Fine Structures of Amylose and Amylopectin from Large,Medium, and Small Waxy Barley Starch Granules

Amylose and amylopectin were prepared from large, medium, and small granule starches of classified waxy barley flour, and their fine structures were investigated. The amylose content had a wide distribution range (≈1.4–9.4%). Number‐average degrees of polymerization (DP_n) of the amyloses were similar among the samples (≈1,200–1,300). But number of chains per molecule (NC) decreased from the surface to the center (≈6–10 chains). DP_n of the amylopectins varied from 4,657 to 14,604; decreased in the order of large, medium, and small granules in same fractions of the grain; and increased from the surface layer to the center. Longest chains (LC) were not found in any of the amylopectin molecules. The large amylopectin molecule had more long chains and fewer A chains than the small molecule. The amylose content had definite effects on the transition temperature range and crystal formation of the starch granules. There were positive correlations between DP_n of the amylopectin and relative crystallinity (γ = +0.69) and enthalpy value (γ = +0.80), respectively. These findings may help to elucidate biosynthesis mechanism of starch.     

Amylopectin Staling of Cooked Milled Rices and Properties of Amylopectin and Amylose

Starches of waxy rices that showed varietal differences in hardness testing of cooked rice after amylopectin staling and high-amylose content (AC) rices differing in gel consistency (GC) and starch gelatinization temperature (GT) were studied to determine the factors related to varietal differences in amylopectin staling of cooked rice. Intermediate- and high-GT starches showed greater amylopectin staling of gelatinized rice by hardness testing values or differential scanning calorimetry (DSC) endotherm than did low-GT starches in both waxy and nonwaxy rices. Isoamylase-debranched amylopectins of waxy rices differed in the ratio of weight-average degree of polymerization (DP_w) fractions, but these fraction ratios were not simply related to differences in amylopectin staling of cooked rice. Among high-AC rices, amylopectin from low-GT starch was confirmed to have higher iodine affinity (2.3–2.5%) than amylopectin from intermediate-GT starches (1.7–1.8%), regardless of GC. Within high-AC starch of the same GT type, soft-GC rice corresponded with more A + B₁ DP_w 16–18 and less B₃ DP_w 150–200 fractions of debranched amylopectin and low DP_w of amylose. Amylopectin of amylose extender mutant of IR36 was confirmed to have a longer chain length than ordinary rice amylopectin: the debranched amylopectin has more B₂ DP_w 47–51 fraction, less A + B₁ DP_w fraction, but no B₄ fraction with DP_w > 200. Only high-AC amylopectin had debranched fraction with DP_w >120.     

Molecular Structure and Some Physicochemical Properties of Buckwheat Starches

The molecular structure and pasting properties of starches from eight buckwheat cultivars were examined. Rapid viscograms showed that buckwheat starches had similar pasting properties among cultivars. The actual amylose content was 16–18%, which was lower than the apparent amylose content (26–27%), due to the high iodine affinity (IA) of amylopectin (2.21–2.48 g/100 g). Amylopectins resembled each other in average chain‐length (23–24) and chain‐length distributions. The long‐chains fraction (LC) was abundant (12–13% by weight) in all the amylopectins, which was consistent with high IA values. The amyloses were also similar among the cultivars in number‐average DP 1,020–1,380 with 3.1–4.3 chains per molecule. The molar‐based distribution indicated that all the amyloses comprised two molecular species differing in molecular size, although the weight‐based distribution showed a single species. A comparison of molecular structures of buckwheat starches to cereal starches indicated buckwheat amylopectins had a larger amount of LC, and their distributions of amylose and short chains of amylopectin on molar basis were similar to those of wheat and barley starches.     

Physicochemical Properties and Molecular Structures of Starches from Millet (Pennisetum typhoides) and Sorghum (Sorghum bicolor L. Moench) Cultivars in Nigeria

Some physicochemical properties and molecular structures of starches from millet (Pennisetum typhoides, Doro and Gero) and sorghum (Sorghum bicolor, red and white) in Nigeria were examined. Starch granules of millet and sorghum were 3–14 μm and 4–26 μm in diameter, respectively. Millet cultivars had similar peak viscosities (204–205 RVU) on pasting, while sorghum showed similar minimum viscosities (155–156 RVU). The actual amylose content (%) calculated from iodine affinity (IA, g/100 g) was 20.1 and 21.4 for sorghum and 21.3 for millet. The IA of amylopectin was high (1.27–1.42) and its average chain lengths were 20–21 with β‐amylolysis limit of 56%. Amylopectins showed a polymodal molecular weight distribution on a molar basis. The distributions differed among the samples with a higher amount of larger molecules in Doro and red sorghum. Weight‐ and molar‐based distributions of debranched amylopectins on HPSEC were polymodal with weight‐based distribution showing presence of long chains. Peak DP values for A+B₁ and B₂+B₃ chain fractions were 13–16 and 42–43, respectively. The (A+B₁)/(B₂+B₃) ratio on molar basis (9.0–11.5) was similar to maize and rice amylopectins. Peak DP on molar‐based distribution for white sorghum and millet amyloses were similar (490–540) and the DP_n range was narrow (1,060–1,300), but weight‐based distribution profiles differed. The average chain lengths were 260–270 with 3.9–4.8 chains per molecule.     

Molecular and Gelatinization Properties of Rice Starches from IR24 and Sinandomeng Cultivars

The differences in pasting properties involving gelatinization and retrogradation of rice starches from IR24 and Sinandomeng cultivars during heating‐cooling processes were investigated using a Rapid Visco Analyser (RVA)and a dynamic rheometer. The results were discussed in relation to the molecular structure, actual amylose content (AC), and concentration of the starches. Generally, both starches possessed a comparable AC (≈11 wt%), amylose average chain length (CL), iodine absorption properties, and dynamic rheological parameters on heating to 95°C at 10 wt% and on cooling to 10°C at higher concentrations. In contrast to Sinandomeng, IR24 amylose had a greater proportion of high molecular weight species and number‐average degree of polymerization (DP_n). IR24 amylopectin possessed a lower DP_n and greater CL, exterior CL (ECL), and interior CL (ICL). Comparing the results of RVA analysis and dynamic rheology, the gelatinization properties and higher retrogradation tendencies of IR24 starch can be related to the structural properties and depend on starch concentration. In addition, the exponent n of starch concentration for storage moduli at 25°C (G′₂₅ ∝ Cⁿ) increased linearly with increasing AC.     

Effects of Amylopectin Branch Chain Length and Amylose Content on the Gelatinization and Pasting Properties of Starch

Structures and properties of starches isolated from different botanical sources were investigated. Apparent and absolute amylose contents of starches were determined by measuring the iodine affinity of defatted whole starch and of fractionated and purified amylopectin. Branch chain-length distributions of amylopectins were analyzed quantitatively using a high-performance anion-exchange chromatography system equipped with a postcolumn enzyme reactor and a pulsed amperometric detector. Thermal and pasting properties were measured using differential scanning calorimetry and a rapid viscoanalyzer, respectively. Absolute amylose contents of most of the starches studied were lower than their apparent amylose contents. This difference correlated with the number of very long branch chains of amylopectin. Studies of amylopectin structures showed that each starch had a distinct branch chain-length distribution profile. Average degrees of polymerization (dp) of amylopectin branch chain length ranged from 18.8 for waxy rice to 30.7 for high-amylose maize VII. Compared with X-ray A-type starches, B-type starches had longer chains. A shoulder of dp 18–21 (chain length of 6.3–7.4 nm) was found in many starches; the chain length of 6.3–7.4 nm was in the proximity of the length of the amylopectin crystalline region. Starches with short average amylopectin branch chain lengths (e.g., waxy rice and sweet rice starch), with large proportions of short branch chains (dp 11–16) relative to the shoulder of dp 18–21 (e.g., wheat and barley starch), and with high starch phosphate monoester content (e.g., potato starch) displayed low gelatinization temperatures. Amylose contents and amylopectin branch chain-length distributions predominantly affected the pasting properties of starch.     

Comparison of Physicochemical Properties and Structures of Sugary‐2 Cornstarch with Normal and Waxy Cultivars

Starches from normal, waxy, and sugary‐2 (su2) corn kernels were isolated, and their structures and properties determined. The total lipid contents of normal, waxy, and su2 corn starches were 0.84, 0.00, and 1.61%, respectively. Scanning electron micrographs showed that normal and waxy corn starch granules were spherical or angular in shape with smooth surfaces. The su2 starch granules consisted of lobes that resembled starch mutants deficient in soluble starch synthases. Normal and waxy corn starches displayed A‐type X‐ray patterns. The su2 starch showed a weak A‐type pattern. The chain‐length distributions of normal, waxy, and su2 debranched amylopectins showed the first peak chain length at DP (degree of polymerization) 13, 14, and 13, respectively; second peak chain length at DP 45, 49, and 49, respectively; and highest detectable DP of 80, 72, and 76, respectively. The su2 amylopectin showed a higher percentage of chains with DP 6–12 (22.2%) than normal (15.0%) and waxy (14.6%) amylopectins. The absolute amylose content of normal, waxy, and su2 starches was 18.8, 0.0, and 27.3%, respectively. Gel‐permeation profiles of su2 corn starch displayed a considerable amount of intermediate components. The su2 corn starch displayed lower gelatinization temperature, enthalpy change, and viscosity; a significantly higher enthalpy change for melting of amylose‐lipid complex; and lower melting temperature and enthalpy change for retrograded starch than did normal and waxy corn starches. The initial rate of hydrolysis (3 hr) of the corn starches followed the order su2 > waxy > normal corn. Waxy and su2 starches were hydrolyzed to the same extent, which was higher than normal starch after a 72‐hr hydrolysis period.     

Structural Characteristics,Properties, and In Vitro Digestibility of Rice

Using rice samples derived from normal rice cultivars and endosperm starch mutant, we investigated key factors contributing to the enzyme digestibility of steamed rice grains. The chemical composition of polished rice grains, structural features of endosperm starch, and enzyme digestibility of steamed rice grains were examined. The protein content of polished rice grains was 4.6–9.1%, amylose content was 4–27%, the DP_n of purified amylose was 900–1,600, the amylopectin short/long chain ratio was 1.2–5.9, and the enzyme digestibilities of steamed polished rice grains were 0.9–12.6 °Brix. Amylose content and RVA parameters (viscosity, breakdown, and setback) correlated significantly with enzyme digestibility of steamed rice grains. Multiple regression formulas were constructed to predict digestibility of steamed rice grain as a function of the molecular characteristics of the starch. When both amylose content and the short/long chain amylopectin ratio were used as predictor variables, they accounted for >80% of the observed variance in digestibility of steamed rice grains. Multiple regression revealed that the more digestible rice samples had starch with a lower amylose content and more short‐chain amylopectin. Reassociation of amylose‐lipid complex and recrystallization of amylopectin in the stored steamed rice grains was monitored by differential scanning calorimetry (DSC), and the observed retrogradation properties were related to the structural characteristics of starch and to the enzyme digestibility of steamed rice grains.     

Structures and physicochemical properties of six wild rice starches

Starches from six wild rice cultivars were studied for their chemical structures and physicochemical properties and compared with a long-grain rice starch. The six wild rice starches were similar in morphological appearance, X-ray diffraction patterns, swelling power, and water solubility index but different in amylose content, beta-amylolysis limit, branch chain length distribution, thermal properties, and pasting properties. The structure of the wild rice amylopectins was close to that of waxy rice amylopectin with more branching and a larger proportion of short branch chains of degree of polymerization 6-12 as compared with that of amylopectin from rice starch with a similar amylose content. The differences in branch chain length distribution of amylopectin and amylose content were assumed to contribute to the differences in physicochemical properties among the six wild rice starches as well as to the differences between the wild rice starches and the rice starch.     

Effect of Growth Location in the United States on Amylose Content,Amylopectin Fine Structure,and Thermal Properties of Starches of Long Grain Rice Cultivars

Starch was isolated from kernels of 27 rice samples consisting of nine U.S. long grain rice cultivars grown in three different locations (Missouri, Arkansas, Texas). Amylose (AM) content of the starches and the fine structure of the respective amylopectin (AP) were determined and used to explain differences observed in gelatinization properties. The AM content of rice cultivars grown at the lower temperature Missouri location increased 0.4–3% and 0.5–4% when compared with the same rices grown in Arkansas and Texas, respectively. AP values of the rice samples were isolated, debranched, and separated by low‐pressure size‐exclusion chromatography. The eluted AP linear chains were divided into three fractions to represent extra long (FrI), long (FrII), and short chains (FrIII). The corresponding average degree of polymerization (DP_n) at the peaks of fractions FrI, FrII, and FrIII were 100, 39, and 16, respectively. Total carbohydrate analysis of the fractions indicated that cultivars grown in Missouri had a consistently higher proportion of FrIII and lower proportion of FrII as the same cultivars grown in Arkansas and Texas. Furthermore, the Missouri samples showed a shift toward shorter DP_n in FrII and FrIII and had more of the shortest chain components (DP_n < 6) of AP. The proportion of FrI did not follow a trend and varied depending on the cultivar and across location. Thermal analysis indicated that the higher temperature growth environments (Arkansas and Texas) resulted in higher onset, peak, and heat of gelatinization for the starches, suggesting longer cooking time and higher heat requirement. Overall, the data support the nonfield findings of other researchers that higher growing temperature results in AP with more DP_n short chains that are within a range of DP >10 to form consistent crystallites, and thus results in higher gelatinization temperatures and enthalpies.     

Correlations Between the Fine Structure,Physicochemical Properties,and Retrogradation of Amylopectins from Taiwan Rice Varieties

Fourteen varieties of rice from Taiwan, including five Indica, five Japonica, and four waxy cultivars, were used in this study for the examination of fine structure and physicochemical properties of amylopectin. The results indicated that the amylopectin of Indica rice had lower molecular weight, lower average degree of polymerization (DP), and lower average chain number when compared to Japonica and waxy varieties. The shortest average DP was 6 glucose units for all 14 rice varieties. The average chain lengths (CL) of amylopectin were 18–22, 15–18, and 17–20 for Indica, Japonica, and waxy rice, respectively. Indica varieties with high amylose content had amylopectin that comprised a few extra long chains (DP >100). The CL distribution profiles of amylopectins for these 14 varieties could be divided into two factions: CL 10–15 and CL 40–44. Amylopectin of the Indica rice had a relatively high blue value and λ_max, implying that a high proportion existed as long branches. The amylopectin of three Indica varieties with lower DP exhibited higher intrinsic viscosity, which might be attributed to the more elongated rod conformation of the few extra long chain amylopectins. The proportion of short chains with DP 6–9 glucose units seemed to influence the rate of the retrogradation of amylopectins.     

Properties of Starches from Several Low‐Amylose Rice Cultivars

The starch properties of five low‐amylose rice cultivars, Yawarakomachi, Soft 158, Hanabusa, Aya, and Snow Pearl, were compared with those of two normal amylose rice cultivars, Nipponbare and Hinohikari. There were no large differences in the distributions of the amylopectin chain length determined by high‐performance anion‐exchange chromatography, and the starch gelatinization properties determined by differential scanning calorimetry, between normal and low‐amylose rice cultivars. Results obtained using rapid viscosity analysis indicated that low‐amylose rice starches had lower peak viscosity, breakdown, and setback values than normal amylose rice starches. Starch granules from low‐amylose rice cultivars had a higher susceptibility to glucoamylase than those from normal amylose rice cultivars. The results of this study showed some differences between normal and low‐amylose rice starches in pasting properties and enzymatic digestibility.     

Composition,Molecular Structure,Properties, and In Vitro Digestibility of Starches from Newly Released Canadian Pulse Cultivars

Pulse starches were isolated from different cultivars of pea, lentil, and chickpea grown in Canada under identical environmental conditions. The in vitro digestibility and physicochemical properties were investigated and the correlations between the physicochemical properties and starch digestibility were determined. Pulse starch granules were irregularly shaped, ranging from oval to round. The amylose content was 34.9–39.0%. The amount of short A chains (DP 6‐12) of chickpea starch was much higher than the other pulse starches, but the proportions of B1 and B2 chains (DP 13‐24 and DP 25‐36, respectively) were lower. The X‐ray pattern of all starches was of the C type. The relative crystallinity of lentil (26.2–28.3%) was higher than that of pea (24.4–25.5%) and chickpea starches (23.0–24.8%). The swelling factor (SF) in the temperature range 60–90°C followed the order of lentil ≈ chickpea > pea. The extent of amylose leaching (AML) at 60°C followed the order of pea ≈ chickpea > lentil. However, in the temperature range 70–90°C, AML followed the order of lentil > pea > chickpea. The gelatinization temperatures followed the order of lentil > pea > chickpea. The peak viscosity, setback, and final viscosity of pea starch were lower than those of the other starches. Lentil starch exhibited lower rapidly digestible starch (RDS) content, hydrolysis rate, and expected glycemic index (eGI). The resistant starch (RS) content of both lentil cultivars was nearly similar. However, pea and chickpea cultivars exhibited wide variations in their RS content. Digestibility of the pulse starches were significantly correlated (P < 0.05) with swelling factor (60°C), amylose leaching (60°C), gelatinization temperature, gelatinization enthalpy, relative crystallinity, and chain length distribution of amylopectin (A, B1, and B2 chains).     

Changes in Retrogradation Properties of Rice Starches with Amylose Content and Molecular Properties

The increases in storage modulus (G′), retrogradation enthalpy change (ΔH) and ΔH‐related Avrami kinetic parameters of gelatinized rice starch dispersions at 25% (w/w) were investigated with respect to storage period, amylose content (AC), and molecular properties. Three high‐AC and five low‐AC rice cultivars were compared for understanding the multiple influences of AC and molecular properties involved. After refining the results of correlation analysis, the G′ of just‐cooled samples changed positively, mainly with AC and additionally with the average chain length of amylose (CL_AM) and the weight ratio of extra‐long plus long chains to short chains of amylopectin (AP) (r_APchain). The developed ΔH on short‐term storage (10 days) elevated with increasing AC and CL_AM and decreasing degree of polymerization of AP (DP_AP), but after long‐term aging for one to three months with increasing r_APchain, especially for the low‐AC cultivars examined. Greater Avrami rate constants for retrogradation could be attributed to the combination of a lower DP_AP and r_APchain or AP chain length and a greater CL_AM. The polynomials using these critical factors to describe the retrogradation parameters were elucidated and could account for 85–99.6% of data deviations.     

Structural and Retrogradation Properties of Rice Endosperm Starch Affect Enzyme Digestibility of Steamed Milled-Rice Grains Used in Sake Production

Structural and physicochemical characteristics of endosperm starch from milled rice grains of seven Japanese cultivars used in sake production were examined. Amylose content was 15.2–20.2%, number-average degree of polymerization (DP_n) of amylose was 900–1,400, and the ratio of short-to-long chain amylopectin was 2.7–3.5, respectively. The degree of retrogradation of purified starch stored for seven days at 4°C after gelatinization was 20–31%. The degree of retrogradation correlated negatively with the ratio of short-to-long chain amylopectin. The effect of holding time after steaming on enzyme digestibility and starch retrogradation of steamed rice grains was investigated. The longer the holding time after steaming, the greater the extent of retrogradation, and the less the degree of enzymatic digestibility. The decreased rate of enzyme digestibility correlated with amylopectin chain length distribution. Samples with short-chain amylopectin exhibited a slow decrease in enzyme digestibility. It was determined that the structure and retrogradation properties of endosperm starch in Japanese rice cultivars affect the decreasing rate of enzyme digestibility of the steamed, milled rice grains.     

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.     

Unit and Internal Chain Profile of Millet Amylopectin

The unit chain compositions of debranched foxtail, proso, pearl, and finger millet amylopectins and their ϕ,β‐limit dextrins were analyzed by high‐performance anion‐exchange chromatography. The ϕ,β‐limit dextrins reflected amylopectin internal chain profiles. The amylopectins had average chain lengths ranging from 17.94 to 18.12. The ranges of external chain length, internal chain length, and total internal chain length of the millet amylopectins were 11.85–12.33, 4.75–5.09, and 11.64–12.28, respectively. The relative molar concentration of B‐chains in the amylopectins was close to 50% in all samples. Significant differences were, however, observed in the proportions of very short “fingerprint” B‐chains (B_fp, degree of polymerization 3–7) and the major group of short B‐chains (BS_major): foxtail and proso millets possessed high amounts of B_fp‐chains, whereas finger and pearl millets had higher amounts of BS_major‐chains, suggesting possible differences in the fine structure of the clusters and building blocks of the amylopectins. Millet amylopectin can be classified structurally as type 2.     

Molecular Size Distribution and Amylase Resistance of Maize Starch Nanoparticles Prepared by Acid Hydrolysis

The molecular size distribution of maize starch nanoparticles (SNP) prepared by acid hydrolysis (3.16M H₂SO₄) and their amylase‐resistant counterparts, before and after debranching, was investigated. The weight average molecular weight (M_w) and linear chain length distribution were determined by high‐performance size‐exclusion chromatography (HPSEC) and high‐performance anion‐exchange chromatography (HPAEC), respectively. The objective was to understand the role of amylose involvement in the formation of SNP showing different crystalline structures (A‐ and B‐types). The HPSEC profiles of SNP before debranching from waxy, normal, and high‐amylose maize starches showed broad monomodal peaks. Debranched SNP from waxy maize eluted in a single narrow peak, whereas those from nonwaxy starches showed a multimodal distribution. Similar trends were also observed for the chain length distribution patterns, for which the longest detectable chains (degree of polymerization [DP] 31) in waxy maize were significantly lower than those of nonwaxy maize starches (DP 55–59). This indicated the potential amylose involvement in the SNP structure of normal and high‐amylose starches. Further evidence of amylose involvement was ascribed to the resistance of SNP toward amylolysis (Hylon VII > Hylon V > normal > waxy). The amylase‐resistant residues of SNP from high‐amylose maize starches were composed of both low M_w linear and branched chains.     

Observations on the α‐Amylolysis Pattern of Some Waxy Maize Starches from Inbred Line Ia453

Maize starches of the endosperm mutants waxy (wx), dull:waxy (duwx), and amylose‐extender:dull:waxy (aeduwx) from inbred line Ia453 lack amylose. However, in addition to high molecular weight (HMW) amylopectin, the duwx and aeduwx starches contained 40 and 80%, respectively, intermediate branched material of low molecular weight (LMW). As gelatinized, the amylopectin of the wx starch was easily hydrolyzed into small dextrins by the α‐amylase of B. amyloliquefaciens, but components of duwx and aeduwx possessed partial resistance to amylolytic attack. Residual material of intermediate size obtained by a 4‐hr α‐amylolysis could not be separated from LMW dextrins by fractional precipitation in methanol. It is suggested that this material possessed a more regularly branched structure, in which the d ‐glucosyl chain segments were too short to allow α‐amylase action. The granular starches of duwx and aeduwx genotypes were initially considerably more resistant than the wx sample to α‐amylase attack. This was possibly due to an altered structure in the amylopectin component or the high content of intermediate material in the former granules.     

Solubilization Effects on Molecular Weights of Amylose and Amylopectins of Normal Maize and Barley Starches

Structural characteristics of starches have been important to determine their physicochemical and functional properties. Solubilization procedures were tested to find a higher solubilization percentage and thereafter to study the structural characteristics of amylose and amylopectin. Size‐exclusion chromatography with refractive index (SEC‐RI) system using a pullulan standard curve was tested to study the amylose molar mass. Also, a microbatch system using a MALLS detector was used to determine the molar mass and gyration radius of starch and amylopectin. Microwave heating produced higher solubility percentages than autoclaving, and there was a difference between both starches. The sample solubilized with microwave heating presented higher molar mass and gyration radius values than autoclave samples, showing that this process for structural studies provided information representative of the initial starch sample. When starch components were separated, amylose showed lower purity than amylopectin. Lower purity was obtained for amylose separated from barley starch, but no difference was obtained for purity of amylopectin separated from both starches. Barley amylopectin had a higher solubility percentage than maize amylopectin. Molar mass of barley amylose was 1.03 × 10⁵ g/mol and for maize of 2.25 × 10⁵ g/mol. Molar mass values of amylopectin separated from both starches were lower than the starch counterparts, although the same solubilization procedure (microwave heating) was used. The difference might be due to depolymerization during separation of starch components.