Natural Deep Eutectic Solvents for Solubility and Selective Fractionation of Bioactive Low Molecular Weight Carbohydrates.

Natural deep eutectic solvents (NADESs) have been shown to be selective and environmentally friendly solvents for the extraction of bioactive compounds. However, studies on the solubility of low-molecular-weight carbohydrates (LMWCs) in NADESs are scarce. In this work, new solubility data of LMWCs in NADESs are provided and a new approach based on the use of these solvents for the efficient fractionation of bioactive carbohydrates was explored for the first time.

Quality Evaluation of Dietary Supplements for Weight Loss Based on .

Food supplements of plant origin for weight control are increasingly being demanded by consumers as a way to promote good health. Among them, those based on (GCFS) are widely commercialized considering their bioactive properties, mainly due to (-)-hydroxycitric acid ((-)-HCA). However, recently, controversy has arisen over their safety; thus, further research and continuous monitoring of their composition is required.

Development of a multianalytical strategy for detection of frauds in Coleus forskohlii supplements.

A new multianalytical methodology based on gas chromatography (GC) and liquid chromatography (LC) coupled to mass spectrometry (MS) has been proposed to evaluate frauds affecting the composition of Coleus forskohlii root supplements (FKS). After optimization and validation of chromatographic methods, 24 FKS were analyzed. Forskolin, their main bioactive component, was only found in 50% of the FKS evaluated (in the 0.

A multi-analytical strategy for evaluation of quality and authenticity of artichoke food supplements for overweight control.

Despite the widespread use of artichoke-based food supplements for obesity control (FSOC), studies on evaluation of the quality/authenticity of these commercial products are scarce. To that aim, a new multi-analytical strategy, based on the use of gas chromatography coupled to mass spectrometry (GC-MS) and high performance liquid chromatography coupled to ultraviolet and mass spectrometry detection (HPLC-UV-MS), in combination with chemometrics, has been developed. Twenty-one artichoke FSOC and different bract and leaf extracts (used as reference samples) were analysed.

Microwave Assisted Extraction of Bioactive Carbohydrates from Different Morphological Parts of Alfalfa ( L.).

Despite the nutritional properties of alfalfa, its production is mainly for animal feed and it is undervalued as a food source. In this study, the valorization of alfalfa as a potential source of bioactive carbohydrates [inositols, α-galactooligosaccharides (α-GOS)] is presented. A Box-Behnken experimental design was used to optimize the extraction of these carbohydrates from leaves, stems, and seeds of alfalfa by solid-liquid extraction (SLE) and microwave-assisted extraction (MAE).

Separation of di- and trisaccharide mixtures by comprehensive two-dimensional liquid chromatography. Application to prebiotic oligosaccharides.

Carbohydrates are one of the most important ingredients in foods. They are normally present as complex mixtures with different glycosidic linkages, monomeric units and degrees of polymerization. This structural heterogeneity impairs their comprehensive characterization and requires the use of analytical techniques with high resolving power and sensitivity.

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.

A new method for microwave assisted ethanolic extraction of Mentha rotundifolia bioactive terpenoids.

A new microwave-assisted extraction (MAE) method using ethanol as solvent has been optimized by means of a Box-Behnken experimental design for the enhanced extraction of bioactive terpenoids from Mentha rotundifolia leaves; 100°C, 5 min, 1.125 g dry sample: 10 mL solvent and a single extraction cycle were selected as optimal conditions. Improved performance of MAE method in terms of extraction yield and/or reproducibility over conventional solid-liquid extraction and ultrasound assisted extraction was also previously assessed.

Enzymatic Synthesis and Structural Characterization of Theanderose through Transfructosylation Reaction Catalyzed by Levansucrase from Bacillus subtilis CECT 39.

This work addresses the high-yield and fast enzymatic production of theanderose, a naturally occurring carbohydrate, also known as isomaltosucrose, whose chemical structure determined by NMR is α-d-glucopyranosyl-(1 → 6)-α-d-glucopyranosyl-(1 → 2)-β-d-fructofuranose. The ability of isomaltose to act as an acceptor in the Bacillus subtilis CECT 39 levansucrase-catalyzed transfructosylation reaction to efficiently produce theanderose in the presence of sucrose as a donor is described by using four different sucrose:isomaltose concentration ratios. The maximum theanderose concentration ranged from 122.

Assessment of Maillard reaction evolution, prebiotic carbohydrates, antioxidant activity and α-amylase inhibition in pulse flours.

In this paper, the quality of bean, chickpea, fava beans, lentil and pea flours from Algeria has been evaluated. Maillard reaction (MR) indicators, modifications in the carbohydrate and protein fractions, antioxidant activity and α-amylase inhibitor of raw, toasted and stored samples were evaluated. Fava beans, beans and peas showed higher content of raffinose family oligosaccharides while chickpeas and lentils showed higher polyol content.

Characterization of post-translationally modified peptides by hydrophilic interaction and reverse phase liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry.

This work explores the use of both hydrophilic interaction liquid chromatography (HILIC) and reverse phase liquid chromatography (RPLC) for the separation and subsequent characterization of bovine caseinomacropeptide (CMP) phosphopeptides and O-glycopeptides using a quadrupole-time-of-flight (QTOF) mass spectrometer with electrospray ionization. Two neutral, ethylene bridged hybrid (BEH) amide and polyhydroxyethyl aspartamide (PHEA), and a zwitterionic, sulfobetaine (ZIC), stationary phases were used for the HILIC mode, whilst an octadecylsilane (C18) stationary phase was employed for the RPLC separation. Overall, developed HILIC-QTOF method using the ZIC or BEH amide stationary phases resulted to be the most efficient methods to separate and characterize post-translationally modified (PTM) peptides without the need of any previous fractionation or derivatization step.

Hydrolyzed caseinomacropeptide conjugated galactooligosaccharides support the growth and enhance the bile tolerance in Lactobacillus strains.

In this study bioactive caseinomacropeptide was conjugated with prebiotic galactooligosaccharides (hCMP:GOS) by Maillard reaction to synthesize value added prebiotic compounds to Lactobacillus strains. Growth study showed the ability of hCMP:GOS to serve as a sole carbon source for Lactobacillus strains. A significant amount of acetate and lactate was detected in cell free culture supernatant by HPLC.

Evaluation of different operation modes of high performance liquid chromatography for the analysis of complex mixtures of neutral oligosaccharides.

Chromatographic methods based on different HPLC operation modes, reverse phase (RP), high performance anion exchange chromatography (HPAEC), graphitized carbon chromatography (GCC) and hydrophilic interaction liquid chromatography (HILIC), have been developed and compared for the analysis of complex mixtures of neutral oligosaccharides with functional properties. Whereas GCC gave the best chromatographic separation of isomeric oligosaccharides with the same molecular weight (R(s) values in the range 1.0-4.

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.

Separation of disaccharides by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry. Application to honey analysis.

A new method based on comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-ToF MS) has been developed for the first time for the analysis of complex mixtures of disaccharides previously converted to their trimethylsilyl oximes (TMSO). Among the different experimental parameters considered for optimization, both the column set combination and the dimensions of the second-dimension column were found to be the most significant with regard to the complete resolution of structurally similar disaccharides. Application of the optimized method to honey analysis allowed the separation of most of the honey disaccharides previously described in the literature.

Development of a new method using HILIC-tandem mass spectrometry for the characterization of O-sialoglycopeptides from proteolytically digested caseinomacropeptide.

This work addresses the optimization of HILIC (hydrophilic interaction liquid chromatography)-ESI-MS(n) conditions for the comprehensive characterization of O-glycopeptides from proteolytically digested caseinomacropeptide. O-Glycopeptides were satisfactorily analysed on a zwitterionic HILIC column based on their glycan structure and amino acid sequence. The contribution of ionic interactions to the retention of charged glycopeptides was found to be substantial.

Carbohydrate composition of high-fructose corn syrups (HFCS) used for bee feeding: effect on honey composition.

In this study, the carbohydrate composition of high-fructose corn syrups (HFCS) from commercial manufacturers as well as from beekeepers was characterized by GC-MS. Sucrose syrups (SS) were also included in this work for comparison. Fructosyl-fructoses and some unknown carbohydrates, which could correspond to fructosyl-glucoses, have been detected in HFCS for the first time, whereas SS were mainly characterized by the high contents of sucrose.

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.

Mass spectrometric characterization of glycated beta-lactoglobulin peptides derived from galacto-oligosaccharides surviving the in vitro gastrointestinal digestion.

A mass spectrometric study has been carried out to elucidate the structures of glycated peptides obtained after in vitro gastrointestinal digestion of bovine beta-lactoglobulin (beta-LG) glycated with prebiotic galacto-oligosaccharides (GOS). The digests of both native and glycated beta-LG were analyzed by MALDI-MS, LC-ESI-MS, and LC-ESI-MS/MS. MALDI-MS profiles showed marked differences mainly related to the lower intensity of ions corresponding to the digest of glycated beta-LG.

Simultaneous analysis of lysine, Nepsilon-carboxymethyllysine and lysinoalanine from proteins.

Protein quality was assayed by simultaneous measurement of lysine (Lys), carboxymethyllysine (CML) and lysinoalanine (LAL). GC-FID analysis of N-tert-butyl dimethylsilyl (tBDMSi) derivatives of these amino acids was undertaken. tBDMSi derivates were separated on a CP-SIL 5CB commercially fused silica capillary column (25 m x 0.

Characterization and in vitro digestibility of bovine beta-lactoglobulin glycated with galactooligosaccharides.

Galactooligosaccharides (GOS) are well-known prebiotic ingredients which can form the basis of new functional dairy products. In this work, the production and characterization of glycated beta-lactoglobulin (beta-LG) with prebiotic GOS through the Maillard reaction under controlled conditions ( a(w) = 0.44, 40 degrees C for 23 days) have been studied.

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.

Influence of glycosidic linkages and molecular weight on the fermentation of maltose-based oligosaccharides by human gut bacteria.

A structure-function study was carried out to increase knowledge of how glycosidic linkages and molecular weights of carbohydrates contribute toward the selectivity of fermentation by gut bacteria. Oligosaccharides with maltose as the common carbohydrate source were used. Potentially prebiotic alternansucrase and dextransucrase maltose acceptor products were synthesized and separated into different molecular weights using a Bio-gel P2 column.

Selective fermentation of gentiobiose-derived oligosaccharides by human gut bacteria and influence of molecular weight.

Gentiooligosaccharides and alternansucrase gentiobiose acceptor products were fractionated by their degree of polymerization (DP) on a Bio-Gel P2 column. Fractions were characterized by matrix-assisted laser desorption ionization time-of-flight mass spectroscopy, and incubated with human faecal bacteria under anaerobic conditions at 37 degrees C. The growth of predominant gut bacteria on the oligosaccharides was evaluated by fluorescence in situ hybridization and a prebiotic index (PI) was calculated.