Wet‐Milling and Dry‐Milling Properties of Dent Corn with Addition of Amylase Corn

A transgenic corn (amylase corn) has been developed that produces an endogenous α‐amylase that is activated in the presence of water and elevated temperature (>70°C). Wet‐ and dry‐milling characteristics of amylase corn were evaluated using laboratory wet‐ and dry‐milling procedures. Different amounts of amylase corn (0.1–10%) were added to dent corn (with the same genetic background as the amylase corn) as treatments. Samples were evaluated for wet‐ and dry‐milling fraction yields using 1‐kg laboratory procedures. Milling yields for all amylase corn treatments were compared with the control treatment (0% amylase corn or 100% dent corn). No significant differences were observed in wet‐ and dry‐milling yields between the control and the 0.1, 1, and 10% amylase corn treatments. Most of the amylase activity (77%) in wet‐milling fractions was detected in the protein fraction. In dry‐milling, amylase activity (68.8%) was detected in endosperm fractions (fines, small grits, and large grits).     

Effects of Selected Harvest Moistures and Frozen Storage Times on Selected Yellow Dent Corn: Wet‐Milling Yields and Starch Pasting Properties

The effects of harvest moistures and frozen storage times on corn wet‐milling yields and the pasting properties of the resulting starch were studied. Pioneer hybrid P‐0916‐XR harvested at three moisture contents (49, 35, and 21% wb) were stored frozen for three days or for five months, followed by wet‐milling. The pasting properties of the resulting starch were evaluated with a Rapid Visco Analyzer. The yields of starch and germ increased by 1.2 and 1.9 percentage points, respectively, when harvest moisture decreased from 49 to 21% wb, whereas the yields of steep water solids, total fiber, and gluten decreased by 2.1, 0.7, and 0.6 percentage points, respectively. The frozen corn had lower coarse fiber yields but higher cellular fiber yields. The starch pasting properties showed that peak and breakdown viscosities decreased by 8% (3,824 ± 36 versus 3,520 ± 38 cP) and 13% (2,336 ± 47 versus 2,029 ± 60 cP), respectively, when harvest moisture decreased from 49 to 21% wb, whereas peak time increased by 5% (6.32 ± 0.06 versus 6.62 ± 0.07 min). The setback and final viscosities of starch from long‐term frozen storage (five months) were 14% (1,574 ± 65 versus 1,828 ± 79 cP) and 8% (3,063 ± 27 versus 3,317 ± 101 cP) lower, respectively, than that from control (unfrozen) corn.     

Effect of Steeping with Sulfite Salts and Adjunct Acids on Corn Wet‐Milling Yields and Starch Properties

Two corn hybrids (3394 and 33R87) were steeped with three sulfite salts and five acids to test the effect of sulfur dioxide (SO₂) source and acid sources on wet‐milling yields and starch properties. Milling yields from each treatment were compared with a control sample that was steeped with 2,000 ppm of SO₂ (using sodium metabisulfite) and 0.55% lactic acid. Sulfur dioxide sources were potassium sulfite, sodium sulfite, and ammonium sulfite; acids were acetic, hydrochloric, oxalic, phosphoric, and sulfuric. Starch yields were affected by the SO₂ source and steep acids but the effects were hybrid‐dependent. Different steep acids gave different starch yields when wet milled at the same pH. Among the acids tested, weak acids (lactic and acetic) tended to give higher starch yields compared with strong acids (hydrochloric, sulfuric, phosphoric, and oxalic). Some differences were observed with different sulfite salts and acids on starch pasting properties; however, there were no clear trends.     

Effect of Stress Cracks on Corn Wet‐Milling Yields

U.S. No. 2 yellow dent corn was randomly probe‐sampled from rail cars being shipped to a wet‐milling plant from a Corn Belt local elevator. The probe samples were blended together and kernels were sorted into four levels of stress cracks (0, 1, 2, or multiple). Each level of stress cracking was then laboratory wet‐milled in triplicate. The only statistically observed differences were in total fiber and in protein content of the gluten meal fraction. The starch yield difference between zero stress cracked corn and multiple stress cracked corn was smaller (0.8%) than would be expected if stress cracking were an indicator of damage to the wet‐milling characteristics of the corn.     

Effects of Maturity on Grain Quality and Wet‐Milling Properties of Two Selected Corn Hybrids

The effects of maturity on grain quality and wet‐milling properties were investigated for two hybrids of corn. Significant differences for hybrid and maturity were observed for all grain quality parameters. Test weight, absolute density, and thousand‐grain weight all increased as the corn matured. Kernel hardness increased and breakage susceptibility varied with increased maturity. Water uptake parameters decreased with maturity of the grain. The starch yield results from wet milling showed that the starch yield increased significantly within each cultivar in the early stages of grain maturity, but there were no significant differences between hybrids. Mathematical models using selected grain quality parameters accurately predicted trends in starch yield for the immature and mature corn samples in this study.     

Wet‐Milling Characteristics of 10 Lines from Germplasm Enhancement of Maize Project Compared with Five Corn Belt Lines

The use of corn (Zea mays L.) hybrids with high grain yield and starch extractability has steadily increased in the processing industry. In light of widespread corn seed industry participation in the Germplasm Enhancement of Maize Project (GEM), which seeks to enhance exotic germplasm, future hybrids may contain more exotic sources in genetic backgrounds. It is necessary to establish and monitor physical, compositional, and milling characteristics of the new exotic breeding materials to determine the processing value. The present study was conducted to determine the wet‐milling characteristics of a set of GEM lines compared with typical Corn Belt lines. Ten GEM lines introgressed with exotic materials from Argentina, Chile, Cuba, Florida, and Uruguay and previously identified as having different starch yields, three commercial inbred lines, and two public inbred lines (B73 and Mo17) were analyzed using both near‐infrared transmittance (NIT) and a 100‐g wet‐milling procedure. There were statistical differences (P < 0.05) in the yield of wet‐milled fractions (starch, fiber, gluten, and germ). The GEM lines AR16035:S19‐227‐1‐B and CUBA117:S1520‐562‐1‐B had similar or better starch yield and starch recovery than B73 and the other adapted inbred lines, indicating that they may be useful in improving the proportion of extractable starch present in kernels of hybrids. Residual protein levels in the starch and gluten fractions were 0.26–0.32% and 38–45%, respectively. The starch yield of GEM lines from wet milling correlated positively with starch content from NIT and was negatively correlated with protein content of the corn kernels. Oil content in the germ varied from 50 to 60%. Our results indicate that incorporating GEM lines in a breeding program can maintain or even improve wet‐milling characteristics of Corn Belt materials if lines with appropriate traits are used.     

Use of Proteases to Reduce Steep Time and SO2 Requirements in a Corn Wet‐Milling Process

To eliminate the diffusion barriers associated with enzyme addition during conventional steeping, we have developed a two‐stage milling procedure to evaluate the effects of enzyme addition on corn wet milling. The current study compares the effects of the addition of commercially available enzyme preparations during conventional steeping to their comparable addition in the two‐stage procedure. Results are presented in terms of yields of fiber, starch, germ, and gluten. The results demonstrate that the application of enzymes to the normal steeping step of wet milling is not an effective means of decreasing the steeping time or sulfur dioxide usage. Only when specific enzymes are added to the hydrated ground corn, using the modified two‐stage procedure, are enzymes effective in decreasing the steeping time and sulfur dioxide requirements. The overall steeping time with the two‐stage modified procedure ranges from 6 to 8 hr, representing a 67–83% reduction over the conventional process. The modified process greatly decreases, and possibly eliminates, the need for sulfur dioxide addition, while producing starch yields and quality equivalent to that from the conventional process.     

Intermittent Milling and Dynamic Steeping Process for Corn Starch Recovery

A procedure that reduces diffusional limitations by periodically milling the corn to reduce particle size and stirring the ground mash in the presence of sulfur dioxide (SO₂) and lactic acid was developed. The process, called intermittent milling and dynamic steeping (IMDS), includes three main stages: initial soaking (a short-time immersion in water) of whole kernels, initial cracking of the partially hydrated kernels, and dynamic steeping with interspersed milling. This study evaluated the three stages of the process separately, evaluating the effect of variables on each stage of the process. Corn fractions yield (germ, fiber, gluten, starch) were used to decide the best conditions for the soaking and steeping stages, and germ damage was used to determine the best kernel cracking method. Starch, gluten, and germ yields were not affected by soak temperatures (52–68°C) or soak time (1–3 hr). A temperature of 60°C was chosen for soaking because it increased the rate of kernel hydration without gelatinizing starch, which happens at higher temperatures. A 2-hr soak time was preferred because there was less fiber in the germ fraction and less germ damage was observed. Although there were no advantage to using SO₂ or lactic acid in the soak water, the presence of these compounds during dynamic steeping enhanced starch yield. The starch yield for 3 hr of dynamic steeping was not statistically different from the starch yield for a 7.5-hr dynamic steep. The Bauer mill was preferred over the use of a roller mill or a commercial grade Waring blender for kernel cracking. The IMDS process produced, on an average, 1 percentage point more starch than the conventional 36-hr steeping process. Total steep or kernel preparation time was reduced from 24–40 hr for conventional wet-milling to 5 hr for the IMDS process.     

Extrusion of Cross‐Linked Hydroxypropylated Corn Starches I. Pasting Properties

A series of cross‐linked (0, 0.014, 0.018, 0.024, and 0.028% POCl₃, dry starch basis) hydroxypropylated (8%) corn starches were extruded using a Leistritz micro‐18 co‐rotating extruder. Process variables included moisture, barrel temperature, and screw design. Differential scanning calorimetry and X‐ray diffraction studies showed the level of starch crystallinity decreased with increasing severity of extrusion conditions. Pasting properties of the extruded starches were examined using a Rapid Visco Analyser. Pasting profiles of starches extruded at different conditions displayed different hot paste viscosity and final viscosity. Increasing starch moisture content during extrusion and level of cross‐linking increased starch viscosity (P < 0.0001), whereas increasing extrusion temperature and shear decreased starch viscosity (P < 0.0001). Interactions were found between level of cross‐linking and screw design and between extrusion temperature and starch moisture content (P < 0.0001).     

Pasting Characteristics of Maize Starch Heat‐Treated with Different Water‐Ethanol Mixtures

Pasting characteristics of maize starch heat‐treated with six different water‐to‐ethanol ratios (%wt base 0:100, 10:90, 20:80, 30:70, 40:60, 50:50) were investigated; treated starches were called EW 0, 10, 20, 30, 40, and 50, respectively. Endotherms in DSC analysis shifted to a higher temperature as the water content in water‐ethanol mixture increased. The removed amount of fatty acids was much higher in treatments for EW 10, 20, and 30. The RVA peak viscosity of EW 10 and 20 were highest among the treated starches and setbacks were more than twice that of untreated starch. The characteristic change in the RVA viscogram corresponded to the amount of leached amylose from the granule. EW 30 displays similar properties as conventional heat‐moisture‐treated starch, but maintained a higher viscosity of ≈300 RVU throughout the heating process. In treatment with water‐ethanol mixtures, heat‐moisture treatment and defatting effects generated new types of modified starches. EW 40 and 50 had no clear pasting peak on RVA, and showed a viscosity at low temperature similar to granular cold water gelling.     

Phosphorus Concentrations and Flow in Maize Wet‐Milling Streams

Marketing of coproducts such as corn gluten meal (CGM) and corn gluten feed (CGF) is important to the maize wet‐milling industry. High phosphorus concentrations could lead to limited markets for CGF due to its potential to increase phosphorus in animal wastes. The objective was to measure the concentration and flow of phosphorus in the wet‐milling process and identify streams that could be altered. Samples were taken from 21 process streams of three facilities and the phosphorus content of each was determined. Flow of phosphorus was simulated using a computer model for a 2,700 tonne/day (105,000 bu/day) wet‐milling plant. Phosphorus concentrations of streams varied from <10 mg/kg to >14,000 mg/kg. Phosphorus content of many streams differed significantly among facilities. Flow of phosphorus (kg/day) varied dramatically among streams. However light steepwater, light gluten, and process water streams (5,960, 3,080, and 970 kg/day, respectively) accounted for much of the phosphorus flow. Modification of these streams could reduce phosphorus content of coproducts. The high phosphorus content of either CGF or CGM could be reduced markedly if phosphorus was reduced in the appropriate streams.     

Structure and Pasting Properties of Oat Starch

Following a period of declining food use, oats are now increasing in importance because of perceived nutritional benefits. The pasting properties of oat starch were regarded as similar to those of other cereal starches until the development of instruments with a more rapid mixing system than the amylograph showed characteristic differences in oats. These differences in pasting properties offer opportunities for novel products in both food and industrial areas. The structure, composition, and pasting properties of oat starch are reviewed, with particular emphasis on methods of measurement. Future directions of research in this area are suggested.     

Enzymatic Process for Corn Dry‐Grind High‐Solids Fermentation

A modified dry‐grind process that combined the use of conventional amylases (glucoamylase [GA]), phytase, and granular starch hydrolyzing enzymes (GSHE) to achieve low liquefaction viscosities and low glucose concentrations during simultaneous saccharification and fermentation (SSF) with a high slurry solids content (>33% w/w) was developed. Doses of GSHE and GA were optimized for the modified process. At 35% solids content, the modified process had 80% lower slurry viscosity, 24% lower peak glucose concentration, 7.5% higher final ethanol concentration, and 51% higher fermentation rate compared with the conventional dry‐grind process. At 40% solids content, the modified process had lower viscosities, lower peak and residual glucose concentrations, and higher ethanol concentrations than the conventional process; however, the results were in contrast to those for 35% solids content. At 40% solids content, SSF did not run to completion for conventional or modified processes, and more than 2.5% w/v of residual glucose was left in the fermentation broth. Final ethanol concentration achieved with the modified process at 40% solids content was 19.5% v/v, similar to the ethanol concentration achieved with the modified process at 35% solids content. At 35% slurry solids content, a GSHE level of 1.25 μL/g db of corn and a GA level of 0.25 μL/g db of corn were selected as optimum enzyme doses for the modified process.     

Morphologies and Thermal Properties of Hydroxypropylated High‐Amylose Corn Starch

High‐amylose (80%) corn starch was modified by hydroxypropylation with different molar substitution (MS). The unique microstructure of high‐amylose starch keeps its granules intact after hydroxypropylation. However, the microstructures and thermal properties strongly depend on the MS of hydroxypropylation. With increasing MS, the granule size was increased, which is partly due to disrupted granule structure, particularly in the amorphous region. Unlike normal starch, the modified high‐amylose corn starch showed a narrow gelatinization range measured by differential scanning calorimetry (DSC), which can be explained by destruction of amylose‐lipid complex. Internal microstructures and morphologies of hydroxypropylated starch were investigated using confocal laser scanning microscopy and to further explore the mechanism of chemical reaction and phase transitions.     

Effect of Laboratory Batch Steeping pH on Starch Yield and Pasting Properties of Selected Corn Hybrids

This study evaluated the effect of initial pH on percent of starch yield and pasting characteristics for a laboratory wet‐milling procedure. Four commercial hybrids, selected because they have significantly different starch yield values, were laboratory wet‐milled, and the pasting properties of the starch fractions were evaluated using a Rapid Visco Analyser (RVA). Percent starch yield (db) decreased when initial pH values were >4.0 but was unaffected by any lower initial pH values. The pasting properties of some of the selected hybrids were more sensitive to steepwater pH than others. There was an overall increase in peak, trough, and final viscosity as pH increased.     

Study of a Small‐Scale Laboratory Wet‐Milling Procedure for Wheat

The objectives of this research were to study the effects of slurry specific gravity, starch table slope, slurry pumping rate, and their interactions on starch recovery and purity; and to propose a small‐scale laboratory wet‐milling procedure for wheat. First‐order and second‐order response surface regression models were developed to study the effects and interactions of slurry specific gravity, starch table slope, and slurry pumping rate on starch and gluten separation for a 100‐g wheat wet‐milling procedure. The starch and starch protein content data fit the first‐order models (R² = 0.99 and 0.96) better than the second‐order models (R² = 0.98 and 0.93). Regression results from the first‐order models indicated that specific gravity, table slope, pumping rate, and their interactions all had a significant effect on starch yield and purity. However, these effects could be simplified as the effect of the resident time of starch and gluten slurry on the starch table and the specific gravity. Starch yield increased as resident time increased and specific gravity decreased. Protein content in starch decreased as the resident time decreased and the specific gravity increased. The separation condition with specific gravity of 3 Bé, table slope of 1.04 cm/m, and pumping rate of 50 mL/min was recommended. Under this condition, starch recovery was 85.6% and protein content of starch was 0.42%, which was similar to the 1.5‐kg laboratory methods in starch recovery. Total solids recovery was 98.1%, which is similar to that from 1.5‐kg laboratory methods. These results indicated that precision of the 100‐g wheat wet‐milling procedure was similar to that of the 1.5‐kg laboratory methods.     

Starch Pasting Properties and Amylose Content from 17 Waxy Barley Lines

Starch pasting properties and amylose content from 17 waxy barley lines (waxy gene originating from indigenous lines and an artificial mutant) were analyzed using rapid viscosity analysis (Rapid Visco Analyser [RVA]). Amylose contents varied from 0% (Shikoku‐hadaka 97) to 9.5% (Shikoku‐hadaka 96) compared with 30% for normal barley. Eight parameters were obtained from RVA profiles of these lines and correlation between each of these parameters and amylose content were evaluated. These parameters include pasting temperature (PT), peak viscosity (PV), temperature at PV, minimum viscosity (MV), final viscosity (FV), breakdown (BD), setback (SB), and time maintained at >80% PV (hot paste stability [HPS]). Significant correlations (0.64 and 0.61) were found between amylose content and FV and SB, respectively. High correlation (0.72) was found between amylose content and temperature at PV. HPS calculated from RVA profiles showed the highest correlation (0.79) to amylose content. Outer part of barley grains contained higher amounts of amylose than the inner part. There was a tendency that both PT and FV positively correlated to the amylose content of these parts.     

Variation Among Physical,Compositional, and Wet‐Milling Characteristics of the F1 Generation of Corn Hybrids of Introgressed Exotic and Adapted Inbred Lines

Hybrids with high grain yield and higher starch, protein, or oil content are available to corn growers; however, they result from crossing adapted Corn Belt inbred lines that rarely include exotic germplasm. This study was conducted to determine whether Corn Belt lines introgressed with exotic materials from Argentina, Chile, Uruguay, Cuba, and Florida have appropriate wet‐milling characteristics in their hybrids. Ten lines from the Germplasm Enhancement of Maize (GEM) project with different starch contents were crossed to three adapted inbred lines used as testers. The B73×Mo17 hybrid was used as a control. The F₁ generation of these 30 experimental hybrids was analyzed using both near‐infrared transmittance (NIT) technology and a 100‐g modified wet‐milling procedure, and measuring test and 1,000‐kernel weight. There was great variation among physical, compositional, and wet‐milling characteristics of the experimental hybrids, suggesting that exotic germplasm can be used to improve wet‐milling characteristics of Corn Belt hybrids.     

Rheological Properties of Dispersions of Spherulites from Jet‐Cooked High‐Amylose Corn Starch and Fatty Acids

High‐amylose corn starch was cooked in an excess‐steam jet cooker in the presence of 5% oleic or palmitic acid, based on amylose. The cooked product was rapidly cooled in an ice bath and then freeze‐dried or drum‐dried. Amylose was removed from solution by forming helical inclusion complexes with the fatty acid, and the inclusion complexes formed submicron spherical particles upon cooling. The dried material was reconstituted to form a paste that exhibited gel‐like properties upon standing, but that flowed readily when shear was applied. The rheological properties of these pastes were measured to determine the effects on the flow properties of 1) the solids concentration in the reconstituted paste, 2) the method of sample drying and reconstitution, and 3) the fatty acid used. The materials were very spreadable, and at the highest concentrations their flow properties were similar to a commercial shortening. The pasting properties of the dried solids were also examined.