanol concentration, time and temperature of extraction were optimized to make extraction as efficient as possible. The optimized conditions enabled limits of detection to be obtained at the ng/l levels. The fiber tested has a strong affinity for the sulphur compounds studied and enables these analytes to be quantitatively determined in wines. The Carboxen-polydimethylsiloxane-coated fiber is more efficient at extracting than fibers such as those which are polydimethylsiloxane-coated and polyacrylate-coated, but its repeatability is worse. The overall process was successfully applied to identify and quantify sulphur compounds in white, red, rose and vintage wines.

Adsorption↗