CN115052904A - Ultrafine starch or grain-based flour compositions and related methods - Google Patents

Ultrafine starch or grain-based flour compositions and related methods Download PDF

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Publication number
CN115052904A
CN115052904A CN202080095151.3A CN202080095151A CN115052904A CN 115052904 A CN115052904 A CN 115052904A CN 202080095151 A CN202080095151 A CN 202080095151A CN 115052904 A CN115052904 A CN 115052904A
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China
Prior art keywords
screw
starch
flour
shear
high shear
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Pending
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CN202080095151.3A
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Chinese (zh)
Inventor
亚历山德拉·桑伯恩
阿里·阿尤布
希琳·巴塞尔
阿里·哈拉普尔
巴吉特·哥特拉
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Archer Daniels Midland Co
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Archer Daniels Midland Co
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/14Cold water dispersible or pregelatinised starch
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/212Starch; Modified starch; Starch derivatives, e.g. esters or ethers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L7/00Cereal-derived products; Malt products; Preparation or treatment thereof
    • A23L7/10Cereal-derived products
    • A23L7/198Dry unshaped finely divided cereal products, not provided for in groups A23L7/117 - A23L7/196 and A23L29/00, e.g. meal, flour, powder, dried cereal creams or extracts
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/40Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
    • A23P10/43Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added using anti-caking agents or agents improving flowability, added during or after formation of the powder
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P30/00Shaping or working of foodstuffs characterised by the process or apparatus
    • A23P30/20Extruding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/30Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B29B7/482Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws provided with screw parts in addition to other mixing parts, e.g. paddles, gears, discs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/30Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B29B7/488Parts, e.g. casings, sealings; Accessories, e.g. flow controlling or throttling devices
    • B29B7/489Screws
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/022Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50Details of extruders
    • B29C48/505Screws
    • B29C48/507Screws characterised by the material or their manufacturing process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50Details of extruders
    • B29C48/505Screws
    • B29C48/54Screws with additional forward-feeding elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/16Apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L3/00Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08L3/02Starch; Degradation products thereof, e.g. dextrin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2303/00Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08J2303/02Starch; Degradation products thereof, e.g. dextrin

Abstract

A method of forming an ultrafine starch/flour product comprising at least one of (a) or (b), wherein (a) comprises heating a mixture of water and native/modified starch/flour and extruding the mixture with a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw in series to produce an extrudate. Step (b) comprises forming a mixture of water, lipid and native/modified starch/flour and drying the mixture to produce a dried lipid starch/flour intermediate. The starting starch/flour may be milled before or after step (a) or (b). The ultra fine starch/flour particle product has a higher water solubility than a starch/flour particle product produced with a screw configuration without a high shear mixing screw or a starch/flour intermediate produced in the absence of the lipid in (b). In one embodiment, the method is free of chemical or enzymatic reactions.

Description

Ultrafine starch or grain-based flour compositions and related methods
Technical Field
The present invention relates to a starch or grain based flour composition and related methods.
Background
Starch and grain-based flours are naturally occurring ingredients made from agricultural raw materials. Starch is industrially refined by grinding, sieving and drying. Native starch is present in crystalline microscopic particles held together by molecular association. These particles typically have poor solubility in cold water and high viscosity upon gelatinization. These poor solubility and high viscosity characteristics limit the use of native starch and/or require further chemical modification. Starch granules, and more specifically starch granules, have received commercial attention because starch is environmentally friendly, and have been suggested as a promising ingredient in a variety of fields including food, beverages, coatings, cosmetics and pharmaceuticals, as well as various composite materials as used in food and industrial applications.
Various processes have been proposed for producing starch granules of submicron size. U.S. Pat. No. 6,677,386 discloses a chemical reaction extrusion process for preparing biopolymer nanoparticles, in which a biopolymer is plasticized using shear forces and a crosslinking agent is added during processing. The patent discloses that exemplary crosslinking agents are dialdehydes and polyaldehydes, which reversibly form hemiacetals, anhydrides, and mixed anhydrides (e.g., succinic anhydride and acetic anhydride), among others. The patent discloses that suitable dialdehydes and polyaldehydes are glutaraldehyde, glyoxal, periodate-oxidized carbohydrates, and the like, and that glyoxal is a particularly suitable cross-linking agent. This patent describes ultrafine starch particles, aqueous dispersions of said particles and extrudates prepared by this process.
PCT international patent publication No. WO00/40617 discloses a process for the preparation of starch granules using a two-phase system, wherein the process comprises a) preparing a first phase comprising a dispersion of starch in water, b) preparing a dispersion or emulsion of the first phase in a second liquid phase, with the proviso that the second phase is not water, c) cross-linking the starch present in the first phase, d) isolating the starch granules thus formed. Examples of the disclosed crosslinking agent include epichlorohydrin, glyoxal, sodium trimetaphosphate, phosphorus oxychloride, or anhydrides of di-or polycarboxylic acids.
U.S. patent No. 9,828,441 discloses a process for preparing extruded pregelatinized, partially hydrolyzed starch using an acid in an aqueous environment.
U.S. patent 9,510,614 discloses a low shear process for processing soluble whole oat flour (whole grain). The enzyme-treated oat flour is prepared by mixing a whole oat flour starting mixture and a suitable enzyme solution in a mixer (sometimes referred to as a preconditioner) and then heat treating the mixture. The enzyme treated mixture is then subjected to an extrusion process to gelatinize, hydrolyze and cook the oat flour mixture. This patent discloses applying low shear to the mixture in an extruder. The patent discloses that the process does not require high shear because the enzyme has preconditioned the starch. This patent discloses that high shear makes it difficult to control the degree of hydrolysis and also excessively raises the dough temperature, which can overcook the dough, resulting in too overcooked grain flavor. This patent discloses that the low shear extrusion process is characterized by a high moisture and low shear screw design relative to a low moisture and high shear screw design, and that the typical screw speed for the low shear process is 200-350 rpm.
CN102870853 discloses a soybean flour having a particle size of 6.5 μm. ltoreq. D <13 μm. The document indicates that soybean powder is obtained by pulverizing soybeans, and ultra-fine soybean powder is a soybean product obtained by extracting soybean oil, followed by mainly pressing and extracting soybean meal, and then by jet milling. The document indicates that ultra-fine soy flour has better solubility and is more easily absorbed and digested by the human body. This document discloses a bean-based nutritional meal prepared by using ultra-fine soybean powder as a main raw material, and the raw materials are all food grade.
One important limitation is that conventional processes for preparing starch granules for useful applications are complex and require toxic or hazardous organic solvents. For FDA purposes, products from such conventional processes are typically not considered label friendly and are typically not capable of being labeled "clean" in the food and other industrial fields. Other limitations of conventional methods include expensive techniques, which typically require the use of large amounts of solvents and/or high energy. Conventional processes include acidified water techniques that are difficult to control, and wherein the effects of temperature, time, concentration, acid strength, procedure and equipment affect the extent of starch granule modification. The treatment of starch with acid in turn requires the addition of large amounts of alkali for neutralization, which in itself causes considerable disadvantages and difficulties. Furthermore, the acidification method is not applicable to flour due to the presence of other components such as protein, fiber and ash. These components complicate the acid modification and negatively affect the product quality, thus making it unsuitable for commercial use.
Conventional processes produce products that lack suitably high stability and water solubility and often result in phase separation.
In addition to the above challenges facing the industry, there is now an increasing demand for non-chemically or non-enzymatically modified products. There is a need for a simple and reliable process for preparing non-chemically modified cereal/grain based flours and starches, and in particular ultrafine particles.
Disclosure of Invention
The present invention provides advantages over conventional processes and products. In one aspect, a method of forming ultrafine (also referred to as submicron) starch or flour particles includes mixing starch or degermed flour or a combination thereof with liquid water or steam or a combination thereof, thereby producing a mixture. As used herein, ultra-fine or sub-micron is used to characterize particles having a diameter of less than one millionth of a meter.
In one aspect, a method of forming an ultrafine starch or flour product includes at least one of steps (a) or (b). Step (a) comprises heating a mixture of water and native or modified starch or flour to a temperature in the range of from 25 ℃ to less than 200 ℃ and extruding the mixture with a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw in series to produce an extrudate. As used herein, modified starch or modified flour means a starch or flour derivative prepared by physically treating a native starch or flour to alter its properties.
Step (b) comprises forming a mixture of water, lipid and native or modified starch or flour and drying the mixture of water, lipid and native or modified starch or flour to produce a dried lipid starch intermediate or a dried lipid flour intermediate.
In one aspect, the method includes at least one of steps (c) or (d). Step (c) comprises milling the native or modified starch or flour to reduce the particle size of the native or modified starch or flour prior to step (a) or (b). Step (d) comprises breaking up the extrudate produced in (a), or breaking up the dried lipid starch intermediate or flour intermediate produced in (b), to produce an ultrafine starch or flour granule product with high water solubility compared to a starch or flour granule product produced in (a) where the extrusion of the mixture is with a screw configuration consisting of a low shear forward conveying screw and without a high shear mixing screw, or compared to a starch or flour intermediate produced in (b) without a lipid; wherein the method is free of chemical or enzymatic reactions. In one embodiment, the crushing of the extrudate produced in (a), or the crushing of the dried lipid starch intermediate or flour intermediate produced in (b) is by rolling, grinding or milling and combinations thereof.
In one aspect, the method includes heating the mixture to a temperature of 25 ℃ to less than 200 ℃, and extruding the mixture in a screw configuration to produce ultrafine starch granules without chemical or enzymatic reaction. In one aspect, the screw configuration comprises at least one low shear forward conveying screw and at least one high shear mixing screw in series. In one embodiment, the ultrafine (i.e., submicron) starch or flour particles have high water stability compared to starch or flour particles extruded with a screw configuration consisting of a low shear forward conveying screw and without a high shear mixing screw. In one aspect, the method is free of a pulverization step.
In one aspect, an apparatus includes a heat source and a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw section in series, wherein the heat source is configured to heat a mixture of starch or degermed flour or a combination thereof and water to a temperature of from 25 ℃ to less than 200 ℃, wherein the screw configuration is configured to extrude the mixture to produce ultrafine starch granules without chemical or enzymatic reaction as compared to starch or flour granules extruded with a screw configuration consisting of a low shear forward conveying screw and without a high shear mixing screw. In one aspect, the device is free of a comminution device.
In one aspect, an ultrafine starch or cereal-based particle extruded product comprises ultrafine starch or cereal-based particles characterized by a peak size of about 0.12 μm at a bulk density of about 4%, wherein the extruded product preferably does not contain chemical or enzymatic reactants.
In one aspect, an ultrafine starch or grain-based particle extruded product comprises ultrafine starch or grain-based particles characterized by a percent solubility in water in the range of about 75% to 95% for at least 48 hours.
In one aspect, a method includes mixing extruded ultrafine starch particles with water to produce an aqueous solution substantially free of phase separation.
In one aspect, a starch or grain-based flour comprises ultrafine particles having high solubility and stability in aqueous solutions.
In one aspect, a starch or grain-based flour comprises ultrafine particles having high solubility and stability in an oil solution.
In one aspect, an aqueous solution comprises a starch or grain-based flour comprising ultrafine particles free of chemical or enzymatic reactants.
In one aspect, a method includes forming a particulate starch product by using a non-chemically or non-enzymatically modified feed source subjected to mechanical force and shear by mixing starch with water. The present invention provides a process by extrusion at a temperature of 25 ℃ to below 200 ℃ during processing, which surprisingly results in a product exhibiting high solubility and which can be carried out without the use of any additives. In particular, the process need not be carried out under acidic or alkaline conditions or in the presence of chemical additives and/or enzymes.
In one aspect, a method of forming an ultrafine starch or flour product comprises (a) forming a mixture of water, lipid, and natural or modified starch or flour and drying the mixture of water, lipid, and natural or modified starch or flour to produce a dried lipid starch intermediate or a dried lipid flour intermediate; and at least one of step (b) or (c), wherein (b) precedes step (a) and comprises milling the native or modified starch or flour to reduce the particle size of the native or modified starch or flour; wherein (c) comprises breaking the dried lipid starch intermediate or flour intermediate produced in (a) to produce an ultrafine starch or flour granule product having high water solubility as compared to the starch or flour intermediate produced in the absence of lipid in (b). In one embodiment, the method is free of chemical or enzymatic reactions.
In one aspect, the present invention relates to a novel starch or cereal based flour composition consisting of unique ultrafine particulate matter having unique solubility and stability in aqueous systems. The design and use of the process parameters of the present disclosure enables the formation of new and unique starch-based granules. The products and compositions produced by the processes disclosed herein can be used in a variety of fields, including the fields of pharmaceuticals, cosmetics, coatings, and polymer compositions. In particular, the disclosed ultra-fine product compositions and subsequent powder properties may be used in certain food and beverage products with the following improvements and applications:
a. improving sensory and organoleptic functions in high moisture food systems.
b. Improved flavor, oil and micro/macro nutrient provision due to increased surface area and activity required in food and feed.
c. Improve the texture of certain food products (bread, biscuits, bars and gluten-free food products, etc.), wherein high solubility and stability confer better adhesion and texture functions.
d. Improve the solubility of carbohydrates and proteins to provide nutritional functions in food and feed.
e. Improve the composition of the particles for coating applications for paper and improve the adhesion required for products that replace latex and bioadhesives.
These and other aspects, embodiments and related advantages will become apparent from the following detailed description.
Drawings
FIG. 1 illustrates a portion of a low shear conveyor screw according to an aspect of the present invention.
Fig. 2 illustrates a portion of a high shear mixing screw in accordance with aspects of the present invention.
FIG. 3 illustrates a portion of two parallel three-flighted conical screws in accordance with aspects of the present invention.
FIG. 4 illustrates a portion of two parallel feed screws in accordance with aspects of the present invention.
Fig. 5 illustrates a portion of a positive feed Shearlock (Shearlock) screw in accordance with aspects of the present invention.
Fig. 6 illustrates a portion of a reverse lobe shear lock screw in accordance with aspects of the present invention.
Fig. 7 illustrates a screw configuration according to an aspect of the present invention.
Fig. 8 is a plot of bulk density (%) versus size grade (μm) illustrating the moisture particle size distribution of starch granules produced according to aspects of the present invention as compared to the moisture particle size distribution of native dent corn starch.
Fig. 9 is a graph of% solubility versus time illustrating the stability expressed as% solubility in Real Time (RT) for various particles produced according to aspects of the present invention.
Fig. 10 depicts a starch product produced according to aspects of the present invention.
Fig. 11 depicts a flour product produced according to aspects of the present invention that exhibits high solubility in aqueous solutions as compared to conventional flour products in aqueous solutions.
Fig. 12 depicts an X-ray diffraction (XRD) pattern of a corn starch sample made according to aspects of the present invention.
Detailed Description
Fig. 1 illustrates a portion of a low shear conveyor screw 100 according to an aspect of the present invention. The low shear conveyor screw 100 is located within a pipe or conduit (not shown). The low shear feed screw 100 is used to move or convey material through a pipe or tube. The low shear conveyor screw 100 has a helical surface 102 surrounding a central axis 104. The helical surface 102 includes external threads 106. The threads 106 are of the same size and are aligned in the same manner as each adjacent thread 106. The shaft surface 108 is located between adjacent threads 106. The material within the pipe or tube is moved through the pipe or tube by the low shear conveyor screw 100 as the low shear conveyor screw 100 rotates about the axis of the central shaft 104.
Fig. 2 illustrates a portion of an exemplary high shear mixing screw 200 in accordance with aspects of the present invention. The high shear mixing screw 200 is located within a tube or pipe (not shown) and has an asymmetric surface 202 surrounding a central axis 204. The asymmetric surface 202 includes threads 206 offset from each adjacent thread 206. As the high shear mixing screw 200 rotates about the axis of the central shaft 204, the material within the tube or pipe is mixed by the high mixing screw 200. In fig. 2, eight threads 206 are shown. However, more or fewer threads 206 may be used in embodiments of the invention.
Fig. 3 shows a portion of two parallel three-flight conical screws 300 in accordance with an aspect of the present invention.
Fig. 4 shows a portion of two parallel feed screws 400 combined in accordance with aspects of the present invention. Fig. 4 shows the two low shear conveying screws depicted in fig. 1, wherein the screws are aligned such that the flights 106 of one screw are aligned with the shaft surface 108 between the two flights 106 of the other screw.
Fig. 5 illustrates a portion of a forward-feeding lobed shear lock screw 500 in accordance with aspects of the present invention. When the conveying flights 106 as shown in fig. 1 throw work into the extrudate relatively slowly, the paddles (shear locks) of the lobed shear lock screw 500 throw work into the extrudate more quickly. Paddle 502 is an oval shaped piece that is a poor conveying element even though it is constructed as part of a set of elements arranged for "forward conveying". Forward feed is to align paddles 502 such that the general direction of travel of the longest dimension of the paddle (lobe) continues the direction of the conveying element. Neutral feed (not shown) is essentially to arrange the blades such that the lobes are offset by 90 degrees in cross-section from one blade to the next.
Fig. 6 illustrates a portion of a reverse-feeding flapper shear lock screw 600 in accordance with an aspect of the present invention. Reverse feeding is essentially arranging the paddles 602 so that the general direction of travel of the lobes is opposite to the direction of the conveying elements.
One of ordinary skill in the art having benefit of the present disclosure will recognize that blade 502 (shown in FIG. 5) and blade 602 (shown in FIG. 6) may be constructed in groups equal to 0.5D in length. Generally, for a length of 0.5D, one element block may be offset by 90 degrees, such that each paddle may be offset by 30 degrees from the upstream paddle for forward and reverse transport paddles. One skilled in the art will recognize that one way to observe the direction of conveyance of the paddles is to observe the top or bottom of the paddle set as it rotates in the extruder. If the "wave" that appears moves from left to right, the part is conveyed in the forward direction (the direction of extrudate flow). If the "wave" occurs from right to left, the part is transported in reverse (opposite to the direction of extrudate flow).
The present invention is more specifically illustrated by the following examples and comparative examples:
examples of the invention
Material
The non-chemical and non-enzymatic modification processes disclosed herein can be used to produce unique ultrafine starch microparticles from starch or degermed flour or a combination thereof and water or steam or a combination thereof. An exemplary, but non-limiting, dent corn starch is ADM 106 (Archer Daniels Midland). An exemplary de-embryonated flour is a de-embryonated corn flour. The starch of the degermed flour may be derived from plant sources selected from the group consisting of corn, wheat, peas, rice, tapioca, potato and other grains (such as rye, barley and oats) as well as certain legumes such as soybean, peanut and combinations thereof.
Mixing process
The native starch is mixed with water under sufficient shear and mild heating to achieve a characteristic particle size distribution. The water may be added in the form of steam or liquid water. During processing, the temperature is in the range of 25 ℃ (i.e. room temperature, "RT") to less than 200 ℃, preferably in the range of 25 ℃ to less than 140 ℃. The mixing process may be batch or continuous mixing. This initial mixing process preconditions the starch to obtain desired characteristics of the starch for further processing, such as moisture content, pH and temperature.
Example 1
And (3) an extrusion process. Starch granules exhibiting high solubility and stability were produced using a pilot scale TX-57Magnum co-rotating twin screw extruder system (Wenger Manufacturing, Sabetha, KS) which can be fitted with screw shafts and barrels of varying lengths and equipped with water cooling capability and steam heating. For the screw configuration determined as the conventional screw configuration (conveying screw), a twin-screw configuration is used. For the new ADM screw configuration identified as ADM screw configuration (a mixture of forward and reverse feed lobe shear locks, forward cut-flight screws, and shallow flight cut-flight tapers), a twin screw configuration was used. Figure 7 shows the novel ADM screw configuration for the extrusion process described above.
The effect of higher mechanical shear on the final properties of the product was studied using a novel ADM screw configuration (screw configuration 700 shown in figure 7). Those skilled in the art having the benefit of this disclosure will recognize that suitable extruder systems that may be used with the present invention are not limited to a particular screw variety and may also include, for example, single screw, ram or other similar extrusion methods.
As shown in fig. 7, the screw configuration 700 has two screws 702 and 704. Each screw 702, 704. Each screw 702, 704 has a respective first section 706 that includes a forward cross-sectional 1d screw, i.e., a screw having the screw configuration shown in fig. 4. Each screw 702, 704 has a respective second section 708 that includes the 4 x 45 ° positive shear lock screw configuration shown in fig. 5. Each screw 702, 704 has a respective third section 710 comprising a forward cross-section 1d screw, i.e. a screw having the screw configuration shown in fig. 4. A cutting thread 1. Each screw 702, 704 has a respective fourth segment 712 that includes a 3 x 45 ° forward shear lock screw configuration (similar to the configuration shown in fig. 5, but with three shear locks or paddles instead of the four shear locks or paddles shown in fig. 5). Each screw 702, 704 has a respective fifth section 714 that includes a 3 x 45 ° reverse shear lock screw configuration (similar to the configuration shown in fig. 6, but with three shear locks or paddles instead of the four shear locks or paddles shown in fig. 6). Each screw 702, 704 has a respective sixth section 716 that includes a 2 x 45 ° reverse shear lock screw configuration. Each screw 702, 704 has a respective seventh segment 718 that includes a 3 x 30 ° positive shear lock screw configuration. Each screw 702, 704 has a respective sixth section 716 that includes a 2 x 45 ° reverse shear lock screw configuration. Each screw 702, 704 has a respective seventh segment 718 that includes a 3 x 30 ° positive shear lock screw configuration. Each screw 702, 704 has a respective eighth section 720 that includes a 3 x 45 ° positive shear lock screw configuration. Each screw 702, 704 has a respective ninth section 722 that includes a shallow thread truncated cone configuration. Segment 722 has the same configuration as parallel three-start threaded conical screw 300 shown in fig. 300. Zones 1, 2, 3, 4 and 5 (referred to in figure 7 as barrels 1, 2, 3, 4 and 5) have extrusion temperatures as identified in figure 7.
Example 2
And (4) preparing a formula. Different formulations were designed and prepared for the development and evaluation of extruded flours and starches according to aspects of the present disclosure and these formulations are summarized in table 1. The test was run at pH 6. The ADM screw configuration listed in table 1 is shown in fig. 7 as screw configuration 700. The conventional screw configuration listed in table 1 is a screw configuration consisting of only a conventional conveying screw.
TABLE 1
Figure BDA0003772215680000091
Zone 1 is at room temperature (rt), i.e., 25 ℃.
Results
The starch granule distribution was determined for sample 4 (made using ADM screw configuration 700) and sample 3 (made using a conventional screw configuration consisting of only a conventional transport screw). Sample 4, made according to the present disclosure, had a unique starch particle distribution with > 50% of the particles in the submicron range. See table 2 below and fig. 8. As shown in table 2, sample 4 (made using ADM screw configuration 700) had a D90(μm) of 0.591 (peak 1) for 67% of the particles, while sample 3 (made using a conventional screw configuration consisting of only a conventional transport screw) had a D90(μm) of 0.84 (peak 3) for only 1.72% of the particles.
TABLE 2
Figure BDA0003772215680000092
Wet particle size distribution. Fig. 8 is a plot of bulk density (%) versus size grade (μm) showing the wet particle size distribution of starch granules produced according to aspects of the present invention (i.e., sample 4 of table 1, with 20% water added, extruded with the novel ADM screw configuration 700) as compared to the wet particle size distribution of native dent corn starch (i.e., sample 3 of table 1, with 20% water added) extruded using a conventional screw configuration consisting of only a conventional conveying screw. As shown in fig. 8, ultrafine starch granules produced with the novel ADM screw configuration 700 and without chemical or enzymatic reactants are characterized by a peak size of about 0.12 μm at a bulk density of about 4%. As shown in fig. 8, pellets made according to aspects of the present invention (i.e., sample 4 of table 1) had a much greater% bulk density and smaller size grade (see peak 1) than the% bulk density and size grade (peak 3) of native dent corn starch (i.e., sample 3 of table 1) extruded using a conventional screw configuration consisting of only a conventional conveying screw.
Mix with water and determine solubility. In a preferred embodiment, the product prepared according to the present invention will also be substantially completely soluble in cold water, i.e. soluble in water at 25 ℃ (i.e. room temperature). The method for determining the solubility is described below. According to a preferred method for determining cold water solubility, 4.0g (dry basis) of the product is dispersed in 80.0g of distilled water. After stirring for 10 minutes at 25 ℃, the slurry was transferred to a 100mL graduated cylinder and diluted to volume. The cylinder was inverted three times and allowed to stand at 25 ℃ for 12 min. A 20g aliquot of the supernatant was then transferred to a pre-weighed dish. The pan was then placed on a hot plate and evaporated to dryness. The pan was then weighed and recorded as the dry sample weight. The solubility was calculated using the following formula:
solubility ═ [ (weight of dry sample)/0.8 × 100 ]. The product is considered to have high solubility if the solubility is at least about 70%, and more preferably at least about 80%. The products prepared according to the present invention have excellent cold water solubility and are particularly useful for foods, paints, cosmetics, pharmaceuticals, and various composite materials.
Percent solubility versus time. Fig. 9 is a graph of% solubility versus time showing the stability expressed as% solubility in water at Room Temperature (RT), i.e., 25 ℃, of various particles produced according to aspects of the present invention. As shown in fig. 9, the products made according to the present disclosure ( samples 2 and 4, i.e., extruded using the novel ADM screw configuration 700, see table 1) have a% solubility in water over time that is much greater than the corresponding products made using a conventional screw configuration consisting of only a conventional conveying screw ( samples 1 and 3, see table 1). Sample 4 had a% solubility of over 80% at about 2 hours and greater than 75% at 48 hours, as compared to corresponding sample 3, which had a% solubility of about 40% at about 2 hours and about 10% at 48 hours. Sample 2 had a% solubility of over 60% at about 2 hours and about 43% at 48 hours, compared to corresponding sample 1, which had a% solubility of less than 30% at about 2 hours and about 10% at 48 hours.
Example 3
High stability of starch products in aqueous solutions. Fig. 10 is a photograph depicting a starch product 1002 produced according to aspects of the present invention (i.e., sample 4 of table 1, extruded with the novel ADM screw configuration 700) after being combined with water according to the process described in the above heading "mix with water and determine solubility". As shown in fig. 10, starch product 1002 has high stability in aqueous solution without phase separation. The photograph of starch product 1002 in water shown in fig. 10 was taken 24 hours after starch product 1002 was mixed with water.
Example 4
High stability of flour products in aqueous solutions. Fig. 11 is a photograph depicting a flour product 1102 produced according to aspects of the present invention (i.e., extruded with the novel ADM screw configuration 700) after combination with water according to the process described in the heading "mix with water and determine solubility" above, showing high solubility in aqueous solution as compared to a conventional flour product 1104 in aqueous solution. As shown in fig. 11, a flour product 1102 made in accordance with the present disclosure has high stability in aqueous solution without phase separation as compared to a conventional flour product 1104 extruded using a conventional screw configuration consisting of only a conventional conveying screw, which has significant phase separation as shown by the base phase 1106 having more solids than the upper phase 1108. The photographs of the flour product 1102 in water and the conventional flour product shown in figure 11 were taken 24 hours after each mixing with water.
Example 5
Starch/flour and lipid formulations. Aspects of the invention include starch/flour mixtures having a lipid formulation.
Composition of lipid formulations.
Aspects of the method include a lipid formulation according to:
(1) microemulsion (ME): 5 grams of monoglyceride was added to a 5% glycerol solution in DI water and mixed well. Then 2 grams of soy lecithin was added to the solution and mixed well. Then 12 grams of medium chain triglycerides ("MCT") were added to the solution and mixed thoroughly.
(2) Emulsifier blend (EM): 12.6 grams of monoglyceride was added to a 12% glycerol solution and mixed well. Then 5 grams of soy lecithin was added to the solution and mixed well.
(3) Palmitic Acid Formulation (PAF): 2.5 grams of monoglyceride was added to 15 grams of DI water and mixed well. Then 2.5 grams of palmitic acid was added to the solution and mixed well.
Table 3 the composition of the lipid formulations was determined in% by weight.
TABLE 3 composition of lipid formulations
Figure BDA0003772215680000121
The starch/flour is mixed with the lipid formulation. Aspects of the method include a starch/flour mixture having a desired lipid formulation according to: (1) a 10% DS slurry was prepared by adding 30 grams of the desired Dry Solids (DS) of starch/flour to Deionized (DI) water; (2) for the sample to which the lipid formulation was added, then 6 grams of the desired lipid formulation was added to the slurry; (4) the slurry was dried using a gas step (Buchi) B290 spray dryer, with an inlet temperature of 100 ℃, an outlet temperature of about 60 ℃, and a pump speed of 1.1-1.4 mL/min. For spray drying, the liquid sample is pumped to a spray drying nozzle.
Example 6
And (4) grinding. Ultrafine starch or flour is produced by means of a fluidized bed jet mill (Netzsch) Condux CGS 10). Starch or flour was introduced into the jet mill by means of a volumetric feeder and was milled by means of compressed gas supplied at 6 bar to three milling nozzles. The particle size can be adjusted by adjusting the rotational speed of the internal classifier. At a classifier speed of 14,000rpm, starch or flour was produced with a D50 of 3-4 μm and a D90 of less than 10 μm (Table 4). The particle size can also be adjusted by adjusting the milling time. Milled corn starch 1 and milled corn starch 2 have the same starting material, but the milling time for milling milled corn starch 1 is longer than the milling time for milling corn starch 2.
Particle size and surface area of the powder. The powder was analyzed for particle size and surface area using a Malvern Mastersizer 3000 dry module. Changes in particle size and surface area of the dry powder were monitored. Particle size and surface area are shown in table 4. As shown in table 4, with 318m from which the ultra-fine product according to the present disclosure was derived 2 The adjustable process technology for producing these ultra fine products provides up to 3,278m by reducing the particle size D10 to 1.42 μm compared to a base material of particle size D10 of 13.0 μm/kg surface area 2 Increased surface area per kg-see ground rice flour compared to natural rice flour. The ultrafine product of the invention has the following improved properties compared to the base material from which it is derived: (i) milled corn starch 1, particle size D10 decreased 79% (1.82/8.80) and the surface area increased 7.6 times (3073/401); (ii) milled corn starch 2, particle size D10 decreased 80.7% (1.70/8.8) and the surface area increased 4.7 times (1892/401); (iii) milled modified tapioca starch, particle size D10 decreased 80% (1.7/8.67) and surface area increased 5.7 times (3286/573); (iv) milled rice flour, particle size D10 decreased 89.1% (1.42/13.0) and the surface area increased 10.3 times (3278/318). Persons of ordinary skill in the art having benefit of the present disclosure will recognize that adjustable process techniques for producing ultrafine products according to the present disclosure may provide up to 4,000m by reducing particle size D10 to 1 μm as compared to the base material from which the ultrafine products according to the present disclosure are derived 2 Increased surface area per kg. In one embodiment, an ultrafine product according to the present disclosure may have a thickness of 100- 2 A surface area per kg and a particle size D10 of 1-200. mu.m.
TABLE 4 particle size and surface area of the powder
Figure BDA0003772215680000131
The particle size and surface area of the dispersion were analyzed using a malvern Mastersizer 3000 wet module. The effect of different lipid formulations on the particle size and surface area of the milled material is shown in table 5. As shown in table 5, spray drying the milled material with the lipid formulation reduced particle size and increased surface area compared to when the lipid formulation was not present.
Table 5.10 particle size and surface area in aqueous soluble solids (s.s) dispersion
Figure BDA0003772215680000132
Figure BDA0003772215680000141
Example 7
Color and whiteness of the dry powder. Color characterization was analyzed using a colorimeter, hunterli (HunterLab) ColorFlex EZ. The dry powder was monitored for changes in whiteness (L). The color characteristics are shown in table 6. As shown in table 6, suitable process techniques combined with the addition of lipid formulations (e.g., milling, spray drying, and PAF formulations) provide products with retained whiteness characteristics compared to the base material from which the product was derived.
TABLE 6 whiteness of dry powders
Figure BDA0003772215680000142
Example 8
Color characterization was analyzed using a hunter ColorFlex EZ. The reason for monitoring is that
Figure BDA0003772215680000144
Heating in a water bath of (a) for 30 minutes caused a change in whiteness (L) of the 10% s.s aqueous dispersion. The color characteristics are shown in table 7. As shown in Table 7, suitable lipid formulations, such as PAF formulations, provide protection against whiteness loss in ultrafine starch or flour particle products, particularlySpray dried milled modified tapioca starch, milled rice flour, spray dried milled rice flour, milled corn starch, spray dried milled corn starch, with the exception of milled modified tapioca starch (which has not been spray dried). As shown in table 7, suitable lipid formulations, such as PAF formulations, provide protection against whiteness loss in ultrafine starch or flour particle products made using spray drying. Ultrafine starch or flour particle products made using the PAF formulation and spray drying provide increased thermal stability as evidenced by a reduction in whiteness loss compared to products made using spray drying but without the PAF formulation.
TABLE 7.10% whiteness of aqueous S.S. dispersions
Figure BDA0003772215680000143
Figure BDA0003772215680000151
Difference in whiteness before and after heating
Example 13
Differential Scanning Calorimetry (DSC). The thermal properties of the dried product were monitored using a TA instruments DSC 2500. 10 mg of sample DS and 30 mg of DI water were added to the DSC pan and equilibrated at room temperature overnight (about 16-20 hours). The DSC parameters were set from 30 to 170 ℃ at a rate of 5 ℃/min. The temperature associated with the gelatinization process, i.e. the peak temperature, was analyzed on the DSC thermogram using Trios software. The peak temperature characteristics by DSC analysis are shown in table 8. As shown in table 8, milling and adding a lipid formulation, such as a PAF formulation, provided improved thermal stability as characterized by having a higher DSC peak temperature than the base material from which it was derived.
TABLE 8 Peak temperature characteristics by DSC analysis
Figure BDA0003772215680000152
ND: not detected out
Example 14
The X-ray diffraction (XRD) pattern of the corn starch sample is shown in fig. 12. Using a source equipped with a Cu Ka radiation
Figure BDA0003772215680000153
Brooks (Bruker) D8 Advance running at 40kv and 40mA monitored the crystallinity and amylose-lipid complex characteristics of the dried product. The dry product is or is derived from corn starch, wherein the relative crystallinity% (RC) and the relative intensity% (RI) at 2 θ ═ 19.8 ° (%) are determined as follows: a) natural, RC 38%, RI 0%; b) milled, RC 36.9%, RI 4.1%; c) dry blended with PAF formula, RC 35%, RI 6.8%; d) freeze-dried slurry blend with PAF formulation, RC 38.0%, RI 16.7%; e) spray-dried slurry blend incorporating PAF formulation, RC 36.8%, RI 17.1%; and f) paste, RC 0%, RI NA. Using a scintillation counter to scan 0.02 deg. min in a coupled 2 theta scan pattern -1 The relative intensities in the scatter angle range (2 theta) of 4.0-34.0 deg. are recorded. Relative Crystallinity (RC) is expressed in percentage, and the crystalline area (I) obtained from each diffraction pattern using the following equation c ) And amorphous area (I) a ) And (3) calculating: RC (%) ═ (I) c -I a )/I c x 100。
The paste was made by cooking the starting ingredients in Deionized (DI) water at 95 ℃ for 30min and freeze dried immediately. X-ray diffraction of the paste was used as the amorphous area (I) with an RC of 0% a ) (as shown in fig. 12).
Referring to fig. 12, the peak intensity reflections at 15 °, 17 °, 18 °, and 23 ° 2 θ are associated with the a-pattern of the native crystalline structure. The diffraction peak at 19.8 ° 2 θ is due to the formation of starch-lipid complexes, while the peak at 21.3 ° 2 θ is due to free and uncomplexed lipids (see Chao, c., Yu, j., Wang, s., Copeland, l., Wang, s. (2017). mechanismins understanding the formation of complexes between corn starch and lipids [ mechanism of complex formation between corn starch and lipids ]. Journal of Agricultural and Food Chemistry [ Journal of Agricultural and Food Chemistry ] (66), 272-) 278).
The Relative Crystallinity (RC) characteristics analyzed by XRD are shown in table 9. As shown in table 9, milling and incorporation of the lipid formulation (e.g., PAF formulation) maintained particle integrity; since the natural crystallinity of the product is retained by more than 88% compared to the base material from which the product is derived.
TABLE 9 relative crystallinity characteristics by XRD analysis
Figure BDA0003772215680000161
Example 15
X-ray diffraction (XRD). The amount of formation of amylose-lipid complex was analyzed from the intensity of the peak at 19.8 ° 2 θ. Table 10 shows the relative strength at 19.8 ° 2 θ compared to the base material from which the composite was derived. As shown in table 10, incorporation of a lipid formulation, such as a PAF formulation, increased complex formation by up to 25% compared to the base material from which the complex was derived.
Table 10 relative intensity characteristics at 19.8 ° 2 θ analyzed by XRD
Figure BDA0003772215680000171
Example 16
X-ray diffraction (XRD). The effect of particle size on the amount of amylose-lipid complex formation was analyzed from the intensity of the peak at 19.8 ° 2 θ. Table 11 shows the relative strength at 19.8 ° 2 θ compared to the base material from which the composite was derived. As shown in table 9, the claimed process technology for producing ultrafine products enhances amylose-lipid complexation even under ambient conditions; whereas smaller particle size products, such as corn starch, show higher amylose-lipid complex formation than larger particle size products. As shown in table 11, an increase in moisture content, e.g., dry blended versus slurry blended, resulted in an enhanced interaction between the lipid formulation and the base micronized material, increasing amylose-lipid complex by up to 16.7%. As shown in table 11, an increase in drying temperature, e.g., using spray drying versus freeze drying, resulted in an enhanced interaction between the lipid formulation and the base micronized material, increasing amylose-lipid complexes by up to 17.1%.
Table 11 relative intensity at 19.8 ° for different particle sizes of corn starch analyzed by XRD.
Figure BDA0003772215680000172
Example 17
Color absorption rate. The absorption capacity of the product was monitored by the color absorbed using spectrophotometric analysis. A 1% weight/weight solution of the dye (e.g., brilliant green) was prepared in DI water. 0.1 grams of starch/flour DS and 9.9 grams of DI water were added to the centrifuge tube and mixed thoroughly. The tube was then centrifuged at 1000Xg for 5 minutes and the supernatant was analyzed at 625nm using an Agilent Cary 60 UV-Vis. The relative color absorbance was calculated using the following equation: relative color absorptance (%) -100 x (absorptance of bright green-absorptance of sample)/absorptance of bright green. A higher relative color absorbance indicates a higher absorption capacity of the sample. The relative color absorbance characteristics are shown in table 12. As shown in table 12, enhanced adsorption capacity up to 90% was observed.
TABLE 12 relative color absorptivity
Figure BDA0003772215680000181
Benefits of the present disclosure include:
a. a method for developing thermostable lipid complexes by preserving particle integrity and native crystallinity due to improved interaction resulting from increased surface area of lipid and ultrafine starch/flour;
b. an adjustable process technology is disclosed to increase surface area and incorporate lipid formulations while highly retaining product whiteness;
c. improved dispersibility/opacity is observed due to the incorporation of the claimed lipid formulation into ultrafine starch/flour;
d. retention of crystallinity and particle integrity was observed in the product milled and incorporated with the lipid formulation;
e. for starches/flours with lower particle size, higher amylose-lipid complex manufacturing capacity (as determined using XRD) was observed; and
f. the disclosed technology enables the formation of amylose-lipid inclusion complexes with easily oxidizable lipids and heat sensitive ingredients such as flavors, colors, and plant extracts.
The present invention provides a simple, clean and cost-effective process and conditions to produce a variety of ultrafine starch/flour particles that exhibit greater than 75% water solubility and stability over a time span of at least about 48 hours. These stabilities and solubilities of the ultrafine starch/flour particles of the invention exceed those typical of conventional products on the market. The ultrafine starch/flour particles of the present invention provide improved utility in food and industrial applications not achieved by conventional products. Those skilled in the art having the benefit of this disclosure will recognize that the unique ultrafine (also referred to as submicron) starch/flour particles and products, compositions and powder formulations disclosed herein provide the following benefits:
a. ultrafine starch granules produced using a simple, cost-effective, non-chemical modification process are used as bulking agents for certain food applications, such as dry mixes, sweeteners, and the like.
b. Improving sensory and organoleptic functions in food systems such as bread fillings and coatings, cereal bars, extruded snacks, margarines, low fat spreads, shortenings, confections, certain high moisture foods such as sour cream, yogurt, cheese, processed cheese and beverages.
c. As carriers for flavors, micro/macro nutrients, enzymes and dietary supplements.
d. Improving texture provision in food products, where a range of solubility and stability can be adjusted to improve adhesion and develop a desired texture, such as crispness, etc., is important to the end user's eating experience.
e. Improve the solubility of carbohydrates and proteins and thereby obtain advantageous nutritional functions in food and feed.
f. Improved particle composition and improved adhesion for coating applications in industry, cosmetics, paper.
Color absorptivity. Those skilled in the art having the benefit of this disclosure will recognize that the process of the present invention provides novel ultrafine starch particles that can be used in food applications, as carriers, and in coating applications.
The disclosure has been described herein with reference to certain exemplary embodiments, compositions, and uses thereof. However, those of ordinary skill in the art will recognize that various substitutions, alterations, or combinations can be made to any of the exemplary embodiments without departing from the spirit and scope of the present disclosure. Accordingly, the disclosure is not limited by the description of these exemplary embodiments, but rather by the appended claims as originally filed.

Claims (40)

1. A method of forming an ultrafine starch or flour product comprising:
at least one of steps (a) or (b),
(a) heating a mixture of water and natural or modified starch or flour to a temperature in the range of 25 ℃ to less than 200 ℃, extruding the mixture with a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw in series to produce an extrudate; or
(b) Forming a mixture of water, lipid and natural or modified starch or flour and drying the mixture of water, lipid and natural or modified starch or flour to produce a dried lipid starch intermediate or a dried lipid flour intermediate; and
at least one of steps (c) or (d),
(c) milling the native or modified starch or flour to reduce the particle size of the native or modified starch or flour prior to step (a) or (b); or
(d) Breaking up the extrudate produced in (a), or breaking up the dried lipid starch intermediate or flour intermediate produced in (b),
thereby producing an ultrafine starch or flour granule product having high water solubility as compared to the starch or flour granule product produced in (a) in a screw configuration wherein the extrusion of the mixture is with a low shear forward conveying screw and no high shear mixing screw, or as compared to the starch or flour intermediate produced in (b) in the absence of the lipid;
wherein the method is free of chemical or enzymatic reactions.
2. The method as claimed in claim 1, wherein the ultrafine starch or flour particle product has a particle size of 1-200 μm and a surface area of 100-4,000m 2 /kg。
3. The method of claim 1 wherein the whiteness of the ultrafine starch or flour particle product is 97 or less on a L x color scale.
4. The method of claim 1, wherein the gelatinization temperature of the ultrafine starch or flour particle product is in the range of 65 to 80 ℃.
5. The method of claim 1, wherein, using step (a), the ultrafine starch or flour particle product retains a crystallinity in the range of 85% to 98% compared to the native or modified starch or flour from which it is derived.
6. The method of claim 1, wherein, using step (b), the ultrafine starch or flour particle product with lipids retains a crystallinity in the range of 85% to 100% compared to the natural or modified starch or flour from which it is derived.
7. The method of claim 1, wherein, using step (b), the ultrafine starch or flour particle product with lipids has an amylose-lipid complex formation at least 25% greater than the base material from which it is derived.
8. The method of claim 1, wherein the ultrafine starch or flour particle product has an enhanced absorbency of up to 90%.
9. The method of claim 1, wherein the in vitro digestibility of the ultrafine starch or flour particle product is in the range of 10% to 80%.
10. The method of claim 1, wherein the starting native or modified starch or flour contains a starch content of at least 30% by weight and is selected from the group consisting of corn, wheat, barley, rice, potato, tapioca, waxy tapioca, pea, broad bean and lentil.
11. The method of claim 1, wherein, using step (b), the lipid comprises fatty acids with a chain length of 6 to 22 or the corresponding mono-, di-or triglycerides.
12. The method of claim 11, wherein the chain length is 10 to 18.
13. The process of claim 11, wherein the chain length is 12 to 16.
14. A method of making a food product comprising incorporating the ultrafine starch or flour particle product made according to claim 1, wherein the food product is selected from the group consisting of soup products, dairy products, processed meat products, yogurt products, flavored products, frozen food products, fruit juice products, confectionery products and baked products.
15. A method of forming an ultrafine starch or flour particle product comprising:
(a) mixing starch or degermed flour or any combination thereof with water, thereby producing a mixture;
(b) heating the mixture to a temperature in the range of 25 ℃ to less than 200 ℃;
(c) extruding the mixture with a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw in series, thereby producing an extrudate; and
(d) breaking the extrudate to produce an ultrafine starch or flour granule product having high water solubility compared to a starch or flour granule product produced where extrusion of the mixture is with a screw configuration consisting of a low shear forward conveying screw and no high shear mixing screw;
wherein the method is free of chemical or enzymatic reactions.
16. The method of claim 15, wherein the starch or degermed flour is selected from the group consisting of corn, wheat, barley, rice, potato, tapioca, waxy tapioca, pea, broad bean and lentil.
17. The method of claim 15, wherein the at least one low shear conveying screw is a forward cut-flight screw and the at least one high shear mixing screw is a forward shear lock screw.
18. The method of claim 15, wherein the screw configuration comprises a first low shear forward conveying screw, at least one high shear mixing screw, and a second low shear forward conveying screw in series.
19. The method of claim 15, wherein the screw configuration comprises a first low shear forward conveying screw, a first high shear mixing screw, a second low shear forward conveying screw, and a second high shear mixing screw selected from the group consisting of a forward shear lock screw, a reverse shear lock screw, and combinations thereof, in series.
20. The method of claim 15, wherein the screw configuration comprises, in series, a first low shear forward conveying screw comprising a forward shear screw, a first high shear mixing screw comprising a forward shear lock screw, a second low shear forward conveying screw comprising a forward shear screw, a second high shear mixing screw comprising a forward shear lock screw, a third high shear mixing screw comprising a reverse shear lock screw, a fourth high shear mixing screw comprising a reverse shear lock screw, a fifth high shear mixing screw comprising a forward shear lock screw, and a sixth high shear mixing screw comprising a forward shear lock screw,
wherein the first high shear mixing screw, the second high shear mixing screw, the third high shear mixing screw, the fourth high shear mixing screw, the fifth high shear mixing screw, and the sixth high shear mixing screw are each selected from the group consisting of a 4 x 45 ° forward shear lock screw, a 3 x 45 ° reverse shear lock screw, a 2 x 45 ° reverse shear lock screw, a 3 x 30 ° forward shear lock screw, and combinations thereof.
21. The method of claim 15, wherein,
the first high shear mixing screw is a 4 x 45 ° forward shear lock screw;
the second high shear mixing screw is a 3 x 45 ° forward shear lock screw;
the third high shear mixing screw is a 3 x 45 ° reverse shear lock screw;
the fourth high shear mixing screw is a 2 x 45 ° reverse shear lock screw;
the fifth high shear mixing screw is a 3 x 30 ° forward shear lock screw; and is
The sixth high shear mixing screw is a 3 x 45 ° forward shear lock screw.
22. The method of claim 20, further comprising a shallow flighted, truncated conical screw after the sixth high shear mixing screw in series.
23. The method of claim 21, further comprising a shallow flighted, truncated conical screw after the sixth high shear mixing screw in series.
24. The method of claim 15, wherein the screw configuration comprises a first screw configuration and a second screw configuration, wherein the first screw configuration is parallel to the second screw configuration.
25. The method of claim 15, wherein breaking the extrudate comprises applying pressure to the extrudate.
26. The method of claim 25, wherein applying pressure to the extrudate is selected from the group consisting of rolling, grinding or milling, and combinations thereof.
27. An apparatus, comprising:
a heater configured to heat a mixture of starch or de-germ flour or a combination thereof and water to a temperature in a range of 25 ℃ to less than 200 ℃;
a screw configuration comprising at least one low shear forward conveying screw and at least one high shear mixing screw in series, wherein the screw configuration is configured to extrude the mixture to produce an extrudate; and
at least one of a roller press, a grinder, a mill, or a spray dryer configured to break the extrudate to produce an ultrafine starch or flour granule product without chemical or enzymatic reaction, wherein the ultrafine starch or flour granule product has high water solubility compared to a starch or flour granule product without chemical or enzymatic reactants produced without the screw configuration consisting of a low shear forward conveying screw and without a high shear mixing screw.
28. The apparatus of claim 27, wherein the at least one low shear conveying screw is a forward cut-flight screw and the at least one high shear mixing screw is a forward shear lock screw.
29. The apparatus of claim 27, wherein the screw configuration comprises a first low-shear forward conveying screw, at least one high-shear mixing screw, and a second low-shear forward conveying screw in series.
30. The apparatus of claim 27, wherein the screw configuration comprises a first low shear forward conveying screw, a first high shear mixing screw, a second low shear forward conveying screw, and a second high shear mixing screw selected from the group consisting of a forward shear lock screw, a reverse shear lock screw, and combinations thereof, in series.
31. The apparatus of claim 27, wherein the screw configuration comprises, in series, a first low shear forward conveying screw comprising a forward shear screw, a first high shear mixing screw comprising a forward shear lock screw, a second low shear forward conveying screw comprising a forward shear screw, a second high shear mixing screw comprising a forward shear lock screw, a third high shear mixing screw comprising a reverse shear lock screw, a fourth high shear mixing screw comprising a reverse shear lock screw, a fifth high shear mixing screw comprising a forward shear lock screw, and a sixth high shear mixing screw comprising a forward shear lock screw,
wherein the first high shear mixing screw, the second high shear mixing screw, the third high shear mixing screw, the fourth high shear mixing screw, the fifth high shear mixing screw, and the sixth high shear mixing screw are each selected from the group consisting of a 4 x 45 ° forward shear lock screw, a 3 x 45 ° reverse shear lock screw, a 2 x 45 ° reverse shear lock screw, a 3 x 30 ° forward shear lock screw, and combinations thereof.
32. The apparatus of claim 31, wherein,
the first high shear mixing screw is a 4 x 45 ° forward shear lock screw;
the second high shear mixing screw is a 3 x 45 ° forward shear lock screw;
the third high shear mixing screw is a 3 x 45 ° reverse shear lock screw;
the fourth high shear mixing screw is a 2 x 45 ° reverse shear lock screw;
the fifth high shear mixing screw is a 3 x 30 ° forward shear lock screw; and is
The sixth high shear mixing screw is a 3 x 45 ° forward shear lock screw.
33. The apparatus of claim 30, further comprising a shallow flighted, truncated conical screw after the sixth high shear mixing screw in series.
34. The apparatus of claim 32, further comprising a shallow flighted, truncated conical screw after the sixth high shear mixing screw in series.
35. The apparatus of claim 27, wherein the screw configuration comprises a first screw configuration and a second screw configuration, wherein the first screw configuration is parallel to the second screw configuration.
36. An ultrafine starch or cereal-based particle extruded product comprising ultrafine starch or cereal-based particles characterized by a peak size of about 0.12 μm at a bulk density of about 4%, wherein the extruded product is free of chemical or enzymatic reactants.
37. An ultrafine starch or cereal-based particle extruded product comprising ultrafine starch or cereal-based particles characterized by a percent solubility in water in the range of about 75-95% for at least 48 hours, wherein the extruded product is free of chemical or enzymatic reactants.
38. The ultrafine starch or grain-based particle extruded product of claim 27, wherein the percent solubility in water is in the range of about 85-95% for at least 48 hours.
39. A method of forming an ultrafine starch or flour product comprising:
(a) forming a mixture of water, lipid and natural or modified starch or flour and drying the mixture of water, lipid and natural or modified starch or flour to produce a dried lipid starch intermediate or a dried lipid flour intermediate; and
at least one of steps (b) or (c),
(b) milling the native or modified starch or flour to reduce the particle size of the native or modified starch or flour prior to step (a); or
(c) Fragmenting the dried lipid starch intermediate or flour intermediate produced in (a),
thereby producing an ultrafine starch or flour particle product having high water solubility compared to the starch or flour intermediate produced in the absence of the lipid in (b);
wherein the method is free of chemical or enzymatic reactions.
40. The method of claim 39, wherein the crushing of the dried lipid starch intermediate or flour intermediate in (c) is selected from the group consisting of rolling, grinding or milling, and combinations thereof.
CN202080095151.3A 2019-12-12 2020-12-11 Ultrafine starch or grain-based flour compositions and related methods Pending CN115052904A (en)

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