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At least 631 records · Page 35Linked to original sources

Chiral selectors from fruit: application of citrus pectins to enantiomer separations in capillary electrophoresis.

Pectins were investigated as chiral selective agents in capillary electrophoresis. Successful enantioresolution of antihistaminic and antimalarial compounds, as well as others, was achieved by utilizing potassium polypectate as the chiral selector. Changes in pH, chiral additive concentration and capillary type were studied in relation to chiral resolution. The effect of degree of esterification of pectin materials on chiral recognition was also evaluated.

Electrophoresis, Capillary↗

High-performance liquid chromatography of methanol released from pectins after its oxidation to formaldehyde and condensation with 2,4-dinitrophenylhydrazine.

A procedure was developed to measure the content of methanol in pectins after the base-catalysed hydrolysis of galacturonic acid methyl esters and oxidation of released methanol with potassium permanganate followed by condensation of the resulting formaldehyde (HCHO) with 2,4-dinitrophenylhydrazine (DNPH) dissolved in acetonitrile. The constant yields of resultant formaldehyde 2,4-dinitrophenylhydrazone (HCHO-DNPH derivative) were obtained at molar ratios of DNPH/HCHO higher than 5. The separation of the HCHO-DNPH derivative from DNPH reagent was achieved by isocratic reversed-phase HPLC equipped with the spectrophotometric detector set at a wavelength of 351 nm. The calibration curve was linear in the methanol concentration range between 0.04 and 15 micromol/ml (R=0.9995). The total recovery from pectin solutions spiked with methanol was equal to 100.6+/-5.1%.

Acetonitriles↗

Patterns of methyl and O-acetyl esterification in spinach pectins: new complexity.

Driselase-digestion of cell walls from suspension-cultures of spinach (Spinacia oleracea L.), followed by anion-exchange chromatography, gel-permeation chromatography, preparative paper chromatography and preparative paper electrophoresis, yielded ten uronic acid-containing products in addition to free galacturonic acid (GalA). These included 4-O-methylglucuronic acid, alpha-L-rhamnopyranosyl-(1-->4)-D-glucuronic acid and several oligosaccharides containing GalA residues. The structures were unambiguously determined by a combination of 1- and 2-dimensional NMR spectroscopic techniques. Five of the six homogalacturonan-derived oligosaccharides purified contained 3-O-acetyl-GalA residues; however, methyl-esterified GalA residues occurred adjacent to both 2-O-acetyl-GalA and 3-O-acetyl-GalA residues. An acetylated, rhamnogalacturonan-I-derived oligosaccharide that was purified also contained 3-O-acetyl-GalA residues. Taken together with published data, our findings indicate considerable diversity in the patterns of pectin esterification. The implications for the action of pectin esterases are discussed.

Cell Wall↗

Effect of pectin, guar gum, and wheat fibre on serum-cholesterol.

36 G of wheat fibre, pectin, or guar gum was given over 2-week periods to healthy volunteers taking normal diet. Mean serum-cholesterol levels fell significantly while the volunteers were taking guar and pectin by 36-3 and 29-2 mg, per 100. respectively, but rose slightly after wheat fibre by 6-7, mg per 100., Attention should be focused on fruit and vegetable gels rather than wheat fibre in the search of natural hypocholesterolaemic agents.

Adult↗

Effect of pectin on serum lipids and lipoproteins, whole-gut transit-time, and stool weight.

Pectin (12g daily with meals) was taken by twelve healthy men aged 22-45 (mean 25 yr) for 3 weeks. This produced a statistically significant mean decrease in total serum-cholesterol of 0.48 +/- 0.18 mmol/1 (+/- S.E.M.)--i.e., 7.9 +/- 2.6%. The decrease was largely due to a reduction in serum-low-density-lipoprotein-cholesterol of 0.45 +/- 0.19 mmol/1 accompanied by a fall in serum-apolipoprotein-B of 0.11 +/- 0.04 g/1. During pectin administration wet stool weight increased from 150 +/- 10 to 186 +/- 15 g/24 h. There was no clear change in total serum-triglycerides, serum very low density lipoproteins, or in whole-gut transit-time.

Adult↗

A new approach for studying interaction of the polygalacturonase-inhibiting proteins with pectins.

A method for determination of the interaction between pectins and proteins was developed using cross-linked polygalacturonic acid (CLPG) as the pectic substrate and polygalacturonase-inhibiting proteins (PGIPs). Defined water-insoluble pectins were prepared by chemical substitutions with acetyl or methoxyl groups on CLPG. In the presence of 0.1 M NaCl, PGIPs fully bound to CLPG but not to cross-linked alginic acid (CLAL), which had a similar pK(a) to CLPG, suggesting that the inhibitor was not simply bound to the substrate by nonspecific electrostatic interaction. Optimum binding of PGIPs to CLPG occurred at pH 2.4 to 4.7. The binding ability of the inhibitor to CLPGs with degree of methylation (DM) of 66% or degree of acetylation (DAc) of 133% was not significantly changed. In contrast, the DM of 82% or 95% decreased the binding. These results indicated that the carboxylic groups of galacturonic acid residues were involved in the recognition of the substrate by PGIPs.

Cross-Linking Reagents↗

Oral mucosal bioadhesive tablets of pectin and HPMC: in vitro and in vivo evaluation.

The potential of tablets containing 1:4, 1:1 and 4:1 weight ratios of pectin and hydroxypropyl methylcellulose (HPMC) for the sustained release of diltiazem by sublingual administration has been investigated. Measurements of maximum adhesive force to rat peritoneal membrane indicated a satisfactory bioadhesive strength. An in vitro sustained release of diltiazem over 5 h was achieved with bilayer tablets composed of a drug-free ethylcellulose layer in addition to the pectin/HPMC layer containing drug. Plasma concentration-time curves obtained following sublingual administration to rabbits of single and bilayer tablets with 1:1 weight ratios of pectin and HPMC showed evidence of sustained release of diltiazem. Bioavailability of diltiazem was 2.5 times that achieved by oral administration for single layer tablets and 1.8 times for the bilayered tablets.

Adhesives↗

Pectin microspheres as ophthalmic carriers for piroxicam: evaluation in vitro and in vivo in albino rabbits.

Microparticulate polymeric delivery systems have been suggested as a possible approach to improve the low bioavailability characteristics shown by standard ophthalmic vehicles (collyria). Purpose of this study was the evaluation of pectin microspheres as delivery system for piroxicam (Px). The microspheres were prepared by a spray-drying technique; their morphological characteristics were investigated by scanning electron microscopy (SEM), and their in vitro release behavior was evaluated in pH 7.0 USP buffer using a flow-through apparatus. Px loaded in the pectin microspheres showed a faster in vitro dissolution rate with respect to solid micronized drug. The precorneal retention of fluorescein-loaded microspheres was evaluated in vivo in albino rabbits: an aqueous dispersion of fluorescent microspheres showed a significantly increased residence time in the eye (2.5 vs. 0.5 h) when compared with a fluorescein solution. In vivo tests in rabbits of dispersions of Px-loaded microspheres also indicated a significant improvement of Px bioavailability in the aqueous humour (2.5-fold) when compared with commercial Px eyedrops. The potential advantages and limitations of this delivery system are discussed.

Animals↗

Characterization of association and gelation of pectin in methanol-water mixtures.

Turbidity, swelling, and rheological features of semidilute systems of pectin in methanol-water media of different composition have been investigated. By increasing the percentage of methanol in the mixture, the thermodynamic properties of the pectin/methanol/water system become poorer, as shown by increasing turbidity and decreasing swelling. Effects of oscillatory and steady shear flows on intermolecular associations and gelation of pectin in methanol/water mixtures are reported. The effects of methanol concentration on the growth and structure of shear-induced gels, stabilized through hydrogen bonds, are analyzed. Steady shear measurements on these systems reveal shear thickening at low shear rates and disruption of intermolecular associative junctions at high shear rates.

Adsorption↗

Chromatographic and enzymatic strategies to reveal differences between amidated pectins on a molecular level.

The intermolecular distributions of amide groups within two commercial LMA pectins was studied after removal of the methyl esters followed by fractionation of the different populations by anion exchange chromatography. The populations obtained had almost equal degrees of amidation while the values of the degree of blockiness were not the same, indicating also a different intramolecular distribution of the substituents considered as semirandom. Populations from the methyl-esterified amidated pectins showed a rather random distribution for almost all populations. A striking difference between these different populations was that, despite the same level of substitution, the ratio between amide groups and methyl esters varied significantly, indicating a heterogeneous amidation process.

Amides↗

The influence of gel strength on aroma release from pectin gels in a model mouth and in vivo, monitored with proton-transfer-reaction mass spectrometry.

The course of events from taking a food into the mouth to the perception of the food's flavor involves many steps, from dilution with saliva, mastication, and transportation of the compounds to the olfactory epithelium to transformation into signals that go to the brain. In addition, there are also the effects of the food's structure and properties. In this study, a proton-transfer-reaction mass spectrometer (PTR-MS) was used to investigate how four pectin-containing systems with different structures and strengths affected the release of aroma compounds in a model mouth and in the nose of an assessor. Both the model mouth and the in-nose measurements showed that the strength and structure of pectin-containing systems are important with regard to the quantity of aroma compounds that are released. Mastication and saliva were also shown to have a large influence on how much of the aroma compound is released from the mouth to the nose.

Chemical Phenomena↗

Production and characterization of O/W emulsions containing droplets stabilized by lecithin-chitosan-pectin mutilayered membranes.

The possibility of producing stable oil-in-water (O/W) emulsions containing oil droplets surrounded by multiple layer interfacial membranes from food grade ingredients has been demonstrated. These emulsions were produced using a three stage process that relies on the adsorption of charged biopolymers to oppositely charged surfaces. Emulsions (0.5 wt % corn oil, 0.1 wt % lecithin, 0.0078 wt % chitosan, 0.02 wt % pectin, and 100 mM acetic acid, pH 3.0) containing oil droplets stabilized by lecithin-chitosan-pectin membranes were formed using this interfacial layer-by-layer deposition process. The droplets in these emulsions had good stability to aggregation over a wide range of pH values and salt concentrations (pH 4-8 at 0 mM NaCl and pH 3-8 at 100 mM NaCl). This technology could be extremely useful to the food industry for the creation of O/W emulsions with improved properties or novel applications, e.g., improved stability to environmental stresses, protection of labile substances, controlled release, and triggered release.

Adsorption↗

Influence of aroma compounds on the mechanical properties of pectin gels.

A detailed study of the rheological behavior of pectin gels, in the presence of aroma compounds in food concentration is reported. In high methoxylated pectin (HMP) gels, it has not yet been shown if aroma compounds can be responsible for modifications in rheology. Two rheological techniques were used to measure the impact of aroma substances on rheological properties of HMP-based systems. Maximum strain to fracture (sigma F) was compared between flavored and unflavored gels on stress-displacement curve, which was obtained with uniaxial compression until fracture. An oscillatory rheometer was applied to determine the gelation time (Tgel). It appeared that all the aroma compounds studied increased significantly sigma F. It is generally acknowledged that hydrophobic interactions are the main interactions leading to HMP gelation, and the more hydrophobic interactions there are, the higher the sigma F. It is assumed that esters might increase sigma F through the increase of hydrophobic interactions in HMP network. For solvents (ethanol, propylene glycol), a cosolute effect could explain the increase in firmness for HMP-based gels.

Food Analysis↗

Activity and process stability of purified green pepper (Capsicum annuum) pectin methylesterase.

Pectin methylesterase (PME) from green bell peppers (Capsicum annuum) was extracted and purified by affinity chromatography on a CNBr-Sepharose-PMEI column. A single protein peak with pectin methylesterase activity was observed. For the pepper PME, a biochemical characterization in terms of molar mass (MM), isoelectric points (pI), and kinetic parameters for activity and thermostability was performed. The optimum pH for PME activity at 22 degrees C was 7.5, and its optimum temperature at neutral pH was between 52.5 and 55.0 degrees C. The purified pepper PME required the presence of 0.13 M NaCl for optimum activity. Isothermal inactivation of purified pepper PME in 20 mM Tris buffer (pH 7.5) could be described by a fractional conversion model for lower temperatures (55-57 degrees C) and a biphasic model for higher temperatures (58-70 degrees C). The enzyme showed a stable behavior toward high-pressure/temperature treatments.

Capsicum↗

Elucidation of the emulsification properties of sugar beet pectin.

A protocol has been developed to fractionate sugar beet pectin using hydrophobic affinity chromatography. Three samples eluted from the column using 4 M NaCl as solvent (fractions 1A, 1B, and 1C), two fractions eluted using 2 M NaCl (fractions 2A and 2B), and one fraction eluted using water (fraction 3). The fractions were shown to be very polydisperse, and differences between the GPC refractive index and UV absorbance (214 nm) elution profiles demonstrated chemical heterogeneity. They were found to contain significantly different proportions of protein (1A, 2.79%; 1B, 0.97%; 1C, 0.77%; 2A, 1.41%; 2B, 5.09%; and 3, 5.89%) and ferulic acid (approximately 1A, 0.5%; 1B, 0.5%; 1C, 0.9%; 2B, 1.5%; and 3, 2%). The weight-average molecular mass, M(w), of the fractions also varied (1A, 153 kDa; 1B, 155 kDa; 1C, 306 kDa; 2A, 562 kDa; 2B, 470 kDa; 3, 282 kDa). Three fractions, that is, 1A, 1B, and 3, produced orange oil emulsions with a relatively small droplet size that were stable over a period of weeks. The other three fractions (1C, 2A, and 2B with higher M(w) values) produced emulsions with an initially larger droplet size, and the droplet size increased considerably over time. The increased droplet size may be influenced by the viscosity of the aqueous continuous phase. There was no simple relationship between protein or ferulic acid content and emulsification ability. For example, fraction 1B, which contained the lowest proportion of both protein and ferulic acid, produced stable emulsions of similar droplet size to fraction 3, which contained the largest proportion of protein and ferulic acid. The role of protein in the emulsification process was investigated by measuring the amount of protein in the aqueous phase before and after emulsification. It was clearly demonstrated that proteinaceous material adsorbed at the oil-water interface. It is evident that the emulsification properties of sugar beet pectin are influenced by the accessibility of the protein and ferulic acid groups to the surface of the oil droplets, the proportion of ester groups, and the molecular mass distribution of the fractions.

Amino Acids↗

Stabilizing behavior of soy soluble polysaccharide or high methoxyl pectin in soy protein isolate emulsions at low pH.

The stability of emulsions prepared with soy protein isolates was investigated as a function of pH in the presence of two negatively charged polysaccharides: high methoxyl pectin (HMP) and soy soluble polysaccharide (SSPS). Both polysaccharides are composed of a backbone which contains galacturonic acid but, when added to soy protein isolate-stabilized emulsions, SSPS showed a different behavior than that of HMP. At neutral pH and above a critical concentration of stabilizer (0.05%), HMP caused flocculation of the emulsion droplets via a depletion mechanism. On the other hand, the emulsions containing a similar amount of SSPS did not show creaming or flocculation. At acidic pH (<4.0) the addition of pectin caused extensive droplet aggregation, while no aggregation was observed with the addition of SSPS. The differences in the stabilization behavior between the two polysaccharides can be attributed to their differences in charge, neutral sugars side chains, and molecular weight.

Drug Stability↗

Immobilized zinc affinity chromatography of pectin hydroxamic acids for purification of trypsin inhibitors from soybean and sweet potato.

Commercial pectin (with a 94% degree of esterification, DE94) suspended in methanol was reacted with methanolic alkaline hydroxylamine at room temperature for 20 h to prepare pectin hydroxamic acids (PHAs). The prepared PHA was coupled to the epoxy-activated Sepharose 6B gel to get immobilized PHA resins. The immobilized PHA resin was then balanced in column with 2 mM ZnCl2 in 50 mM Tris-HCl buffer (pH 7.9) to test the immobilized Zn-PHA gel as solid phase for immobilized metal affinity chromatography for the purification of trypsin inhibitors (TIs) from soybean and sweet potato. Using TI activity staining, it was found that purified TIs from the commercial soybean and sweet potato after trypsin affinity column purification could be adsorbed onto an immobilized Zn-PHA affinity column and eluted by 100 mM EDTA in 10 mM Tris-HCl buffer (pH 7.9). The immobilized Zn-PHA affinity column was used for TI purifications from crude extracts of sweet potato. The recovery of TI activity for one step was 90%, with 19.74-fold purification increase.

Chromatography, Affinity↗