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Chemical and Functional Properties of Food Saccharides

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© 2004 by CRC Press LLC<br />

TABLE 22.2<br />

Experimental Approaches to Obtain Molecular <strong>and</strong> Supramolecular<br />

Characteristics <strong>of</strong> Starch Polysaccharides<br />

Experimental Approach Information<br />

Thin layer chromatography (TLC)<br />

Enzymatic assays<br />

Reversed phase high performance liquid<br />

chromatography (rpHPLC)<br />

High performance anion-exchange<br />

chromatography – pulsed amperometric<br />

detection (HPAEC-PAD)<br />

Enzymatically controlled step-by-step<br />

fragmentation + fragment analysis by rpHPLC<br />

or size-exclusion chromatography (SEC)<br />

Semipreparative SEC: staining <strong>and</strong> complexing<br />

+ spectroscopy<br />

Identification <strong>and</strong> quantification <strong>of</strong> soluble<br />

components, monosaccharides, disaccharides,<br />

oligosaccharides obtained from direct<br />

extraction or enzymatic <strong>and</strong> acidic hydrolysis<br />

Branching characteristics: chain-lengths<br />

distribution, branching percentage<br />

Mass fractions separated according excluded<br />

volume for subsequent processing or analysis;<br />

fraction-specific branching characteristics;<br />

SEC: mass + st<strong>and</strong>ards Calibrated molecular weight distribution, degree<br />

<strong>of</strong> polymerization distribution, molecular<br />

weight averages<br />

Absolute molecular weight distribution, absolute<br />

degree <strong>of</strong> polymerization distribution, excluded<br />

SEC: mass, light scattering, <strong>and</strong> viscosity<br />

volume distribution, polysaccharide-coil<br />

packing density distribution<br />

Quantitative terminal labeling <strong>of</strong> polysaccharides<br />

+ SEC: mass/molar<br />

Absolute molecular weight distribution <strong>of</strong> molar<br />

fractions<br />

Intrinsic viscosity Excluded volume, overlapping concentration<br />

Viscosity at varying shear stress Viscous + elastic contributions (visoelasticity);<br />

gel properties<br />

Viscosity at increasing thermal stress Gelatinization temperature (range);<br />

disintegration temperature (range)<br />

Viscosity at varying thermal + constant<br />

mechanical stress (Brabender viscograph)<br />

Stability or resistance toward applied energy<br />

(temperature, shearing, periods); disintegration<br />

or reorganization capacities<br />

Differential scanning calorimetry (DSC) Modifications in conformation; phase transitions<br />

Photon correlation spectroscopy (PCL) Diffusion mobility <strong>of</strong> molecular <strong>and</strong><br />

supermolecular polysaccharide structures<br />

<strong>of</strong> the appropriate sequences <strong>of</strong> preparation <strong>and</strong> analyses for starch-containing crop<br />

materials: sampling at the location <strong>of</strong> harvesting followed by comprehensive <strong>and</strong><br />

time-consuming fractional preparations <strong>and</strong> analyses. In case <strong>of</strong> particular interest<br />

in individual parameters or a limited parameter group only, this scheme may be<br />

simplified; however, comprehensive information requires the full set.

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