Relationship between viscosity and molecular weight in an andosol humic acid

Viscosity and molecular weight of particle size fractions obtained from an Andosol humic acid (HA) were determined. Viscosity was determined both in solutions with and without the addition of 0.1 M NaCl (Cs 0.1 and Cs 0, respectively) at pH 7.0. Polyelectrolytic character was observed in the particle size fractions based on the changes in the concentration dependence of reduced viscosity with NaCI concentrations. The use of a Cs 0.1 solution was suitable for the determination of the values of intrinsic viscosity ([η]) of the particle size fractions. The [η] value increased with increasing weight average molecular weight ( M _w) determined by gel permeation chromatography (GPC), and ranged from 4.3 to 12.9 X 10-3 (L g^-1) in the Cs 0 solution and from 3.5 to 6.6 × 10^-3 (L g^-1) in the Cs 0.1 solution. A linear relationship between [η] in the Cs 0.1 solution and M _w on a logarithmic scale, which was similar to the MarkHouwink equation, was observed. The value of the constant a calculated from the relationship, which reflected the polymer morphology, was 0.75 in the Cs 0.1 solution, and it corresponded to a polymer with flexible chains.     

Molecular Characterization of Corn Starch Using an Aqueous HPSEC‐MALLS‐RI System Under Various Dissolution and Analytical Conditions

Molecular characteristics based on absolute weight‐average molecular weight (M_w) and z‐average radius of gyration (R_g) of normal corn starch were analyzed by high‐performance size‐exclusion chromatography (HPSEC) attached to multiangle laser‐light scattering (MALLS) and refractive index (RI) detectors under different starch dissolution and analytical conditions. Autoclaving (121°C, 20 min) or microwave heating (35 sec) provided better HPSEC recovery and higher M_w for starch molecules than simple dissolution in hot water. The M_w for the autoclaved corn amylopectin and amylose fractions separated with a TSK G5,000 column at 60°C were 201 × 10⁶ and 3.3 × 10⁶, respectively. The specific volume for gyration (SV_g) calculated from M_w and R_g could be used for the comparison of molecular compactness which was inversely related to the degree of branching. The SV_g values of amylopectin and amylose fractions in the chromatogram (TSK G5,000, autoclaved for 20 min) were 0.092 and 0.529, respectively. But a portion (20–30%) of large amylopectin molecules did not pass the injection membrane filter (3.0 μm) and the SEC column, resulting in incomplete recovery. The unfiltered portion varied according to the dissolution treatment. Homogenization (7,000 rpm, 5 or 10 min) of the starch solution improved the recovery of the amylopectin fraction, but significantly increased the M_w of the amylose fraction (17 × 10⁶). Sonication for 5 min degraded starch molecules. For accurate analysis of a native starch using an aqueous SEC, the starch should be fully dissolved with proper treatment such as autoclaving or microwaving, and the column should be improved for full recovery of large amylopectin molecules.     

Starch Molecular Mass and Size by Size-Exclusion Chromatography in DMSO-LiBr Coupled with Multiple Angle Laser Light Scattering

The weight average molar mass (M_w) and root mean square radii of starches from waxy maize (Amioca), waxy rice flour, cassava, Hylon V, Hylon VII, and potato amylose were determined by size-exclusion chromatography (SEC) and multiple-angle laser light scattering (MALLS). Dimethylsulfoxide (DMSO) containing 50 mM LiBr was used to dissolve the starches and also served as the mobile phase. SEC with large particle size polystyrene divinylbenzene packing materials and MALLS instrumentation were evaluated for the ability to separate and determine molar mass (MM) of starch polymers, respectively. The determination of M_w by MALLS is necessary because the M_w of many cereal starches exceeds the available molecular standards by one or two orders of magnitude. The M_w depends on the method of calculation. The M_w (Berry method) of starch from waxy corn was 2.27 × 10⁸ Da, waxy rice 8.9 × 10⁷ Da, cassava 5.7 × 10⁷ Da, Hylon V 2.7 × 10⁷ Da, Hylon VII 4.8 × 10⁶ Da, and potato amylose 1.9 × 10⁵ Da. Recovery dropped dramatically for molecules with root mean square radii >200 nm.     

Structural characterization of corn fiber gums from coarse and fine fiber and a study of their emulsifying properties

The stabilities of orange oil emulsions stabilized with various concentrations of two different types of corn fiber gum (CFG-1 and 2) isolated from coarse (pericarp) and fine (endosperm) fiber from corn wet milling have been studied. The emulsion stabilities in all these studies increased with increasing gum concentration up to a gum-to-oil ratio of 0.05, and after that it either levels off or changes very slightly. These results indicate that only 0.25% of CFG is required to make stable emulsion containing 5% orange oil under the experimental conditions used in this study. At this CFG concentration, CFG-2 from each fiber source was found to be a superior emulsifier relative to the corresponding CFG-1 from each source in a 10-day emulsion stability study at room temperature. The emulsion stability was also investigated by confocal laser scanning microscopy measurement, and it was found that CFG-1 and 2 from both coarse and fine fiber made stable emulsions with an average particle size of less than 1 mum for 10 days at room temperature. Sugar composition analysis of CFGs from both sources indicated that they were typical galactoglucuronoarabinoxylans containing mainly 55-59% xylose, 29-36% arabinose, and 4-6% galactose as neutral sugars and 3-5% glucuronic acid. Methylation analysis revealed a highly branched structure of all CFGs, in which only 16-25% of the 1--> 4-linked xylose residues were not substituted at O-2 and/or O-3. Arabinose is present both as a terminal residue and at branch points.     

Fractionation, characterization, and study of the emulsifying properties of corn fiber gum

Corn fiber gum (CFG) has been fractionated by hydrophobic interaction chromatography on Amberlite XAD-1180 resin using ionic, acidic, basic, and hydrophobic solvents of different polarities. Characterization, including determination of total carbohydrate, acidic sugar, and protein content, has been done for each fraction together with measurements of molar mass, polydispersity, radius of gyration, Mark-Houwink exponent, and intrinsic viscosity using multiangle laser light scattering and online viscosity measurements. Emulsification properties of all fractions in an oil-in-water emulsion system with 20:1 oil to gum ratio were studied by measuring turbidity over 14 days. The results indicate that CFG consists of different components differing in their molecular weights and carbohydrate and protein contents. The main fraction eluted with NaCl, although low in protein content, has the highest average molecular weight and was determined to be a better emulsifier than the other fractions. The unfractionated CFG, which contains different molecular species, is the best emulsifier.     

Structural Changes of Debranched Corn Starch by Aqueous Heating and Stirring

Aqueous dispersions (2 mg/mL) of debranched corn starches of different amylose contents (waxy, normal, and high‐amylose) were subjected to extensive autoclaving and boiling‐stirring, and then the changes in starch chain profile were examined using medium‐pressure, aqueous, size‐exclusion column chromatography. As autoclaving time increased from 15 to 60 min, weight‐average chain length (CL_w) of waxy, normal, and high‐amylose corn starches determined using pullulan standards decreased from 46 to 41.2, from 122.1 to 96.3, and from 207.3 to 151.8, respectively. Number‐average chain length (CL_n) measured by the Nelson‐Somogyi method also decreased from 23.0 to 18.4, from 26.4 to 21.8, and from 66.5 to 41.5, respectively, indicating that thermal degradation of starch chains occurred. The CL_w/CL_n ratio for normal corn starch was higher than that for waxy corn starch, indicating an increase in polydispersity of the amylose fraction. Thermal degradation was also observed when the debranched starch was subjected to the boiling‐stirring treatment (0–96 hr). During 96 hr, the CL_w and relative proportion of B≥2 chains of amylopectin released by debranching waxy corn starch increased, whereas those of B1 chains decreased. This change may indicate physical aggregation of B1 chains. But branches from normal and high‐amylose corn starches showed increases in CL_w and the proportion of both B1 and B≥2 chains, along with substantial decreases in those of amylose chains. Therefore, thermal degradation of amylose was greater than that of amylopectin.     

Molecular Characterization of Wheat Amylopectins by Multiangle Laser Light Scattering Analysis

Weight-average molecular weight (M_w) and chain length of eight amylopectins isolated from one Australian, two United States, and five Korean wheats were measured using multiangle laser light scattering (MALLS) and refractive index (RI) detectors operated in a microbatch mode, and in a high-performance size-exclusion chromatography (HPSEC) mode. The M_w of amylopectins measured in the microbatch mode ranged from 29 × 10⁶ to 349 × 10⁶. Three amylopectins (Geuru, Tapdong and WW) showed significantly high M_w values over 200 × 10⁶. The M_w measured by HPSEC mode with MALLS-RI detectors (42 × 10⁶ to 73 × 10⁶) were significantly less than those obtained in the microbatch mode with exception of dark northern spring hard wheat (DNS) amylopectin, indicating the possible variation of M_w by the analysis mode. Root-mean square of the radius of gyration (R_g) also was greater when the microbatch mode was used (122–340 vs. 95–116 nm). Chain length distributions of debranched amylopectins of different cultivars, measured by the HPSEC-MALLS-RI system, were similar. Weight average degrees of polymerization (DPw) of A, B₁, and larger B chains (B_≥2) had ranges of 13–22, 26–46, and 58–73, respectively, and mass ratios of A and B chains ranged from 0.7 to 1.1.     

Effect of Processing on Viscosity and Molecular Weight of (1,3)(1,4)‐β‐Glucan in Western Australian Oat Cultivars

Six Australian milling oat cultivars grown over two growing seasons were characterized for differences in (1,3)(1,4)‐β‐glucan (β‐glucan) viscosity, solubility, molecular weight (M_w), and the effect of processing. Oat cultivars grown in 2012 had significantly higher extracted β‐glucan viscosity from oat flour than the same oat cultivar grown in 2011 (P < 0.05, mean 137 and 165 cP, respectively). Noodle β‐glucan mean viscosity for 2012 (147 cP) was significantly higher than for 2011 (128 cP). β‐Glucan from ‘Williams’ and ‘Mitika’ oats had the highest viscosity (P < 0.05) in flour (5.92 and 5.25%, respectively) and noodles (1.64 and 1.47%, respectively) for both years, compared with the other oat cultivars. β‐Glucan (M_w) of Williams for 2012 and ‘Kojonup’ for both years were the least affected by processing, with an average drop of 33% compared with a maximum of 63% for other cultivars. Therefore, Williams showed superior β‐glucan properties to other oat cultivars studied, and can potentially provide improved health benefits. High and low β‐glucan M_w populations were found in the same elution peak after processing. Oat cultivars chosen for processing should be those with β‐glucans that are more resistant to processing, and that maintain their physiochemical properties and, therefore, bioactivity.     

Comparisons of Various Chemical Extracts as Quantity Factors to Determine Metal-Buffering Capacity of Soils

Applicability of various chemical extracts was investigated as quantity (Q) factors to determine cadmium (Cd), zinc (Zn), and copper (Cu) desorption quantity–intensity (Q/I) relationships in soils. The metal extracts were sums of sequential metal fractions (except the residual fraction) using Tessier's (TSE) and Community Bureau of Reference (BCR) procedures and various single chemical extracts: 1.0 M potassium nitrate (KNO₃), 1.0 M magnesium nitrate [Mg(NO₃)₂], 1.0 M magnesium chloride (MgCl₂), and 0.11 M acetic acid (CH₃COOH) solutions. Water-extractable metal was applied as a fixed intensity (I) factor. The TSE or BCR metal fractions were significantly correlated with diethylenetriaminepentaacetic acid (DTPA)–extractable metals, and all the metal desorption Q/I curves were linearly fitted. However, most of metal BC values estimated by using the single chemical extracts were very low and did not have consistent trends for target metals. Only 0.11 M CH₃COOH-extractable metals might be reliable. Therefore, TSE and BCR metal fractions can be applicable to replace DTPA-extractable metals, and 0.11 M CH₃COOH-extractable metals might also be useful.     

Assessment of the effect of molecular size on the electrophoretic mobility of humic substances

The basic principles of the electrophoretic behaviour of humic substances (HS) still need to be systematically investigated. HS extracted from a Cryorthod (HS–1) and from an Haplumbrept (HS–2) were first fractionated by ultrafiltration to obtain two series of fractions of reduced polydispersity with a nominal mean relative molecular mass (M) of 7500, 20000, 40000, 75000 and 200 000 Da. Fractions extracted from the same soil behaved like an homologous series when tested by size exclusion chromatography, showing a linear relation of M with molecular size. When plotted against their mean M, the elution volumes of HS fractions extracted from the two different soils originated lines of different slope. Absolute electrophoretic mobilities of the fractions were determined in polyacrylamide gel slabs of increasing polyacrylamide concentration using a single buffer system; in all gels there was a close linear relation between the electrophoretic mobility and the logarithm of the mean M of HS fractions. Extrapolation of mobilities of HS–1 at zero gel concentration gave intercepts that did not differ significantly, showing that there was a constant mobility for all fractions in free solution. These results mean that charge differences have little effect on the electrophoretic mobilities of HS extracted from the same soil and imply the theoretical possibility of determining M distributions of HS by polyacrylamide gel electrophoresis in a single buffer system. Mobilities of HS–2 fractions were compared with those of HS–1: the latter fitted the regression equations of mobility against logarithm of the molecular weight obtained from HS–1 humic substances only in gels of small acrylamide concentration. Deviations were larger at small M, probably because of the increasing fulvic character of the fractions, and increased in gels of greater acrylamide concentration, indicating that charge differences may not be negligible when comparing humic substances extracted from different soils.     

Rheological Properties of (1→3),(1→4)-β-d-Glucans from Raw,Roasted, and Steamed Oat Groats

Effects of hydrothermal treatments (steaming, roasting) of oat grain on β-glucan extractability and rheological properties were tested on oat cultivars with low (Robert) and high (Marion) β-glucan content. Steaming of grain reduced the amount of β-glucan that could be extracted, compared with raw or roasted grain, but the extracts from steamed grain had much greater viscosity. Increased extraction temperatures increased the amount and the average relative molecular mass (M _r) value of β-glucan extracted. In boiling water extractions, the average M _r values among raw, roasted and steamed oat samples were equivalent, but extracts from steamed oat grain had significantly higher intrinsic viscosity than the extracts from roasted or raw oat grains. β-glucan solutions purified from steamed grain extracts were very viscous and highly pseudoplastic, as described by the power law equation. Oat β-glucan from steamed samples were more viscoelastic than β-glucan from roasted or raw oat samples. Because viscous properties of β-glucan from boiling water extracts are influencedhydrothermal treatments without affecting polymer molecular weight, polymer interaction with the solvent must be affected. Steaming may disrupt intramolecular cross-linkings in native β-glucan, allowing a linear chain configuration to generate greater viscosity.     

Fractionation and distribution of selenium in soils

Abstract

A modified selenium (Se) fractionation procedure was used to study Se distribution in three soils (two silt loams and one silty clay). This sequential procedure consisted of: i) 0.2 M potassium sulfate (K₂SO₄)‐soluble fraction, ii) 0.1 M potassium dihydrogen phosphate (KH₂PO₄)‐exchangeable fraction, iii) 0.5 M ammonium hydroxide (NH₃H₂O)‐soluble fraction, iv) 6 M hydrochloric acid (HCl)‐extractable fraction, and v) residual fraction digested with perchloric (HClO₄) and sulfuric (H₂SO₄) acids. The fractionation procedure had high recovery rates (92.5 to 106%). The Se distribution in soil was controlled by soil properties, such as pH, oxide, clay, and calcium carbonate (CaCO₃) contents. In the untreated soil samples, residual Se fraction was dominant. In the Se‐enriched soils, the silty clay had significantly more Se in the NH₃H₂O and residual fractions while in the two silt loams the largest were KH₂PO₄ and residual fractions. The Se availability in the two silt loams was higher than in the silty clay. The Se availability pattern in the untreated soils was: unavailable (HCl + residual fractions) >> potentially available (KH₂PO₄ + NH₃H₂O fractions) > available (K₂SO₄ fraction), while in the Se‐enriched soils it was potentially available > unavailable > available.     

Soil Test to Predict the Copper Availability in Pasture Soils

Abstract

The proportion of copper (Cu) that can be extracted by soil test extractants varied with the soil matrix. The plant‐available forms of Cu and the efficiency of various soil test extractants [(0.01 M Ca(NO₃)₂, 0.1 M NaNO₃, 0.01 M CaCl₂, 1.0 M NH₄NO₃, 0.1 M HCl, 0.02 M SrCl₂, Mehlich‐1 (M1), Mehlich‐3 (M3), and TEA‐DTPA.)] to predict the availability of Cu for two contrasting pasture soils were treated with two sources of Cu fertilizers (CuSO₄ and CuO). The efficiency of various chemical reagents in extracting the Cu from the soil followed this order: TEA‐DTPA>Mehlich‐3>Mehlich‐1>0.02 M SrCl₂>0.1 M HCl>1.0 M NH₄NO₃>0.01 M CaCl₂>0.1 M NaNO₃>0.01 M Ca(NO₃)₂. The ratios of exchangeable: organic: oxide bound: residual forms of Cu in M1, M3, and TEA‐DTPA for the Manawatu soil are 1:20:25:4, 1:14:8:2, and 1:56:35:8, respectively, and for the Ngamoka soil are 1:14:6:4, 1:9:5:2, and 1:55:26:17, respectively. The ratios of different forms of Cu suggest that the Cu is residing mainly in the organic form, and it decreases in the order: organic>oxide>residual>exchangeable. There was a highly significant relationship between the concentrations of Cu extracted by the three soil test extractants. The determination of the coefficients obtained from the regression relationship between the amounts of Cu extracted by M1, M3, and TEA‐DTPA reagents suggests that the behavior of extractants was similar. But M3 demonstrated a greater increase of Cu from the exchangeable form and organic complexes due to the dual activity of EDTA and acids for the different fractions and is best suited for predicting the available Cu in pasture soils.     

Separation and Characterization of Barley Starch Polymers by a Flow Field‐Flow Fractionation Technique in Combination with Multiangle Light Scattering and Differential Refractive Index Detection

Flow field‐flow fractionation (flow FFF) with frit inlet and frit outlet mode (FIFO) was coupled online to multiangle light scattering (MALS) and refractive index (RI) detectors to investigate the molecular characteristics of normal and zero amylose barley starch polymers. Application of two different cross‐flows, 0.35 mL/min followed by 0.1 mL/min, and constant channel and frit flows of 0.1 and 1.0 mL/min, respectively, permitted a complete separation of amylose and amylopectin. The improved signals from the detectors due to application of the FIFO mode enabled the proper characterization of the small molecular weight species, as well as significantly enhanced the reproducibility of the measurements. The weight‐average molecular weight (M_w) and zaverage root‐mean‐square (RMS) radii of gyration (R_g) values for amylose and amylopectin in the normal starch samples were 2.3 × 10⁶ and 280 × 10⁶, and 107 and 260 nm, respectively. The M_w and R_g of amylopectin in the zero amylose starch samples were 360 × 10⁶ and 267 nm, respectively. The slopes (α) obtained by plotting log M_w versus log R_g for amylose and amylopectin were 0.6 and 0.3, respectively. These results are in good agreement with the theoretical prediction of the molecular conformation of amylose and amylopectin.     

Parameterization and regionalization of Cd sorption characteristics of sandy soils. I. Freundlich type parameters

Cd sorption isotherms (n = 24) were established for arable, sandy soils of the ‘Fuhrberger Feld’ catchment area northeast of Hannover (Germany) using 0.01 M_c Ca(NO₃)₂ solution with Cd additions ranging from 0 to 44 μM_c Cd. Alternative fractions of initially (prior to analysis) sorbed Cd (S₀) were added to the amount sorbed during the experiments. The Freundlich equation was fitted to the resulting isotherms. The obtained retention parameters k and M varied with respect to the different S₀ fractions. Isotherms corrected with Cd_EDTA as S₀ fraction were nonlinear in their log-form. The highest degree of log-linearity is obtained if S₀ is characterized by 40% of the agua regia extractable Cd. The corresponding k values ranged from 36 to 1275 g^1-M L^M kg^?1 (mean 338 g^1-M L^M kg^?1, cv = 92%). The Freundlich exponent M showed less variation (0.7 to 1.1, cv = 12%) with a mean of 0.88. Functions based on these parameters predicted Cd concentrations in Ca(NO₃)₂?soil suspensions well (r² = 0.96) but were hardly related to Cd concentrations of ‘fresh’ soil solutions (r² = 0.20).     

Sulphur mineralization and release of soluble organic sulphur from camp and non-camp soils of grazed pastures receiving long-term superphosphate applications

Summary Topsoils (0–75 mm) from four soil types with different sulphate retention capacities were collected from stock camp and non-camp (main grazing area) sites of grazed pastures in New Zealand which had been annually fertilized with superphosphate for more than 15 years. These soils were analysed for different S fractions and incubated at 30°C for 10 weeks using an open incubation technique in order to assess the extent of S mineralization and the release of soluble soil organic S from camp and non-camp soils during incubation. The soils were preleached with 0.01 M KCl, followed by 0.04 M Ca(H₂PO₄)₂ before being incubated. Pre-incubation leachates and weekly 0.01 M KCl leachates were analysed for mineralized S (i.e., hydriodic acid-reducible S) and total S. Soluble organic S was estimated as the difference between these two S fractions. Results obtained show higher cumulative amounts of all three S fractions in leachates over a 10-week incubation period in camp than in non-camp soils, suggesting that higher mineralization occurred in camp soils. Cumulative amounts of mineralized S from camp and non-camp soils showed a linear relationship with duration of incubation (R ²0.985^***), while the cumulative release of soluble organic S followed a quadratic relationship (R ²0.975^***). A significant proportion (14.6%–40.8%) of total S release in KCl leachates was soluble organic S, indcating that organic S should be taken into account when assessing S mineralization. Mineralized S and soluble organic S were best correlated with 0.01 M CaCl₂-extractable soil inorganic S (R ²=0.767^***) and 0.04 M Ca(H₂PO₄)₂-extractable soil inorganic S(R ²=0.823^***), respectively. Soil sulphate retention capacity was found to influence amounts of mineralized S and soluble organic S, and thus periodic leaching with KCl to remove mineralized S from soils may not adequately reflect the extent of soil S mineralization in high sulphate-retentive soils. In low (<10%) sulphateretentive soils, increasing the superphosphate applications from 188 to 376 kg ha^–1 year^–1 increased S mineralization but not amounts of C-bonded and hydriodic acid-reducible soil S fractions.     

Macromolecular Features of Amaranth Starch

High-performance size-exclusion chromatography (HPSEC), static light scattering (SLS) and dynamic light scattering (DLS) techniques were used for the structural characterization of amaranth starch, solubilized in water by microwave heating in a high-pressure vessel. Apparent average molar mass (M _w) gyration radius (R _G), and hydrodynamic radius (R _H) values were obtained from Berry and Zimm treatment of light-scattering data. When heating time increased from 35 to 90 sec, the M _w, R _G, and R _H decreased, demonstrating a possible polymer degradation due to temperature. Apparent M _r values from HPSEC at 35 sec (27 ± 2 × 10⁷ g/mol) and 50 sec (20 ± 2 × 10⁷ g/mol) were lower than those determined by SLS (35 sec = 69 × 10⁷ g/mol, 50 sec = 56 × 10⁷ g/mol). However, at 70 and 90 sec, the inverse pattern was obtained. The fractal dimensions (d′_f) from HPSEC study for samples dissolved for 35 (3.26), 50 (3.24), and 70 sec (3.14) are characteristic of a particle that has the internal structure of hard sphere, and for samples dissolved for 90 sec (2.19), are characteristic of a fully swollen, randomly branched macromolecule. From SLS, d′_f decreased with increasing treatment time (d′_f = 2.44, 2.18, 1.50, and 1.03 for 35, 50, 70, and 90 sec, respectively). The particle-scattering factors and Kratky plots, well-suited for studying the internal structure of a macromolecule, showed a sample degradation when treatment time increased. Results from DLS showed bimodal distributions with differences in the peak locations when treatment time increased. The ratio of R _G to R _H (ρ) for samples analyzed were between 0.88 and 1.3; these values are characteristic of a sphere or globular structure.     

几种测定石灰性土壤有效磷的方法的比较

土壤有效磷的测定有助于了解土壤的磷素供给能力,为施用磷肥提供参考,但是测定方法虽多,却各有优缺点;生物方法的结果比较接近实际情况,但操作不便,需时较久;化学方法简便快速,但往往适用范围不广,至今尚无适用所有土壤的化学浸提方法.     

β-Glucanase Activity and Molecular Weight of β-Glucans in Barley After Various Treatments

β-Glucanase activity interferes with molecular characterization of mixed-linkage (1→3)(1→4)-β-d -glucans (β-glucans). Reductions in β-glucanase activity were determined after barley cvs. Azhul, Waxbar, and Baronesse were treated with autoclaving (120°C, 45 min), calcium chloride (0.05M, 1 hr), 70% ethanol (80°C, 4 hr), hydrochloric acid (0.1N, 1 hr), oven heating (120 and 140°C, 40 min), sodium hydroxide (0.0025M, 1 hr), and 5% trichloroacetic acid (TCA) (40°C, 1 hr). High-performance size-exclusion chromatography (HPSEC) of α-amylase-treated aqueous extracts was used to demonstrate the effects of treatments on the molecular weights of β-glucans. The HPSEC system included multiple-angle, laser light scattering, refractive index, and fluorescence detectors. β-Glucanase activities, ranging from 52 to 65 U/kg of barley, were reduced by autoclaving (50–75%), hot alcohol (67–76%), oven heating (40–96%), CaCl₂ (75–95%), NaOH (76–89%), and TCA (92–96%). Some malt β-glucanase activity remained after most treatments. HCl and TCA treatments reduced extraction and molecular weights of β-glucans. Weight-average molecular weights (M_w) for β-glucans extracted with water at 23°C were low (most <8 × 10⁵). Base treatment (pH 9) and extraction at 100°C for 2.5 hr resulted in the greatest extraction of β-glucans and highest M_w. As a result, the conditions seem appropriate for measurement of physical characteristics of β-glucans in cereal products.     

Light-Scattering Molecular Weights and Intrinsic Viscosities of Processed Waxy Maize Starches in 90% Dimethyl Sulfoxide and H2O

Waxy maize starch was treated by a variety of gentle and severe methods: direct dispersion-solubilization into 90% dimethyl sulfoxide (DMSO) and H₂O solvent, extrusion followed by dispersion-solubilization of the ground exudate into solvent, or jet-cooking or stirred autoclaving of an aqueous starch slurry followed by transfer into solvent. Intrinsic viscosities [η] and multiangle light-scattering measurements were made in 90% DMSO-H₂O. A Mark-Houwink relation, [η] = (0.28–1.2) M_w^{0.29 ± 0.04}, was obtained over a molecular weight range of ≈30–700 million. However, there was a large amount of scatter in the data when [η] were >140 mL/g. The power law relationship R_g ∝ M_w^0.41±0.04 was noted between radii of gyration and molecular weights. We infer from our data that over the entire range of M_w distributions, the amylopectin existed in solution as relatively compact molecules or aggregates and that in the higher molecular weight region, the size and possibly the shape of the “dissolved” amylopectin was highly sensitive to the method of dispersal and treatment.