WO2020124201A1

WO2020124201A1 - A composition and method for producing an edible product containing starch particles having improved health effects

Info

Publication number: WO2020124201A1
Application number: PCT/CA2019/051411
Authority: WO
Inventors: Nicolas BORDENAVE
Original assignee: University Of Ottawa
Priority date: 2018-12-18
Filing date: 2019-10-02
Publication date: 2020-06-25

Abstract

An edible composition comprising starch particles comprising about 10-90% of slowly digestible starch and about 10-90% resistant starch and a method of making starch particles from a native starch, the method comprising: forming a starch slurry in an aqueous dispersion or an aqueous solution; heating the starch slurry to form gelatinized starch; forming, from the gelatinized starch, starch particles; cooling the formed starch particles; either (a) hydrolyzing a native starch before the step of forming the starch slurry; (b) forming the starch slurry using a native starch and after the step of forming the starch particles, hydrolyzing the formed starch particles; or (c) forming the starch slurry using a native starch and after the step of cooling, hydrolyzing the cooled formed starch particles; and wherein the conditions of hydrolyzing are such that after the step of hydrolyzing, the starch remains a high molecular weight starch.

Description

A composition and method for producing an edible product containing starch particles having improved health effects

RELATED APPLICATIONS

[0001] This application claims priority to U.S. provisional application serial No.

62/781,272 filed December 18, 2018, which is incorporated by reference in its entirety.

TECHNICAL FIELD

[0002] Example embodiments relate to composition and method for producing an edible product containing starch particles having improved health effects.

BACKGROUND

[0003] Chronic consumption of high glycemic response foods and the subsequent uncontrolled glycemia are associated with chronic diseases such as type II diabetes, obesity, cardiovascular diseases and some forms of cancer. In some respects, uncontrolled glycemia is associated with decrease in intellectual performance (e.g. ability to focus and function, mood swings), in the short term.

[0004] Foods eliciting moderate and prolonged glycemic responses as well as improved satiety and gut health benefits are limited to fruits and vegetables as well as whole grain cereal products (e.g. whole grain pasta, oatmeal). Most of these foods exhibit either poor convenience and portability or poor organoleptic properties, and therefore little consumer acceptance.

[0005] Some food and beverage forms can elicit moderate and/or prolonged glycemic responses. Of those food and beverage forms that are able to elicit one or more of moderate and prolonged glycemic responses, improved satiety, gut health benefits, and acceptable organoleptic properties, these foods are not formulated to retain the benefits after certain treatments required by food safety measures, such as the application of heat and and/or pasteurization treatment. For example, native starches are highly resistant to digestion. However, this resistance to digestion is lost during the application of heat. Therefore, when food and beverage forms that incorporate the native starches are subsequently subjected to heat treatment, the beneficial glycemic response of the native starch will be at least reduced (see for example, Thomas MS Wolever, B Jan- Willem van Klinken, Nicolas Bordenave, Melissa Kaczmarczyk, Alexandra L Jenkins, YiFang Chu, Laura Harkness; Reformulating cereal bars: high resistant starch reduces in vitro digestibility but not in vivo glucose or insulin response; whey protein reduces glucose but disproportionately increases insulin, The American Journal of Clinical Nutrition, Volume 104, Issue 4, 1 October 2016, Pages 995-1003,

https://doi.org/10.3945/ajcn.116.132431, incorporated by reference in its entirety).

[0006] There is a need to develop edible products that are acceptable for consumers that will retain one or more of moderate and prolonged glycemic response, improved satiety, gut health benefits, and acceptable organoleptic properties, to manage, for example, glycemia.

SUMMARY

[0007] According to one embodiment, there is provided an edible composition and method for producing the edible composition comprising starch particles having improved health effects.

[0008] According to one embodiment, there is provided an edible composition and method for producing the edible composition comprising significant amounts of slowly digestible starch and/or resistant starch. In some embodiments, the edible composition is a solid food product, such as a snack, or beverage product, such as a ready -to-drink beverage, that is formulated to elicit a prolonged and moderate glycemic response, improved satiety and gut health benefits.

[0009] In some aspects, upon ingestion of the edible composition, the starch particles comprising significant amounts of resistant starch are fermented in the colon and the fermentation products may have one or more of anti-inflammatory effects, antioxidant effects, and satiety-inducing effects. According to one embodiment, ingestion of the edible composition provides prebiotic effect and satiety-inducing effects owing to the production of short chain fatty acids, particularly butyrate, upon colonic fermentation by microorganisms. In some embodiments, ingestion of the edible composition reduces the individual’s glycemic response and the insulinemic response.

[0010] According to one embodiment, there is provided an edible composition and method for producing the edible composition which is formulated to withstand usual heat and moisture treatment such as pasteurization or sterilization, and still provide the intended health effects.

[0011] According to one embodiment, there is provided an edible composition comprising starch particles comprising about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch. In one aspect, there is provided a use of the edible composition for management of weight, for treatment of obesity, or for health maintenance and treatment of diabetic and prediabetic individuals. In another aspect, there is provided a use of the edible composition for the preparation of a formulation for management of weight, for treatment of obesity, or for health maintenance and treatment of diabetic and prediabetic individuals.

[0012] According to one embodiment, there is provided a method of making starch particles from a native starch, the method comprising: forming a starch slurry of about 1 to about 70% w/w starch in an aqueous dispersion or an aqueous solution;

heating the starch slurry to form gelatinized starch; forming, from the gelatinized starch, starch particles; cooling the formed starch particles at about 0 to about 5°C for about 15 minutes to about 72 hours; either (a) hydrolyzing a native starch before the step of forming the starch slurry; (b) forming the starch slurry using a native starch and after the step of forming the starch particles, hydrolyzing the formed starch particles; or (c) forming the starch slurry using a native starch and after the step of cooling, hydrolyzing the cooled formed starch particles; and wherein the conditions of hydrolyzing are such that after the step of hydrolyzing, the starch remains a high molecular weight starch [0013] According to one embodiment, there is provided a method to produce starch particles having a desired proportion of slowly digestible starch to resistant starch. According to one embodiment, there is provided a method which allows for the adjustment of the proportion of the slowly digestible starch to the resistant starch.

BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 is a graph depicting the timeline of starch digestion in the small intestine;

[0015] Figure 2a outlines a procedure for producing starch particles, in accordance with an embodiment of the present invention;

[0016] Figure 2b shows a syringe deposition method, in accordance with an embodiment of the present invention;

[0017] Figure 3 is a schematic of the in vitro simulated digestion process, in accordance with an embodiment of the present invention;

[0018] Figure 4 is a graph which shows Rapidly Digestible Starch (RDS), Slowly

Digestible Starch (SDS) and Resistant Starch (RS) content ± SEM (n=3) of starch particles exposed to different acid hydrolysis treatments expressed as a percentage of total starch (TS): (A) 2M acid treated particles; (B) 3M acid treated particles; (C) particles from 2M acid treated native starch; and (D) particles from 3M acid treated native starch. (CS) is com starch or (PS) is potato starch and * indicates optimized conditions from Surface Response models;

[0019] Figure 5 is a graph which shows slowly digestible starch (SDS) content ±

SEM as a percent of Total Starch (TS), n=3 of com starch (CS) or potato starch (PS) particles exposed to 2-3M HC1 for 1-5 days after or before particle formation against their digestion rate in vitro : (A) shows slowly digestible starch (SDS) content of CS or PS particles exposed to 2-3M HC1 for 1-5 days against their digestion rate in vitro, (B) shows slowly digestible starch (SDS) content of starch particles made from native CS or PS exposed to 2-3M HC1 for 1-5 days then used to form particles, against their digestion rate in vitro ; and

[0020] Figure 6 shows gelatinization enthalpy DH (kJ/mol) ± SEM (n=2) of com starch (CS) and potato starch (PS) particles or native starch used to form particles exposed to 2M or 3M HC1 for 1-5 days, against their digestion rate in vitro: (A) gelatinization enthalpy DH (kJ/mol) of CS and PS particles exposed to 2M or 3M HC1 for 1-5 days, against their digestion rate in vitro, (B) gelatinization enthalpy DH (kJ/mol) of native CS and PS exposed to 2M or 3M HC1 for 1-5 days then used to form particles, against their digestion rate in vitro.

PET ATT ED DESCRIPTION OF EXAMPLE EMBODIMENTS

[0021] Reference will be made below in detail to exemplary embodiments of the invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numerals used throughout the drawings refer to the same or like parts.

[0022] As used herein, the following terms and phrases shall have the meanings set forth below. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the invention, non- limiting methods and materials are now described.

[0023] The singular forms“a,”“an,” and“the” include plural reference unless the context clearly dictates otherwise. By way of example, "an element" means one element or more than one element.

[0024] As used herein,“satiety” means the absence of desire to eat or the absence of the feeling of hunger.. Satiation is the point in time during a meal where you achieve satiety. Such effects typically extend the time between food intake by an individual and can result in a smaller amount of food and/or fewer calories consumed in a single or subsequent sitting.

[0025] As used herein,“native starches” include all starches as found in nature in any plant source, isolated and in their semi-crystalline form. In some embodiments, native starch can be, but not limited to, starch that is sourced from rice, wheat, tapioca, com, potato, and that can specifically be high amylose com starch, high amylose potato starch or high amylose wheat starch. Native starches are found in the form of semi crystalline granule and may comprise different percentages of amylose and amylopectin, the latter being the main contributor to the native granule’s crystallinity. Native starches are sensitive to heat and/or moisture. When heated, the starch becomes disorganized (i.e. loses its semi-crystalline structure). Upon cooling, the starch is re-ordered (retrograded) and becomes at least partially crystalline and where the amylose is now the main contributor to the starch’s crystallinity.

[0026] As used herein,“subject” and“individual” are used interchangeably and may encompass any vertebrate including mammals, but not limited to humans, non human primates, rats, and mice. In a preferred embodiment, the mammal is a human.

[0027] Figure 1 is a graph depicting the timeline of starch digestion in the small intestine. As shown, rapidly digestible starch (RDS) will cause a glycemia spike.

Slowly digestible starch (SDS), on the other hand, will cause a reduced glycemic response as compared to RDS. Resistant starch (RS) escapes digestion and will lead to a reduced glycemic response as compared to RDS.

[0028] The present invention relates to an edible composition (i.e. food and beverage products) comprising starch particles comprising about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch. In some

embodiments, the slowly digestible starch and resistant starch when incorporated into food and beverage products that when consumed, can provide for a relatively lower glycemic index, which can also increase satiety. According to one embodiment, the starch particles comprise about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch.

[0029] In some embodiments, the starch particles are modified by hydrolysis treatment. In some embodiments, the hydrolysis treatment comprises using acid or enzymes to act on the native starch, to act on starch that has undergone heating and forming steps, or to act on starch that has undergone heating, forming, and retrograding steps.

[0030] In some embodiments, the starch particles are dimensioned so as to present a suitable specific surface area for digestion when the edible composition is consumed by the individual. In some embodiments, the starch particles are dimensioned from about 2 mm to about 2 cm, from about 5 mm to about 2 cm, or from about 3 mm to about 1 cm, in diameter.

[0031] The present invention also relates to methods of making starch particles which are modified by hydrolysis treatment. In some embodiments, the method allows a manufacturer to customize the degree of resistance to digestion, to raise or lower the glycemic response, depending on the desired outcome. In particular, the method can be used to modify the relative proportions of rapidly digestible starch (RDS), slowly digestible starch (SDS), and resistant starch (RS), as required.

[0032] For example, in some circumstances it may be desired to formulate a food or beverage product to elicit a prolonged and moderate glycemic response, have improved satiety, and gut health benefits. In this circumstance, the food or beverage product may be formulated so that the starch has a much greater relative proportion of at least one of RS and SDS to RDS.

[0033] In other circumstances it may be desired that a food or beverage product provide a relatively greater proportion of RS to SDS or vice versa.

[0034] According to one embodiment, there is provided a method to produce starch particles from a native starch. In this embodiment, the native starch is first hydrolyzed by acid or enzymatic treatment sufficient to hydrolyze the glycosidic bonds of the starch. According to one embodiment, the acid treatment can comprise a strong acid, which can be suitable for human consumption. In one embodiment, the strong acid can comprise HC1 and the HC1 can be in any concentration that is sufficient to hydrolyze the bonds of the starch. In aspects, the HC1 is from 2M to 3M or from 2M to 5M.

[0035] In one embodiment, the enzymatic treatment can comprise enzymes including, but not limited to, a-amylase, b-amylase, isoamylase, or pullulanase. The conditions of the enzymatic treatment are selected to sufficiently hydrolyze the glycosidic bonds of the starch.

[0036] According to an embodiment, the relative proportions of the RDS, SDS, and RS can be adjusted by varying the conditions of the hydrolyzing treatment. For example, the duration of acid treatment can be greater or less than 5 days. In some aspects, the time of incubation with acid is from about 1 day to about 5 days. Without being limited to any particular theory, a short term incubation will generally result in an increased proportion of SDS and RS to RDS. Whereas relative to shorter term incubation, a longer term incubation will generally result in a relatively decreased proportion of SDS and RS to RDS. In accordance with an embodiment of the method, it is within the scope of the present disclosure to provide for a range of different starches that are formulated to have varying degrees of digestibility, as required. In one embodiment, the method can produce starch particles with specific and controlled digestion characteristics owing to the ability of altering the relative proportions of RDS, SDS, and RS in the produced starch particles.

[0037] According to an embodiment, the duration and conditions of the hydrolysis treatment is such that at the end of the hydrolysis treatment, the weight- average molar mass of hydrolyzed starch remains that of a high molecular weight starch. In aspects, the weight-average molar mass of hydrolyzed starch is about equal to or greater than about 80,000 g/mol. [0038] Without being limited to any particular theory, the hydrolyzing treatment alters the crystalline structure of the starch or the degree of relative crystallinity of the starch to allow manipulation of the digestibility of these starch particles.

[0039] The hydrolyzed starch (e.g. acid or enzyme treated starch) is then formed into starch particles. In one embodiment, the hydrolyzed starch is mixed with an aqueous solution, such as water, to form a hydrolyzed starch slurry. The hydrolyzed starch slurry can be from about 1 to about 70% w/w in an aqueous solution. In another embodiment, the hydrolyzed starch slurry can be from about 5 to about 50% w/w starch in an aqueous solution. In another embodiment, the hydrolyzed starch slurry can be about 20% w/w starch in an aqueous solution.

[0040] In another aspect, the hydrolyzed starch is mixed with an aqueous dispersion comprising the aqueous solution, such as water, and one or more other components that may be poorly soluble in the aqueous solution. In one aspect, the one or more other components comprise polyphenols. In one aspect, the polyphenols are polyphenolic extracts. Exemplary polyphenolic extracts include, but are not limited to, gallic acid, ferrulic acid, caffeic acid, epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, proanthocyanidins, gallotannins or ellagitannins. In another aspect, the polyphenols are from whole plant extracts. Exemplary whole plant extracts include, but are not limited to, green tea extract, grape seed extract, or apple pomace phenolic extract. In one aspect, the concentration of the polyphenols is from about 1 to about 100 mmol/L. The hydrolyzed starch slurry can be from about 1 to about 70% w/w in an aqueous dispersion. In another embodiment, the hydrolyzed starch slurry can be from about 5 to about 50% w/w starch in an aqueous dispersion. In another embodiment, the hydrolyzed starch slurry can be about 20% w/w starch in an aqueous dispersion.

[0041] In one embodiment, the polyphenols and/or polyphenolic extracts will give a desired colour to the starch particles and to the edible composition comprising the starch particles. Specific polyphenols and/or the polyphenolic extracts may also have additional benefits/properties. [0042] Among other properties, the polyphenols and/or the polyphenolic extracts, may at least partially inhibit the digestive enzymes in the digestive system of the individual consuming the edible composition of the present disclosure. Accordingly, the formulation of the edible composition can be adjusted to take into consideration those biological processes that are affected when polyphenols and/or the polyphenolic extracts are included as a component of the edible composition.

[0043] For example, when polyphenols and/or the polyphenolic extracts are incorporated into the starch particles, the starch particles may be formulated or modified so that it can have a slightly less proportion of SDS and/or RS to RDS that would otherwise be necessary in the absence of the added enzyme inhibiting functionality provided by the polyphenols and/or the polyphenolic extracts.

[0044] In another example, when polyphenols and/or the polyphenolic extracts are incorporated into the starch particles, the moisture content of the formed starch particles can be relatively high, and in some embodiments, the moisture content can be greater than about 80% by weight.

[0045] The hydrolyzed starch slurry - that was produced when the hydrolyzed starch was mixed with the aqueous solution or the aqueous dispersion - is then heated until the starch is gelatinized. The duration of the heating can depend, among other things, on the native starch source.

[0046] The gelatinized starch is then formed into starch particles by portioning out an amount of gelatinized starch (using an automated process or manual syringe, for example) and depositing the amounts of gelatinized starch onto a surface. The amount of gelatinized starch deposited onto the surface is selected so that the formed starch particles would be dimensioned from about 2 mm to about 2 cm, from about 5 mm to about 2 cm, or from about 3 mm to about 1 cm, in diameter. In aspects, the selection of the dimensions of the starch particles is done with a view to achieving a desired surface area per unit mass suitable for digestion by a subject after the edible product is consumed. In aspects, the selection of the dimensions of the starch particles is done with a view to achieving a desirable mouthfeel.

[0047] The surface upon which the gelatinized starch is deposited can be cooled and the temperature can range from about room temperature to a cold temperature (e.g. from about 0 to about 25°C). In an aspect, the surface can also be configured to shape the starch particles into any desired shape. In one aspect, the surface is flat or grooved.

[0048] The formed starch particles are then allowed to undergo a retrogradation procedure. In one embodiment, the formed starch particles are cooled at about 0 to about 5°C for about 15 minutes to about 72 hours to allow the starch particles to retrograde.

[0049] In another embodiment, there is provided another method to produce starch particles from native starch. In this embodiment, the native starch is first formed into a starch slurry in an aqueous dispersion or an aqueous solution. The formed starch slurry is then heated until the starch is gelatinized, the gelatinized starch is then formed into starch particles. In this embodiment, however, the formed starch particles are then hydrolyzed by acid or enzymatic treatment, as described herein above. After the hydrolysis step, the hydrolyzed starch particles are then made to undergo a retrogradation procedure, as described herein above.

[0050] In yet another embodiment, there is provided yet another method to produce starch particles from native starch. In this embodiment, the native starch is first formed into a starch slurry in an aqueous dispersion or an aqueous solution. The formed starch slurry is then heated until the starch is gelatinized, the gelatinized starch is then formed into starch particles, and the formed starch particles are then made to undergo a retrogradation procedure, as described herein above. In this embodiment, however, it is the cooled and retrograded starch particles that are hydrolyzed by acid or enzymatic treatment after the retrogradation procedure, as described herein above.

[0051] Upon analysis by the Englyst method to characterize starch digestibility

(Ref: Classification and measurement of nutritionally important starch fractions, PMID: 1330528), the starch particles made in accordance with the methods of the present disclosure comprise about 10 to about 90% slowly digestible starch and about 10 about 90% resistant starch.

[0052] In some embodiments, the rapidly digestible starch comprises less than or about equal to 20% of total starch composition and the slowly digestible starch and/or the resistant starch comprise the remaining percentage of the total starch composition.

[0053] In an aspect, the method further comprises sealing the deposited starch particles during the retrogradation procedure so that the starch particles can retain their moisture. According to an embodiment, the starch particles may have a final moisture content that is less than about 80% by weight.

[0054] According to an embodiment, the method further comprises drying the starch particles. In some embodiments, the drying is carried out at a temperature of about 80 to about 200°C. In some embodiments, the duration of the drying process is from about 5 to about 45 minutes with or without air circulation.

[0055] The slowly digestible starches and resistant starches of the present invention can be used to modulate the glucose release of certain food and beverage products. Food products, both solid and liquid, including beverage products, containing slowly digestible starches and resistant starches are generally healthier than food products containing similar levels of more rapidly digestible starch. The slowly digestible starches and resistant starches, of the present disclosure, in solid and liquid food products would be useful for weight management, the treatment of obesity, and for health maintenance and treatment of diabetic and prediabetic individuals. Solid and liquid food products containing slowly digestible starch and resistant starches may also provide health maintenance and treatment benefits for individuals exhibiting glucose intolerance, insulin resistance, and hyperglycemia. Solid and liquid food products containing slowly digestible starch may also provide health benefits by improving cardiovascular indicators. [0056] In one embodiment, the present invention relates to an edible composition comprising starch particles comprising about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch.

[0057] In aspects, the edible composition is a liquid food product or a solid food product. In aspects, the liquid food product further comprises a beverage base. In aspects, the liquid food product has a beverage base to starch particle ratio of between 1: 1 to 20: 1 (beverage base: starch particles, by mass). In an embodiment, the beverage base is a ready -to-drink beverage. In aspects, the ready -to-drink beverage is a fruit puree, a fruit smoothie, a fruit juice, a coffee preparation, or a tea preparation.

[0058] In aspects, the solid product comprises a solid base to starch particle ratio of between 1: 1 to 20: 1 (solid base: starch particles, by mass). In an embodiment, the solid food product is a cereal bar, a fruit bar, or a protein bar.

[0059] In one embodiment, the edible composition further comprises

polyphenols. In aspects, the polyphenols are polyphenolic extracts. Exemplary polyphenolic extracts include gallic acid, ferrulic acid, caffeic acid, flavonoids such as epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, procyanidins, proanthocyanidins, as well as gallotannins or ellagitannins. In another aspect, the polyphenols are from whole plant extracts. Exemplary whole plant extracts include, but are not limited to, green tea extract, grape seed extract, or apple pomace phenolic extract. In one aspect, the edible composition comprises a concentration of the polyphenols from about 1 to about 100 mmol/L.

[0060] In one embodiment, the present invention relates to edible compositions and methods of making the edible compositions comprising starch particles that are resistant to exposure the usual conditions that are required to minimize or eliminate, for example, microbial contamination, as required by various governmental health and food inspection agencies. Some of these conditions include high heat and/or sterilization treatment, including but not limited to pasteurization. Resistant means that the benefits of the starch particles, as described herein, are not lost upon exposure to heat treatment and/or sterilization treatment. The starch particles made in accordance with the methods of the present disclosure may maintain the desired glycemic response despite heat treatment to about 130 to 140°C. Without being limited to any particular theory, this may be because the methods of the present disclosure produce starch particles having a crystalline structure that is able to withstand the heat treatment. In some embodiments, the crystalline structure is predominantly crystalline amylose.

[0061] EXAMPLES

[0062] The following examples are intended to illustrate but not to limit the invention in any manner, shape, or form, either explicitly or implicitly. While they are typical of those that might be used, other procedures, methodologies, or techniques known to those skilled in the art may alternatively be used.

[0063] Particle Formation and Acid Treatment

[0064] With reference to figures 2A and 2B, native starch from potato (PS) or com (CS) was divided in two groups: group (a) and group (b).

[0065] In group (a), the native starch was heated until the starch was gelatinized.

Once the starch had completely gelatinized, this gelatinized starch was made into starch particles using a syringe deposition method wherein the gelatinized starch was inserted into a syringe and an amount of gelatinized starch was then expelled from the syringe and deposited on a cold surface.

[0066] The expelled amount was such that the deposited starch particle would have a diameter about 5 mm. These deposited particles were then sealed in plastic to retain their moisture and the starch particles were allowed to retrograde overnight at 4°C.

[0067] After retrogradation, the starch particles were subjected to an acid hydrolysis treatment as outlined by Shujun et al. (Shujun, W., Jinglin, Y., Jiugao, Y., Haixia, C. & Jiping, P. The effect of acid hydrolysis on morphological and crystalline properties of Rhizoma Dioscorea starch. Food Hydrocoll. 21, 1217-1222 (2007)). Briefly, formed starch particles were exposed to various concentrations of HC1 (2M or 3M) for 1 to 5 days.

[0068] In group (b), the native starch was first subjected to acid hydrolysis treatment comprising exposing the starch to various concentrations of HC1 (2M or 3M) for 1 to 5 days. The acid treated starch was heated until it was gelatinized. Once the acid treated starch had completely gelatinized, the gelatinized starch was made into starch particles using the syringe deposition method and allow to retrograde overnight, as described above.

[0069] Simulated Digestion

[0070] With reference to figure 3, in vitro digestion (IVD) was performed on all samples following the standard three-stage in vitro digestion method outlined in Minekus et al. (Minekus, M. et al. A standardised static in vitro digestion method suitable for food - an international consensus Food Funct. 5, 1113-1124 (2014)). Briefly, the samples with incubated with alpha-amylase in artificial saliva pH=7 for about 2 minutes (oral phase); then in pepsin in artificial gastric fluid pH=3 for about 2 minutes (gastric phase); and then Pancreatin/ Amyloglucosidase in artificial intestinal fluid, pH=7 for about 2 hours (intestinal phase).

[0071] A glucometer was used to measure glucose concentration over time during intestinal phase (mmol/L).

[0072] The digestion rate was quantified following methods of Sopade and

Gidley (Sopade, P. A. & Gidley, M. J. A Rapid In-vitro Digestibility Assay Based on Glucometry for Investigating Kinetics of Starch Digestion. Starch - Starke 61, 245-255 (2009)).

[0073] Differential Scanning Calorimetry

[0074] Change in Enthalpy (AH) was measured in pW/°C, and maximum temperature (Tm-), onset temperature (To-) and conclusion temperature (Tc-) were measured in °C using a Nano-DSC (D) (TA Instruments, New Castle, DE USA). As described and reviewed by Pratiwi et al. (Pratiwi, M., Faridah, D.N., Lioe, H.N.

Structural changes to starch after acid hydrolysis, debranching, autoclaving-cooling cycles, and heat moisture treatment (HMT): A review (2018) Starch/Staerke, 70, 1-2) enthalpy changes were measured through a temperature range of 5°C to 130°C at a heating rate of l°C/min. Data was processed using Nanoanalyze software (TA

Instruments, New Castle, DE USA).

[0075] Results and Discussion

[0076] Acid treated starch particles increased SDS and RS content

[0077] Figure 4 shows rapidly digestible starch, slowly digestible starch and resistant starch content of starch particles exposed to different acid hydrolysis treatments expressed as a percentage of total starch (TS). Figure 4A shows the results of 2M acid treated particles; figure 4B shows the results of 3M acid treated particles; figure 4C shows the results of particles from 2M acid treated native starch; and figure 4D shows the results of particles from 3M acid treated native starch. Surface Response models were generated (R²=0.86 for Native CS, R²=0.53 for Native PS, R²=0.86 for PS Particles, R²=0.59 for CS Particles), establishing a mathematical relationship (quadratic with interactions) between acid concentration and time of hydrolysis on the one hand, and kinetics of digestion on the other hand. As shown in figure 4, acid hydrolysis treatment (2M or 3M for 1 to 5 days) increased SDS and RS content at the expense of RDS content. The conditions that resulted in minimizing RDS and maximizing SDS have been identified by an asterisk. Overall, this example demonstrates that manipulation of starch structure, through acid hydrolysis treatment, provides an ability to control the glycemic response.

[0078] In some embodiments, the acid treated starch particles have a generally higher SDS content compared to hydrolysis of native starch before starch particle formation. Without being limited to any particular theory, acid treatment of native starch may decrease molar mass amylose by hydrolyzing the amorphous regions of starch granules (richer in amylose) and therefore limit retrogradation (amylose-driven) and formation of RDS and SDS in the final particles. Conversely, acid treatment of formed particles may hydrolyse the amorphous regions of the particles (amylopectin-rich) and proportionally increase their relative crystallinity and their RS and SDS content.

[0079] Particles with High SDS Showed A Relatively Higher Digestion Rate

[0080] With reference to figure 5, various starch particles with high SDS content were plotted against their digestion rate. Figure 5A shows slowly digestible starch (SDS) content of com starch (CS) or potato starch (PS) particles exposed to 2-3M HC1 for 1-5 days against their digestion rate in vitro. Figure 5B shows slowly digestible starch (SDS) content of starch particles made from native com starch (CS) or potato starch (PS) exposed to 2-3M HC1 for 1-5 days then used to form particles, against their digestion rate in vitro. As can be seen, the samples with higher SDS content showed a relatively higher digestion rate. The starch particles being high in RS and RDS in the first place, digestibility can be controlled by accelerating digestion, therefore favoring RDS at the expense of RS. However, extensive hydrolysis may favor RDS and the expense of RDS and RS.

[0081] Gelatinization Enthalpy of Select Particles with High SDS Content

Plotted Against Digestion Rate

[0082] Figure 6 shows the DSC results of samples of the present invention.

Figure 6A shows the gelatinization enthalpy AH (kJ/mol) of com starch (CS) and potato starch (PS) particles exposed to 2M or 3M HC1 for 1-5 days, against their digestion rate in vitro. Figure 6B shows the gelatinization enthalpy AH (kJ/mol) of native com starch (CS) and potato starch (PS) exposed to 2M or 3M HC1 for 1-5 days then used to form particles, against their digestion rate in vitro. As compared to the controls, the samples had higher gelatinization enthalpy which is indicative of increased crystallinity and increased SDS/RS content. Based on these DSC results, it would appear that for the samples of starch according to the present disclosure, it was the amorphous region was hydrolyzed first. The majority of the non-hydrolyzed starch was more crystalline which is relatively more resistant to starch digestive enzymes (Utrilla-Coello, R. G. et al. Acid hydrolysis of native com starch: Morphology, crystallinity, rheological and thermal properties. Carbohydr. Polym. 103, 596-602 (2014)).

[0083] All publications and patents cited in this specification are herein incorporated by reference as if each individual publication or patent were specifically and individually indicated to be incorporated by reference and are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the publications are cited. The citation of any publication is for its disclosure prior to the filing date and should not be construed as an admission that the present disclosure is not entitled to antedate such publication by virtue of prior disclosure. Further, the dates of publication provided could be different from the actual publication dates that may need to be independently confirmed.

[0084] The preceding merely illustrates the principles of the invention. It will be appreciated that those skilled in the art will be able to devise various arrangements which, although not explicitly described or shown herein, embody the principles of the invention and are included within its spirit and scope. Furthermore, all examples and conditional language recited herein are principally intended to aid the reader in understanding the principles of the invention and the concepts contributed by the inventors to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions. Moreover, all statements herein reciting principles, aspects, and embodiments of the invention as well as specific examples thereof, are intended to encompass both structural and functional equivalents thereof. Additionally, it is intended that such equivalents include both currently known equivalents and equivalents developed in the future, i.e., any elements developed that perform the same function, regardless of structure. The scope of the present invention, therefore, is not intended to be limited to the exemplary embodiments shown.

Claims

1. An edible composition comprising starch particles comprising about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch.

2. The edible composition of claim 1 wherein the edible composition is a liquid food product or a solid food product.

3. The edible composition of claim 2 wherein the liquid food product further

comprises a beverage base.

4. The edible composition of claim 3 wherein the liquid food product has a beverage base to starch particle ratio of between 1: 1 to 20: 1.

5. The edible composition of claim 4 wherein the beverage base is a ready-to-drink beverage.

6. The edible composition of claim 5 wherein the ready-to-drink beverage is a fruit puree, a fruit smoothie, a fruit juice, a coffee preparation, or a tea preparation.

7. The edible composition of claim 2 wherein the solid food product has a solid base to starch particle ratio of between 1 : 1 to 20: 1.

8. The edible composition of claim 7 wherein the solid food product is a cereal bar, a fruit bar, or a protein bar.

9. The edible composition of any one of claims 1 to 8 wherein the edible

composition further comprises polyphenols.

10. The edible composition of claim 9 wherein the polyphenols are polyphenolic extracts.

11. The edible composition of claim 10 wherein the polyphenolic extracts are gallic acid, ferrulic acid, caffeic acid, flavonoids such as epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, procyanidins, proanthocyanidins, gallotannins or ellagitannins.

12. The edible composition of claim 10 wherein the polyphenols are from whole plant extracts.

13. The edible composition of claim 12 wherein the whole plant extracts are green tea extract, grape seed extract, or apple pomace phenolic extract.

14. The edible composition of any one of claims 1 to 13 wherein the starch particles have a final moisture content that is less than about 80% by weight.

15. The edible composition of any one of claims 1 to 14 wherein the starch particles which are dimensioned from about 0.5 mm to about 2 cm, from about 2 mm to about 2 cm, or from about 3 mm to about 1 cm, in diameter.

16. The edible composition of any one of claims 1 to 15 wherein the starch particles are resistant to high temperature and/or sterilization treatment.

17. The edible composition of any one of claims 1 to 16 wherein the starch particles further comprises rapidly digestible starch, wherein the rapidly digestible starch comprises less than or about equal to 20% of total starch composition and the slowly digestible starch and/or the resistant starch together comprise the remaining percentage of the total starch composition, preferably the slowly digestible starch and/or the resistant starch together comprise greater or equal to 90% of the total starch composition.

18. Use of the edible composition of any one of claims 1 to 17 for management of weight, for treatment of obesity, or for health maintenance and treatment of diabetic and prediabetic individuals.

19. Use of the edible composition of any one of claims 1 to 17 for the preparation of a formulation for management of weight, for treatment of obesity, or for health maintenance and treatment of diabetic and prediabetic individuals.

20. A method of making starch particles from a native starch, the method comprising: forming a starch slurry of about 1 to about 70% w/w starch in an aqueous dispersion or an aqueous solution;

heating the starch slurry to form gelatinized starch;

forming, from the gelatinized starch, starch particles;

cooling the formed starch particles at about 0°C to about 5°C for about 15 minutes to about 72 hours;

either (a) hydrolyzing a native starch before the step of forming the starch slurry; (b) forming the starch slurry using a native starch and after the step of forming the starch particles, hydrolyzing the formed starch particles; or (c) forming the starch slurry using a native starch and after the step of cooling, hydrolyzing the cooled formed starch particles; and

wherein the conditions of hydrolyzing are such that after the step of hydrolyzing, the starch remains a high molecular weight starch.

21. The method of claim 20 wherein the starch slurry is from about 5 to about 50% w/w starch in the aqueous dispersion or the aqueous solution.

22. The method of claim 20 wherein the starch slurry is from about 20% w/w starch in the aqueous dispersion or the aqueous solution.

23. The method of any one of claims 20 to 22 wherein the step of hydrolyzing a native starch, hydrolyzing the formed starch particles, or hydrolyzing the cooled formed starch particles, comprises incubating the native starch in acid or in enzymes.

24. The method of claim 23 wherein the duration of hydrolyzing is from about 1 day to about 5 days.

25. The method of claim 23 or 24 wherein the acid is a strong acid, preferably the strong acid is HC1.

26. The method of claim 25 wherein the HC1 is 2M to 5M, preferably 2M or 3M.

27. The method of claim 23 or 22 wherein the enzymes is a-amylase, b-amylase, isoamylase, or pullulanase.

28. The method of any one of claims 20 to 27 wherein, after the step of hydrolyzing, the starch has a weight-average molar mass of about equal to or greater than about 80,000 g/mol.

29. The method of any one of claims 20 to 28 wherein the step of forming the starch particles comprises loading the gelatinized starch into a syringe and expelling an amount of the gelatinized starch from the syringe onto a surface.

30. The method of claim 29 wherein the amount of the expelled starch particles is such that the formed starch particles are dimensioned from about 2 mm to about 2 cm, from about 5 mm to about 2 cm, or from about 3 mm to about 1 cm, in diameter.

31. The method of claim 29 or 30 wherein the surface is cold.

32. The method of claim 29 or 30 wherein the surface is from about 0°C to about 25°C.

33. The method of any one of claims 29 to 32 wherein the surface is configured to shape the starch particles into a desired shape.

34. The method of any one of claims 29 to 33 wherein the surface is flat or grooved.

35. The method of any one of claims 20 to 34 wherein the aqueous solution comprises water and the aqueous dispersion comprises water and polyphenols.

36. The method of claim 35 wherein the polyphenols are polyphenolic extracts.

37. The method of claim 36 wherein the polyphenolic extracts are gallic acid, ferrulic acid, caffeic acid, flavonoids such as epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, procyanidins, proanthocyanidins, gallotannins or ellagitannins.

38. The method of any one of claims 35 to 37 wherein the concentration of the

polyphenols is from about 1 to about 100 mmol/L.

39. The method of any one of claims 20 to 38 wherein the cooling at least partially crystallizes the gelatinized starch.

40. The method of any one of claims 20 to 39 wherein the native starch is rice starch, wheat starch, tapioca starch, com starch, potato starch, high amylose com starch, high amylose potato starch or high amylose wheat starch.

41. The method of any one of claims 20 to 40 wherein the method further comprises drying the starch particles.

42. The method of claim 41 wherein the drying is done at a temperature of about 80°C to about 200°C.

43. The method of claim 41 or 42 wherein the drying is done for about 5 to about 45 min with or without air circulation.

44. The method of any one of claims 20 to 43 wherein the method further comprises dusting the starch particles with an anti-caking agent.

45. The method of claim 41 wherein the anti-caking agent is sodium bicarbonate, powdered cellulose, sodium silicate, or silicon dioxide.

46. The method of any one of claims 20 to 45 wherein, after the step of cooling, the starch particles have a moisture content that is less than about 80% by weight.

47. The method of any one of claims 20 to 46 wherein the starch particles comprise about 10 to about 90% of slowly digestible starch and about 10 to about 90% resistant starch.

48. The method of any one of claims 20 to 47 wherein the starch particles comprise rapidly digestible starch that is less than or about equal to 20% of total starch composition and the slowly digestible starch and/or the resistant starch comprise the remaining percentage of the total starch composition, preferably the slowly digestible starch and/or the resistant starch together comprise greater or equal to 90% of the total starch composition.

49. The method of any one of claims 20 to 48 wherein the starch particles are

resistant to high heat required to minimize or eliminate contamination and/or sterilization treatment.

50. Starch particles produced according to the method of any one of claims 20 to 49.

51. An edible composition comprising the starch particles of claim 50.

52. The edible composition of claim 51 wherein the edible composition is a liquid food product or a solid food product.

53. The edible composition of claim 52 wherein the liquid food product further

comprises a beverage base.

54. The edible composition of claim 53 wherein the liquid food product has a

beverage base to starch particle ratio of between 1 : 1 to 20: 1.

55. The edible composition of claim 54 wherein the beverage base is a ready -to-drink beverage.

56. The edible composition of claim 55 wherein the ready-to-drink beverage is a fruit puree, a fruit smoothie, a fruit juice, a coffee preparation, or a tea preparation.

57. The edible composition of claim 56 wherein the solid food product has a solid base to starch particle ratio of between 1 : 1 to 20: 1.

58. The edible composition of claim 57 wherein the solid food product is a cereal bar, a fruit bar, or a protein bar.

59. The edible composition of any one of claims 51 to 58 for management of weight, for treatment of obesity, or for health maintenance and treatment of diabetic and prediabetic individuals.