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Ivonne Delgadillo

Publications and source records attributed to Ivonne Delgadillo.

11 recordsLinked to original sources

Headspace-solid phase microextraction-gas chromatography as a tool to define an index that establishes the retention capacity of the wine polymeric fraction towards ethyl esters.

A headspace-solid phase microextraction followed by gas chromatographic analysis (HS-SPME-GC) was developed to be applied in the study of the interactions between the wine polymeric fraction and the ethyl esters: ethyl hexanoate, ethyl octanoate, and ethyl decanoate. Wine models (WM) were prepared with 10% (v/v) aqueous ethanol at pH 3.5 with distinct wine polymeric concentrations prepared from white wine of Vitis vinifera L. var. Fernão-Pires: 1.0 g L(-1) (PWM1), with a polymeric concentration approaching the real one in wine; 10.0 g L(-1) (PWM10); and 30.0 g L(-1) (PWM30), saturated with polymeric fraction. A reference wine model (RWM) was prepared without polymeric fraction. Each volatile compound (4.0 mg L(-1)) was added separately to the RWM and to the WM with the three levels of polymeric material (PWM). From the retention index (RI) calculated for each compound using the formula: [RI = 1 - (C(RWM) - C(PWM))/C(RWM)], where C(RWM) is the concentration of the compound in the RWM and C(PWM) is the concentration of the compound in the given PWM, the retention capacity of each wine polymeric fraction towards the three esters was established. The higher retention indexes were observed for ethyl decanoate, the more hydrophobic compound, and for the PWM with higher concentration. Furthermore, this study also suggested that the retained compounds are dosed to the headspace, which may promote the perception of their aroma for a longer period of time.

Adsorption↗

Rapid tool for distinction of wines based on the global volatile signature.

This work describes a novel methodology for the rapid distinction of wines by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry, followed by principal component analysis of the data (HS-SPME-GC-MS-PCA). Headspace SPME is used to extract and concentrate the volatile and semi-volatile fractions. A DB-FFAP fused silica GC capillary column of 30 m at 220 degrees C was used acting as a transfer line of the components sorbed by the Carbowax-divinylbenzene coating fibre to the mass spectrometer, which acts as a sensor (30<m/z<300). In this methodology, which does not require any pre-treatment of the sample, the global volatile signature of the wine headspace (chromatographic profile and m/z pattern of fragmentation in each scan) is evaluated without complete chromatographic separation of its components. In order to retrieve from the data as much chemical information as possible and to extract m/z fragments (markers) for the characterisation and distinction of the wines varieties, a PCA was applied to the data resultant from the unresolved volatile fraction. In the present study, two different monovarietal white wines (Vitis vinifera L. var. Fernão-Pires and Arinto) were tested. Associated to the fast character of the proposed methodology and robustness taking into account the extraction time, it is also important to focus the higher sensibility and the lower effect of the sample moisture of the MS sensor response when compared to the conventional e-noses.

Alcohols↗

Characterization of kafirin and zein oligomers by preparative sodium dodecyl sulfate-polyacrylamide gel electrophoresis.

Quantitative and qualitative analysis of uncooked zein and kafirin fractions were performed through sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) and electrophoretic profiles. Kafirins and zeins present the same oligomer and monomer compositions with the exception of a 66 kDa oligomer that is only present in kafirins. The quantitative analysis showed differences between zein and kafirin. The composition of each oligomer was established via preparative SDS-PAGE. Part of the cooked oligomers resists reduction; the presence of those oligomers could be related to the decrease on protein digestibility with the cooking process.

Electrophoresis, Polyacrylamide Gel↗

Improving pulse sequences for 3D DOSY: COSY-IDOSY.

An improved pulse sequence for measuring diffusion-ordered COSY spectra is achieved by incorporating the diffusion encoding directly into the evolution and detection periods of a gradient-enhanced COSY sequence, giving improved sensitivity and a 32-fold reduction in minimum experiment time.

Journal Article↗

Improving pulse sequences for 3D diffusion-ordered NMR spectroscopy: 2DJ-IDOSY.

An improved pulse sequence for the 3D DOSY experiment 2DJ-DOSY, using diffusion encoding internal to the parent 2DJ spectroscopy sequence (2DJ-IDOSY), is presented. The diffusion-encoding pulses are used to enforce the desired coherence transfer pathway, reducing the minimum experimental time by at least a factor of 4, as compared to existing techniques, and approximately doubling the signal-to-noise ratio for small molecules. The new sequence is demonstrated on a simple mixture and on a complex sample with a high dynamic range (port wine). The principle of internal diffusion encoding can be applied with profit to a range of other 3D DOSY experiments.

Journal Article↗

High-resolution NMR and diffusion-ordered spectroscopy of port wine.

The use of high-resolution NMR and high-resolution diffusion-ordered spectroscopy (DOSY) for the characterization of selected Port wine samples of different ages with the aim of identifying changes in composition is described. Conventional 1D and 2D NMR methods enabled the identification of about 35 compounds, including minor components such as some medium-chain alcohols, amino acids, and organic acids. High-resolution (HR) DOSY extended sample characterization, increasing the number of compounds identified and NMR assignments made, by providing information on the relative molecular sizes of the metabolites present. Port wines of different ages were found to differ mainly in their content of (a) organic acids and some amino acids, (b) an unidentified possible disaccharide, and (c) large aromatic species. The relative amount of these last high Mw aromatics is seen to decrease significantly in the oldest wine, as expected from the known formation and precipitation of anthocyanin-based polymers during red wine aging.

Magnetic Resonance Spectroscopy↗

Sequential in vitro pepsin digestion of uncooked and cooked sorghum and maize samples.

An in vitro protein digestion study, using pepsin, was carried out in uncooked and cooked sorghum and maize flour samples. The digestibility values from the uncooked samples showed that sorghum presents digestibility values similar to those of maize. In the case of the cooked samples, it was found that a wet cooking procedure promotes a decrease in sorghum protein digestibility when compared to maize. Electrophoresis was used to follow the in vitro pepsin sequential digestion procedure, and infrared spectroscopy was applied to establish its efficiency. SDS-PAGE results showed that both uncooked samples (sorghum and maize) behave in a similar way. The wet cooking procedure increases the amount of high molecular weight aggregates and promotes the appearance of two nonreducible and nondigestible 45 and 47 kDa proteins. These two protein fractions are directly related to the loss of digestibility. It was also shown that in cooked sorghum the monomers (gamma-, alpha-, and beta-) are more resistant to digestion than the corresponding uncooked samples.

Digestion↗

Composition of phenolic compounds in a Portuguese pear (Pyrus communis L. var. S. Bartolomeu) and changes after sun-drying.

The composition of phenolic compounds of a Portuguese pear cultivar (Pyrus communis L. var. S. Bartolomeu) was determined by HPLC after thioacidolysis. The average concentration of phenolic compounds in pear harvested at commercial maturity stage was 3.7 g per kg of fresh pulp. Procyanidins were the predominant phenolics (96%), with a mean degree of polymerization (mDP) of 13-44; hydroxycinnamic acids (2%), arbutin (0.8%), and catechins (0.7%) were also present. The most abundant monomer in the procyanidin structures was (-)-epicatechin (99%), which was found as extension and terminal units; (+)-catechin (1%) was found only as a terminal unit. Sun-drying of these pears caused a decrease of 64% (on a dry pulp basis) in the total amount of native phenolic compounds. Hydroxycinnamic acids and procyanidins showed the largest decrease; the B2 procyanidin was not found at all in the sun-dried pear. Less affected were arbutin and catechins. In the sun-dried pear, the procyanidins with high mDP became unextractable in the solvents used.

Arbutin↗

Fourier transform infrared spectroscopy and chemometric analysis of white wine polysaccharide extracts.

Monovarietal white wines from Maria Gomes and Bical Portuguese Bairrada varieties were prepared according to different maceration and pectic enzyme clarification procedures. The polysaccharide-rich extracts, obtained by wine concentration, dialysis, and lyophilization, were fractionated by graded ethanol precipitation. A wide range of fractions rich in polysaccharides were obtained. Using the spectral region between 1200 and 800 cm(-)(1) of the FTIR spectra of the wine polysaccharide dry extracts, using PCA and CCA chemometric methods, it was possible to discriminate the extracts on the basis of their polysaccharide composition. Moreover, it was possible to identify the wine-making processes involved and their influence on the wine polysaccharides. Furthermore, a calibration model using a PLS1 was proposed for the quantification of mannose in the samples obtained by precipitation with 60% ethanol aqueous solutions. This information will allow an expeditious assessment and monitoring of the polysaccharide composition and modifications that occur during the wine-making processing and evolution.

Chemical Fractionation↗

Application of FTIR spectroscopy for the quantification of sugars in mango juice as a function of ripening.

FTIR-ATR spectroscopy and multivariate analysis were used for quantification of sugars in mango juices as a function of ripening. Calibration was based on sucrose/glucose/fructose mixtures, with six concentration levels and following a triangular experimental design. PLS1 regression of the spectra first derivatives gave the best results, enabling quantification of fructose, sucrose, and glucose with 1.4, 1.4, and 4.9% prediction errors, respectively. Throughout ripening, sucrose and fructose were accurately quantified by PLS-FTIR, whereas the accuracy of glucose determination decreased at later stages, when concentrations fell to 0.6-1.5 g/L. These results enabled a correlation with fruit ripening stage to be established. This may be particularly useful to detect over-ripening in fresh fruits, a period when other indicators (pH and % soluble solids (SS)) do not change significantly; this knowledge may help in predicting fruit stability to transport and storage. Similar information obtained for nonfresh juices (in which pH and %SS may be masked by additives), may help determine whether the source fruits had suitable ripening stages.

Beverages↗

Effect of gelatinization and starch-emulsifier interactions on aroma release from starch-rich model systems.

Release of selected volatile aldehyde compounds from starch-rich matrices was studied by headspace extraction, using solid-phase microextraction, and gas chromatography. Changes in the rheological properties of the starch-based matrices, due to starch concentration, gelatinization, and interactions with emulsifiers, were studied by steady shear and dynamic methods. The degree of volatile retention was found to depend on the compound properties, starch concentration, native structure of the granules, and presence of emulsifiers. The nongelatinized starch granules were more effective in lowering the volatile headspace quantities. Loss of the native structural integrity of the granules decreases the retention ability. For the nongelatinized starch dispersions, the more hydrophilic emulsifier showed a more pronounced effect on the matrix rheology and also on the aroma retention. A different behavior was observed for the gelatinized systems. Interpretation of the volatile release profiles was made on the basis of the matrix physical properties and interactions among components.

Chromatography, Gas↗