Extraction and characterization of low molecular weight bioactive carbohydrates from mung bean (Vigna radiata).

Due to the great interest in obtaining natural bioactive carbohydrates to be used as functional ingredients, a selective microwave assisted extraction (MAE) method was optimized to ensure the exhaustive extraction of inositols and α-galactooligosaccharides (α-GOS) from mung bean. Thereafter, a comprehensive characterization of these compounds was carried out by gas chromatography coupled to mass spectrometry (GC-MS). Apart from free inositols and α-GOS, several glycosyl-methyl-scyllo-inositols and glycosyl-inositols were detected for the first time in this legume.

Gas chromatographic-based techniques for the characterization of low molecular weight carbohydrates and phenylalkanoid glycosides of Sedum roseum root supplements.

An extensive characterization of low molecular weight carbohydrates (LMWC) and phenylalkanoid glycosides (PAG) of Sedum roseum root supplements has been carried out for the first time by gas chromatography coupled to mass spectrometry (GC-MS) and by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-ToF MS). Optimization of the required derivatization procedure for improved determination of PAG showed the combined use of trimethylsilylimidazole and trimethylchlorosilane as the most appropriate reagents. Up to 37 compounds were qualitative- and quantitatively characterized in different dietary supplements of S.

Characterization of cyclitol glycosides by gas chromatography coupled to mass spectrometry.

Several cyclitol glycosides have been characterised as trimethylsilyl derivatives by their gas chromatographic (GC) retention data (linear retention indices) and electron impact mass spectrometric (MS) profiles. Both GC-MS results have been related to cyclitol glycosides structural features. Abundance ratios of characteristic m/z ions 133/129 and 260/265 have been proposed to distinguish glycosyl-inositols from glycosyl-methyl-inositols.

Identification and determination of 3-deoxyglucosone and glucosone in carbohydrate-rich foods.

Background: α-Dicarbonyl compounds (α-DCs) such as 3-deoxyglucosone (3-DG) and glucosone are markers of both Maillard and degradation reactions of sugars and also of certain enzymatic processes. However, quantitation of these compounds is not straightforward when more abundant carbohydrates are present in real samples. Therefore in this work a GC/MS method was developed to separate monosaccharides, 3-DG and glucosone and applied to analyze them in carbohydrate-rich food products.

Statistical analysis for improving data precision in the SPME GC-MS analysis of blackberry (Rubus ulmifolius Schott) volatiles.

Statistical analysis has been used for the first time to evaluate the dispersion of quantitative data in the solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis of blackberry (Rubus ulmifolius Schott) volatiles with the aim of improving their precision. Experimental and randomly simulated data were compared using different statistical parameters (correlation coefficients, Principal Component Analysis loadings and eigenvalues). Non-random factors were shown to significantly contribute to total dispersion; groups of volatile compounds could be associated with these factors.

Development of a carbohydrate silylation method in ionic liquids for their gas chromatographic analysis.

This paper reports on the feasibility of silylation of low molecular weight carbohydrates dissolved in different ionic liquids (ILs) for their further analysis by gas chromatography (GC). Derivatization reagents (nature and amounts), temperature and time of reaction and stirring conditions were evaluated for different carbohydrates (i.e.

Low molecular weight carbohydrates in pine nuts from Pinus pinea L.

Low molecular weight carbohydrates in pine nuts from Pinus pinea L. (n = 7) have been studied by gas chromatography-mass spectrometry as their trimethylsilyl oximes. Besides previously reported components, such as glucose, fructose, sucrose, and raffinose, several soluble carbohydrates have been identified for the first time in this product, including saccharides (galactose, maltose, and planteose) and cyclitols (pinitol, galactinol, galactopinitol A1, fagopyritol B1, and other glycosyl-inositols).

Determination of free inositols and other low molecular weight carbohydrates in vegetables.

Different low molecular weight carbohydrates including saccharides, polyalcohols, sugar acids, and glycosides have been identified and quantified in different edible vegetables from Asteraceae, Amarantaceae, Amarylidaceae, Brassicaceae, Dioscoreaceae, and Solanaceae families by gas chromatography-mass spectrometry. Apart from glucose, fructose, and sucrose, other saccharides such as sedoheptulose in chicory, spinach, cabbage, purple yam, eggplant, radish, and oak leaf lettuce, rutinose in eggplant skin, and a glycosyl-inositol in spinach have been identified. chiro-Inositol was found in all vegetables of the Asteraceae family (3.

Derivatization of carbohydrates for GC and GC-MS analyses.

GC and GC-MS are excellent techniques for the analysis of carbohydrates; nevertheless the preparation of adequate derivatives is necessary. The different functional groups that can be found and the diversity of samples require specific methods. This review aims to collect the most important methodologies currently used, either published as new procedures or as new applications, for the analysis of carbohydrates.

Analysis of cyclitols in different Quercus species by gas chromatography-mass spectrometry.

Background: The carbohydrate profile of some woods used for aging wines and spirits has been recently studied using a pressurized liquid extraction method, the main differences found being related to cyclitol content. The aim of this study was to perform a detailed study of these compounds in woods of different Quercus species in order to identify two unknown compounds which appeared in the extracts and to verify whether the obtained profile was homogeneous for other Quercus species.

Results: Besides the known monosaccharides and five cyclitols previously described, three deoxy-inositols (epi-, vibo- and scyllo-quercitol) were identified.

Identification of free disaccharides and other glycosides in wine.

Free soluble carbohydrates of different wine samples were analyzed by GC-MS as their trimethylsilyloximes using a methylsilicone column. Besides alpha,alpha-trehalose, several beta-glucosylglucoses such as cellobiose, sophorose, laminaribiose and gentiobiose were the main disaccharides identified. With the exception of gentiobiose, these disaccharides are now reported for the first time in wine.

Characterization of O-trimethylsilyl oximes of trisaccharides by gas chromatography-mass spectrometry.

Gas chromatography (GC) data (linear retention indices and relative areas) and mass spectra (most representative m/z fragments) of 12 reducing trisaccharides as trimethylsilyl oximes (TMSO) and four non-reducing as trimethylsilyl (TMS) ethers have been described for the first time and related to their structural features. Some trends have been observed: earlier elution of non-reducing compounds and fructotrioses; aldotrioses bearing the reducing end with link in position 6 showing the highest retention. Abundance of several fragment ions and their ratios were useful for trisaccharide characterization; some of these features seem to be useful for the characterization of new trisaccharides.

Study of the precision in the purge-and-trap-gas chromatography-mass spectrometry analysis of volatile compounds in honey.

Data precision in the analysis by purge-and-trap coupled on-line to gas chromatography-mass spectrometry (P&T-GC-MS) of honey volatiles has been studied by statistical analysis. The contribution of non-random factors to dispersion of quantitative results was proven by comparing several statistical parameters (correlation coefficients, principal component analysis (PCA) eigenvalues and loadings) from both experimental and simulated data. PCA was also useful for grouping volatiles with similar dispersion behaviour; these groups being generally related to compounds with common properties or structural features.

Fractionation of honey carbohydrates using pressurized liquid extraction with activated charcoal.

This article describes the development of a new procedure that combines the use of activated charcoal and pressurized liquid extraction (PLE) to obtain enriched fractions of di- and trisaccharides from honey. Honey was adsorbed onto activated charcoal and packed into a PLE extraction cell. Optimum results were obtained at 10 MPa and 40 degrees C using two consecutive PLE cycles: first, 1:99 (v/v) ethanol/water for 5 min and second, 50:50 (v/v) ethanol/water for 10 min.

Short communication: Identification of the aroma compounds responsible for the floral/rose flavor in water-soluble fractions of Manchego cheese.

Water-soluble fractions from Protected Denomination of Origin Manchego cheese, with molecular weight <1,000 Da, were fractionated using gel permeation chromatography and studied using both instrumental and sensorial analysis. In 2 of the fractions, panelists detected a floral, rose-like flavor. Analysis of these fractions by gas chromatography-mass spectrometry after simultaneous distillation extraction with dichloromethane identified 2-phenylethanol and phenylacetaldehyde as the compounds responsible for this flavor.

A new methodology based on GC-MS to detect honey adulteration with commercial syrups.

Honey adulterations can be carried out by addition of inexpensive sugar syrups, such as high fructose corn syrup (HFCS) and inverted syrup (IS). Carbohydrate composition of 20 honey samples (16 nectar and 4 honeydew honeys) and 6 syrups has been studied by GC and GC-MS in order to detect differences between both sample groups. The presence of difructose anhydrides (DFAs) in these syrups is described for the first time in this paper; their proportions were dependent on the syrup type considered.

Estimation of recovery by multistep purge-and-trap gas chromatographic-mass spectrometric analysis of honey volatiles.

Calculation of volatile recovery in dynamic headspace techniques such as purge-and-trap (P&T) usually requires a calibration with standard compounds. When these are not available, application of mathematical models to the results obtained by multistep fractionation of a sample can be used for the estimation of recovery. A comparison of the fit quality of quantitative data (GC peak areas) using different calculation procedures and of the results of recovery estimation is presented for different honey volatiles.

Use of gas chromatography-mass spectrometry for identification of a new disaccharide in honey.

Gas chromatography-mass spectrometry has been used to separate and identify disaccharides of edible honey. According to the characteristic fragmentation behaviour of disaccharide TMS-oximes, fructofuranosyl-(2-1)-fructose (inulobiose) has been structurally characterized. Identification was carried out on the basis of retention time on two columns of different polarity and mass spectrometric analysis.

A GC method for simultaneous analysis of bornesitol, other polyalcohols and sugars in coffee and its substitutes.

A GC method has been developed for the determination of polyalcohols and sugars in aqueous extracts from green coffee beans, ground roasted coffee beans submitted to either conventional or torrefacto processes, coffee blends and soluble instant coffees. Bornesitol was detected in aqueous coffee extracts for the first time. Mannitol, myo-inositol, mannose, fructose, galactose, glucose and sucrose have also been determined.

Purification of lactulose from mixtures with lactose using pressurized liquid extraction with ethanol-water at different temperatures.

The viability of the purification of lactulose from a mixture with lactose [70:30 (w/w)] using pressurized liquid extraction (PLE) at 1500 psi for 30 min was studied. Different temperatures (from 40 to 130 degrees C) and proportions of ethanol:water (70:30, 80:20, 90:10, 95:5, and 100:0) as the extraction solvent were assayed. Lactose and lactulose were measured by gas chromatographic analysis as their trimethylsilyl derivatives.

Recent developments in sample preparation for chromatographic analysis of carbohydrates.

Carbohydrates are a very important group of compounds due to their roles as structural materials, sources of energy, biological functions and environmental analytes; they are characterized by their structural diversity and the high number of isomers they present. While many advances have been made in carbohydrate analysis, the sample preparation remains difficult. This review aims to summarize the most important treatments which have been recently developed to be applied prior to the analysis of carbohydrates by chromatographic techniques.

Development of a robust method for the quantitative determination of disaccharides in honey by gas chromatography.

An iterative method for the GC quantitative determination of TMS-oxime disaccharides in honey has been developed. This approach takes into account possible positive systematic errors caused by unidentified compounds which overlap with the expected disaccharides. The results of its application to the determination of 15 disaccharides in simulated honey samples indicate that the iterative method is more robust that methods based on least-squares regression, improves the accuracy of the quantitative analysis and allows to detect the possible presence of disaccharides not identified.

Characterization of Spanish unifloral honeys by solid phase microextraction and gas chromatography-mass spectrometry.

Volatile compounds have been investigated in unifloral honeys of the most popular types in Spain. A total of 21 eucalyptus samples, 35 rosemary samples, 33 heather samples, and 15 citrus samples were collected in the course of 3 years in different Spanish regions. Samples were analyzed by SPME followed by GC-MS.

Gas chromatographic-mass spectrometric method for the qualitative and quantitative determination of disaccharides and trisaccharides in honey.

An improved method has been developed to identify and quantify honey disaccharides and trisaccharides by gas chromatography and mass spectrometry. The procedure, based on mass spectral and retention data ("retention time windows") determined on two capillary columns with different stationary phases allowed the identification and quantitation in honey of 16 disaccharides and 9 trisaccharides, some of which were not previously identified by GC. The reliability of the analytical results was considerably improved by the use of this procedure: several unidentified disaccharides and trisaccharides were detected, and their presence was taken into account in the quantification.

Patterns in the precision of quantitative data from multicomponent gas chromatographic or gas chromatographic-mass spectrometric analysis.

The dispersion of the quantitative results in the analysis of volatile compounds from multicomponent mixtures by different fractionation techniques (solid-phase microextraction and direct thermal desorption) followed by GC or GC-MS presents nonrandom patterns related to the existence of different factors in the fractionation process or in the chromatographic separation which affect, to a different extent, the recovery of the sample components. Statistical techniques have been used to show the relative importance of these factors. The improvement in data precision achieved by using volatile compound concentration ratios is discussed.