Highly soluble pea starch as substitute for maltodextrins

Abstract

The present invention relates to a highly soluble legume starch having: oligosaccharides having a degree of polymerization (DP) of 1 and 2 in a content of less than 10% by weight, more preferably less than 6% by weight; oligosaccharides having a DP of 3 to 20 in an amount greater than 50% by weight, more preferably greater than 70% by weight; the present invention relates to a composition comprising at least 90% by weight, more preferably more than 95% by weight, a water solubility, less than 500 cP, more preferably less than 100 cP, and characterized by a ratio of [alpha] 1, 4 / [alpha] 1, 6, as determined by 13C NMR, of between 23% and 32%.

Description

[0001] This invention relates to highly soluble legume starch produced by physical means (a cleaning process) (i.e., without the addition of any chemicals or enzymes), and its use as a substitute for maltodextrin in baked goods, sauces and seasonings, dairy products and beverages, and more specifically for flavoring encapsulation. More preferably, this legume starch is pea starch.

[0002] Therefore, the present invention relates to a method that essentially involves cooking a starch-water mixture under certain conditions. Background Technology

[0003] Undeniably, starch is the most important polysaccharide in the human diet. In terms of the abundance of organic compounds in the biosphere, starch is second only to cellulose.

[0004] The appeal of starch in the food and non-food industries can be attributed to its inexpensive, abundant, biodegradable, and non-toxic properties. Starch is readily available from a variety of plant sources, such as cereals, legumes, roots and tubers, and immature fruits.

[0005] The need for modification of natural starch stems from its inherent defects.

[0006] Natural starch is insoluble in water, easily degrades, and is accompanied by associated dehydration shrinkage. Most importantly, gels and pastes made from natural starch are unstable under high temperature, pH and mechanical stress.

[0007] Due to the inherent deficiencies of these natural starches, modification is needed to better suit their functional and physicochemical properties for appropriate industrial applications.

[0008] Starch modification can be broadly categorized into physical modification, chemical modification, biotechnology modification, and enzyme modification, or combinations thereof, appropriately termed dual modification.

[0009] Among them, physical methods are more acceptable because they are usually chemical-free and therefore considered safer for human consumption.

[0010] For environmentally friendly applications, the physical modification of starch is more closely linked to emerging concepts such as "clean label," "green technology," or "sustainable technology."

[0011] In fact, consumers are demanding greater transparency regarding the ingredients in their food, which is driving increased interest in ingredients that meet "clean label" guidelines.

[0012] The cleaning label can be any one or more of the following:

[0013] -Identifiable ingredients

[0014] -Minimum ingredients

[0015] -Minimum processing

[0016] - No one caused the score

[0017] - No preservatives

[0018] -Non-GMO

[0019] -All Natural

[0020] -organic

[0021] -country of origin

[0022] Physical modification of starch can improve water solubility and reduce particle size. This method involves treating starch particles under different combinations of temperature / humidity, pressure, shear, and radiation.

[0023] Physical modification also includes mechanical milling to change the particle size of starch particles.

[0024] Physical modification techniques are often preferred because they do not involve any chemical treatments that could be harmful to human use.

[0025] Starch physical modification is broadly classified into those thermal modifications and other non-thermal modifications.

[0026] The thermal process involves:

[0027] -The thermal processes that disrupt the starch particle structure (all pregelation processes), and

[0028] -The thermal processes that retain the particles (hydrothermal processes: annealing and hot-wet treatment).

[0029] In pregelation, the particle structure of starch is completely destroyed by heating, resulting in depolymerization and fragmentation, and thus the molecular integrity of starch is not preserved.

[0030] Therefore, pregelatinized starch is starch that has undergone gelatinization and thus depolymerization and fragmentation, and whose particle structure is completely destroyed by cooking. The pregelatinization process is achieved through drum drying, spray drying, and extrusion cooking. Properties associated with pregelatinized starch allow it to dissolve immediately in cold water without heating.

[0031] Due to the harsh processing (gelatinization and vigorous drying) used to obtain pregelatinized starch, it is porous and has a higher water absorption index and water solubility index than natural starch.

[0032] However, there are certain limitations associated with pregelatinized starch, which reduces its use in some foods.

[0033] These include granular texture, inconsistency, and weak gelation. The development of particulate cold-water swellable starch has overcome these shortcomings. While maintaining its particle integrity, particulate cold-water swellable starch can exhibit cold-water thickening, with higher viscosity, more uniform texture, and higher clarity than pregelatinized starch, and has greater processing tolerance.

[0034] Unlike natural starch, they rapidly absorb water and increase their viscosity at ambient temperatures. This useful property makes them suitable for a range of products synthesized at low temperatures that contain heat-labile components (e.g., vitamins and colorants) and for use in fast food products.

[0035] Undeniably, the functions and physicochemical properties of various modified starches determine their applications in the food industry.

[0036] Unlike pregelation, annealing and hot-wet treatment involve heating starch in water at a temperature below the gelation temperature (GT) and above the glass transition temperature (Tg). Therefore, the particle structure of the starch is preserved.

[0037] Starch modification is an evolving industry with a wide range of possibilities for generating new starches that include new functions and value-added properties as required by industry.

[0038] In the field of this invention, the applicant is particularly interested in the preparation of maltodextrin and its use in food applications.

[0039] Maltodextrins are polymers of sugars composed primarily of glucose units linked by α-1,4 glycosidic bonds. These starch derivatives are typically produced from corn, rice, potato starch, or wheat starch. Even though they are derived from plants, they are highly processed.

[0040] Maltodextrin is actually obtained classically from enzymatic hydrolysis, with or without acid, but to a lesser extent than required for the production of starch syrup.

[0041] Depending on the production method and source, maltodextrins can be obtained at different molecular weights as dextran equivalents (DE). DE represents the percentage of glycoside-bound hydrolysis, thus indicating their reducing power.

[0042] Maltodextrin offers good oxidative stability for oil encapsulation but exhibits poor emulsifying ability, emulsion stability, and low oil retention. Maltodextrins with a DE of 10 to 20 are suitable as coating materials and show the highest flavor retention. Furthermore, maltodextrin offers a good trade-off between cost and effectiveness, is mild in flavor, has low viscosity at high solids ratios, and is water-soluble, thus contributing to its attractive value in encapsulation. Therefore, maltodextrin is a versatile ingredient in the food industry and has numerous applications, including food and beverages, sauces and seasonings, baked goods, dairy products, flavoring encapsulation, etc.

[0043] However, it is not consumer- and consumer packaged goods (CPG) friendly due to labeling issues. In fact, the classic method of hydrolyzing starch requires acids and / or enzymes to chemically break down the long chains of starch molecules to increase solubility. Problems associated with these technologies include:

[0044] 1. Adding foreign components to natural materials,

[0045] 2. High operating costs due to the addition and removal of foreign components.

[0046] 3. Additional financial costs associated with adding and removing steps.

[0047] For this reason, a number of alternatives have been developed to produce starch derivatives with similar functionality (such as solubility) to maltodextrin, which have high market potential based on customer feedback and marketing strategies.

[0048] However, if various commercial products such as cold water soluble starch or pregelatinized starch are available, their solubility is generally much lower than that of maltodextrin, and therefore they cannot replace the use of maltodextrin.

[0049] Therefore, in order to respect consumers' wishes, "clean label" solutions need to be provided in the relevant fields.

[0050] The applicant found that the solution involved using physical methods to hydrolyze starch to eliminate the addition of chemicals / enzymes, resulting in clean-label soluble starch that meets consumer demand and market trends for green products.

[0051] However, there is no highly effective technological alternative for producing maltodextrin-like products in the existing technology.

[0052] The most commonly used heat treatment is for the preparation of pregelatinized starches. As already discussed, these starches have been fully cooked, i.e., gelatinized, and dried under conditions that allow little or no molecular recassociation. They are described as cold-water soluble, although many such products will develop additional viscosity when their aqueous dispersions are heated. However, even if the resulting pregelatinized starch is more soluble, this solubility is low, typically less than 50%, which is significantly different from the solubility of maltodextrin.

[0053] Depolymerization also occurs during the pregelation process. The molecular weights of amylose and amylopectin typically decrease by 1.5-fold and 2.5-fold, respectively. However, this thermal process requires high-temperature treatment (>140°C during 2 to 12 hours) and the resulting heated starch solution contains high concentrations of compounds exhibiting low degree of polymerization (DP) content (DP<6).

[0054] In this regard, physical non-thermal processes have been developed: direct microwave, milling, or ultrasonic treatment of natural starch.

[0055] However, it is difficult to implement on an industrial scale the use of microwave heating of starch particles in aqueous slurries.

[0056] Milling mechanically reduces the particle size of starch to less than 20 micrometers, but it is extremely energy-intensive. Furthermore, achieving the desired solubility is impossible.

[0057] Therefore, there remains a very strong interest in finding new processing methods for producing maltodextrin substitutes. Summary of the Invention

[0058] This invention relates to highly soluble legume starch, which has the following characteristics:

[0059] - Oligosaccharides with a degree of polymerization (DP) of less than 10% by weight, preferably less than 7% by weight, and preferably less than 6% by weight,

[0060] - Oligosaccharides with a content between 30% and 40% by weight and a DP of 3 to 20.

[0061] - Water solubility greater than 95% by weight, more preferably greater than 98% by weight

[0062] - Viscosity less than 500 cP, more preferably less than 200 cP

[0063] And it is characterized by:

[0064] -pass 13 The α-1,4 / α-1,6 ratio, determined by C NMR, is between 23% and 32%.

[0065] The present invention also relates to a method for preparing highly soluble starch, the method comprising, more preferably, the following steps:

[0066] -Preparation of starch slurry,

[0067] - The starch slurry was gelled.

[0068] -Cook the gelatinized starch.

[0069] - The resulting thermal decomposition solution is purified with activated carbon, filtered, and evaporated.

[0070] -Dry and concentrate the solution to obtain a powder product.

[0071] The present invention also relates to the use of the highly soluble legume starch of the present invention as a substitute for maltodextrin in food applications.

[0072] The present invention also relates to its use as a substitute for maltodextrin in the preparation of baked goods, sauces and seasonings, dairy products and beverages, more specifically for flavor encapsulation (as a carrier for flavor encapsulation), and also for the preparation of fat-free vinaigrettes or powdered beverage formulations such as tropical punch blends or energy drinks. Detailed Implementation

[0073] This invention relates to highly soluble legume starch, which has the following characteristics:

[0074] - Oligosaccharides with a degree of polymerization (DP) of less than 10% by weight, preferably less than 7% by weight, and preferably less than 6% by weight,

[0075] - Oligosaccharides with a content between 30% and 40% by weight and a DP of 3 to 20.

[0076] - Water solubility greater than 95% by weight, more preferably greater than 98% by weight

[0077] - Viscosity less than 500 cP, more preferably less than 200 cP

[0078] And it is characterized by:

[0079] -pass 13 The α-1,4 / α-1,6 ratio, determined by C NMR, is between 23% and 32%.

[0080] According to the present invention, the legume starch has an amylose content ranging from 25% to 60% (dry / dry) and can be exemplified as pea starch, particularly pea starch having an amylose content of at least 30% but less than 50% by weight.

[0081] With such a distribution (which, to the applicant’s knowledge, has never been described), the highly soluble starch or extremely soluble starch according to the invention has a distribution comparable to that of maltodextrin (in terms of DP content, solubility, and viscosity), but has a structure almost identical to that of natural starch (in terms of the α1,4 / α1,6 ratio), from which highly soluble starch or extremely soluble starch is prepared.

[0082] This is also noteworthy by the fact that the highly soluble starch according to the invention is blue in the starch iodine test, while conventional maltodextrin is typically brown, as is known to those skilled in the art.

[0083] The measure of oligosaccharide content with a degree of polymerization (DP) of 1 and 2, and 3 to 20, is typically determined using industry-standard carbohydrate analysis methods.

[0084] Therefore, high-performance liquid chromatography (HPLC) was used with an ion exchange resin in the form of silver (AMINEX HPX-42A resin). The area at a specific retention time corresponding to a single DP value was recorded; the percentage of that particular DP was calculated as follows:

[0085] % DP = Area of ​​a single DP / Sum of the areas of all DPs

[0086] The highly soluble pea starch contains oligosaccharides with a degree of polymerization (DP) of 1 and 2 in an amount of less than 7% by weight, more preferably less than 5% by weight, and oligosaccharides with a DP of 3 to 20 in an amount between 30% by weight and 40% by weight, more preferably between 30% by weight and 35% by weight.

[0087] In contrast, the maltodextrin GLUCIDEX commercialized by the applicant... ® 12 contains approximately 3% DP1 and DP2 oligosaccharides and approximately 44% oligosaccharides with DPs of 3 to 20.

[0088] The statement "oligosaccharide content of DP1 and DP2" refers to the total weight of oligosaccharides in DP1 and DP2.

[0089] In the embodiments, the degree of polymerization (DP) of the highly soluble pea starch according to the present invention is 1 or 2, and the content is at least 4% or preferably at least 4.5%.

[0090] In the embodiments, the degree of polymerization (DP) of the highly soluble pea starch according to the present invention is 1 or 2, and the content is between 4% and 7%, preferably between 4% and 6%, and more preferably between 4% and 5%.

[0091] Solubility can be determined by any method used for determining solubility. Such methods are well known to those skilled in the art. The solubility has been determined by the method given in Example 1.

[0092] Highly soluble pea starch exhibits a water solubility of greater than 95% by weight, more preferably greater than 98% by weight.

[0093] In contrast, maltodextrin GLUCIDEX ® 12 exhibits a water solubility of more than approximately 93%.

[0094] The viscosity is Brookfield viscosity, preferably Brookfield viscosity measured at 15°C. Viscosity is preferably measured on a dispersion with a starch concentration of 45% w / w. The viscosity was measured using the method given in Example 1.

[0095] The procedure is as follows:

[0096] - Dissolve the sample to be tested in deionized water at room temperature to form a solution with a concentration of 45% w / w;

[0097] - Use a Brookfield II viscometer, with a #21 spindle, at 15°C, to measure viscosity according to the manufacturer's specifications;

[0098] - Temperature is controlled using a circulating water bath.

[0099] Highly soluble pea starch exhibits a viscosity of less than 200 cP, more preferably less than 100 cP.

[0100] In contrast, maltodextrin GLUCIDEX ® 12 exhibits a viscosity of less than approximately 600 cP.

[0101] In comparison, the applicant's commercially available natural pea starch N735 has a viscosity of 20 cP.

[0102] Preferably, the highly soluble pea starch exhibits a viscosity greater than 30 cp, and more preferably greater than 40 cp.

[0103] Preferably, the highly soluble pea starch exhibits a viscosity between 30 cP and 700 cP, more preferably between 40 cP and 600 cP, and even more preferably between 40 cP and 500 cP.

[0104] However, if the highly soluble pea starch of the present invention exhibits all these characteristics shared with maltodextrin, then it is certainly not maltodextrin.

[0105] In fact, the highly soluble pea starch of the present invention retains the natural form / structure of natural pea starch, while conventional maltodextrin has a different starch structure.

[0106] It can be obtained through NMR 13 The ratio of α1,4 / α1,6 in macromolecules determined by C is used to illustrate this.

[0107] The NMR followed 13 The C method is based on the following work:

[0108] -Gidley, Michael J., (1985), Carbohydrate Research, Vol. 139, pp. 85-93.

[0109] -Schmitz, Sarah. (2009), Macromolecular Bioscience, Vol. 9, pp. 506-514.

[0110] -Tizzotti, Morgan J., (2011), Journal of Agricultural and Food Chemistry, Vol. 59, No. 13, pp. 6913-6919.

[0111] The procedure is as follows:

[0112] 1. Weigh 10 ± 0.05 mg of starch sample.

[0113] 2. Add 1.0 mL of anhydrous DMSO-d6 containing 0.5% (w / w) LiBr to the sample.

[0114] 3. Add a small stirring rod to the mixture and incubate the sample overnight at 80°C and 300 rpm.

[0115] 4. Cool the sample to room temperature.

[0116] 5. Add 0.5 mL of sample mixture to the NMR tube.

[0117] 6. Add 5.66 μL of deuterated trifluoroacetic acid (d1-TFA) to the medium before NMR measurement.

[0118] 7. Analyze the sample using 1H NMR and obtain the 1H NMR spectrum at 70℃:

[0119] The conditions are as follows:

[0120] -500.13MHz Larmor frequency

[0121] -12 μs 30° pulse

[0122] Repetition time: -15.07s

[0123] Acquisition time: -3.07s

[0124] -12s relaxation delay

[0125] -300 scans.

[0126] For measurement:

[0127] -α-1,4 bond: peak intensity at 5.11 ppm,

[0128] -α-1,6 bond: peak intensity at 4.75 ppm,

[0129] Therefore, the highly soluble pea starch of the present invention has an α-1,4 / α-1,6 ratio between 23% and 32%.

[0130] By comparison:

[0131] Natural pea starch exhibits a typical α-1,4 / α-1,6 ratio of approximately 24% to 31%.

[0132] -GLUCIDEX ® 12 has an α-1,4 / α-1,6 ratio of approximately 22% to 23%.

[0133] This product can be advantageously used in food applications, such as for flavoring encapsulation, as illustrated below.

[0134] This invention also relates to a method for preparing highly soluble starch, the method comprising or consisting of the following steps:

[0135] -Preparation of starch slurry,

[0136] - The starch slurry was gelled.

[0137] -Cook the gelatinized starch.

[0138] - The resulting thermal decomposition solution is purified with activated carbon, filtered, and evaporated.

[0139] -Dry and concentrate the solution to obtain a powder product.

[0140] According to the present invention, the term "highly soluble starch" means that the water solubility of starch (in water at about 20°C) is greater than 95% by weight, more preferably greater than 98% by weight.

[0141] The method for preparing highly soluble starch is preferably used to prepare highly soluble starch as described above.

[0142] First step Preparation of starch slurry.

[0143] The starch in the initial starch-water mixture is expressed as 5% to 30% by weight relative to the total weight of the starch-water mixture.

[0144] The starch in the initial starch-water mixture may be expressed as 5% to 20% by weight relative to the total weight of the starch-water mixture, or more preferably 15% to 30% by weight relative to the total weight of the starch-water mixture, representing 10% to 35% by weight. Objective: To prepare a slurry containing 15% by weight of starch relative to the total weight of the slurry. The mixture is then stirred at room temperature as described in the examples.

[0145] The starch used in this step can be derived from legumes.

[0146] For the purposes of this invention, the term "leguminous plants" should be understood to mean any plant belonging to the family Mimosaceae or Fabaceae, and in particular any plant belonging to the family Fabaceae, such as peas, lentils, broad beans, fava beans, lentils, alfalfa, clover, or lupins.

[0147] This definition specifically includes all plants described in any of the tables contained in the article by R. HOOVER et al. entitled “Composition, Structure, Functionality and Chemical Modification of Legume Starches: a review” (Can. J. Physiol. Pharmacol. 1991, Vol. 69, pp. 79-92).

[0148] Preferably, the starch used in this invention is natural legume starch. Therefore, the starch used in preparing the starch slurry is preferably natural legume starch.

[0149] Preferably, the legume is selected from the group consisting of peas, broad beans, lentils, fava beans and horse broad beans, and more preferably pea or broad bean starch.

[0150] Advantageously, it is a pea, and the term "pea" is considered in its broadest sense in this article, and specifically includes:

[0151] - All wild varieties of "smooth-skinned peas", and

[0152] - All mutant varieties of "smooth-skinned peas" and "wrinkled-skinned peas" ("wrinkled peas"), regardless of the intended use of the varieties (human consumption, animal nutrition and / or other uses).

[0153] The mutant varieties mentioned are particularly those referred to as “r mutants,” “Rb mutants,” “rug 3 mutants,” “rug 4 mutants,” “rug 5 mutants,” and “LAM mutants,” as described by C-liter Heydley et al. in their article entitled “Developing novel pea wrinkled pea,” Proceedings of the Isgri Symposium of the Industrial Biochemistry and Biotechnology Group of the Biochemical Society, 1996, pp. 77–87.

[0154] According to another favorable variant, a legume is a plant, such as various peas or broad beans, in which a given seed contains at least 25%, preferably at least 40%, of starch by weight (dry / dry).

[0155] The term "leguminous starch" or "leguminous starch" is understood to mean any composition extracted in any way from legumes, and particularly from Fabaceae, and having a starch content greater than 40%, preferably greater than 50%, and even more preferably greater than 75%, these percentages being expressed as dry weight relative to the dry weight of the composition.

[0156] Advantageously, the starch content is greater than 90% (dry / dry). It can be particularly greater than 95%, including greater than 98%.

[0157] The starch slurry is then gelled and then cooked at a higher temperature for various purposes:

[0158] -Swelling starch particles

[0159] - To gelatinize the starch and / or loosen the starch rolls.

[0160] -Reduce the size and structure of starch by partially breaking down long molecular chains.

[0161] Second step : Gelation of starch slurry.

[0162] Gel starch can be obtained by processing the gelation of hydrothermal natural starch, particularly by steam cooking, jet cooking, cooking on drums, cooking in kneader / extruder systems, followed by drying, for example, in an oven, by hot air on a fluidized bed, by atomization, by extrusion, or by freeze-drying.

[0163] Starch slurry is typically heated in a starch cooker at a flow rate of 500 g / min at a temperature between 140°C and 150°C.

[0164] Third step Cooking of gelatinized starch under pressure

[0165] This cooking step or further heating treatment is typically performed at temperatures up to 190°C and pressures between 1.43 bar and 12.55 bar.

[0166] The cooking step or further heating treatment can be performed at a temperature of up to 175°C and a pressure between 1.43 bar and 12.55 bar, more preferably between 4.16 bar and 8.94 bar.

[0167] The cooking process can be performed, for example, at a temperature of 175°C ± 2°C and a pressure between 4.16 bar and 8.94 bar.

[0168] The cooking step can be performed, for example, at a temperature of 180°C ± 2°C and a pressure between 9 bar and 9.5 bar.

[0169] The cooking or further heating treatment is typically performed for 5 minutes to 2 hours. When the cooking step or further heating treatment is carried out at a temperature up to 175°C and a pressure between 1.43 bar and 12.55 bar, more preferably between 4.16 bar and 8.94 bar, it can preferably be performed for 30 minutes to 2 hours, more preferably 30 minutes to 60 minutes.

[0170] When the cooking step or further heating treatment is carried out at a temperature of up to 190°C and a pressure between 1.43 bar and 12.55 bar, more preferably between 4.16 bar and 8.94 bar, it is preferably performed for 5 to 30 minutes, more preferably 5 to 20 minutes.

[0171] Step 4: Refining and drying

[0172] The resulting product was purified with activated carbon, filtered, and evaporated to a solution with a dry solid concentration of 30%-70%.

[0173] The decolorized and then evaporated syrup can be dried into powder form using dryers such as drum dryers, rapid dryers, spray dryers, and freeze dryers.

[0174] For example, by spray drying, the inlet temperature is between 150°C and 250°C, more preferably between 170°C and 190°C; and the outlet temperature is between 60°C and 120°C, more preferably between 80°C and 90°C.

[0175] Therefore, the product obtained is:

[0176] It is soluble in cold water, meaning its solubility is ≥95% at around 20℃.

[0177] - It has similar properties to maltodextrin (oligosaccharide DP2-DP20 content >30%).

[0178] - It is a clean label (no chemical additives).

[0179] The present invention also relates to the use of the highly soluble legume starch of the present invention as a substitute for maltodextrin in food applications, particularly for the preparation of baked goods, sauces and seasonings, dairy products and beverages, and more specifically as a carrier for flavor encapsulation, for the formulation of fat-free vinaigrettes and for the preparation of powdered beverage formulations. Attached Figure Description

[0180] one Figure 1 The pilot-scale process developed in accordance with this invention is presented.

[0181] Example

[0182] The invention will be better understood by following the examples, which are given for illustrative purposes only and are not intended to limit the scope of the invention as defined by the appended claims.

[0183] Example 1. Preparation of soluble pea starch according to the present invention

[0184] Materials and equipment

[0185] • Raw material: Natural pea starch N735 (commercialized by the applicant).

[0186] • A commercially available starch / jet cooker (also known as a laboratory starch cooker) by Bottom Line Process Technologies, Inc.

[0187] • Pressure cooker: Parr Pressure Reactor 8500

[0188] • Refining and spray drying equipment

[0189] Process, guiding procedures and operating conditions

[0190] process :

[0191] Pea starch and water are mixed in a mixing tank, liquefied by passing through a starch / jet cooker, and further heat-treated in a pressure reactor. After cooking, the solution is refined and then spray-dried to form soluble pea starch powder.

[0192] Booting procedures and operating conditions :

[0193] The steps and related operating conditions for the bootloader are listed below:

[0194] - 4500g of pea starch, commercialized by the applicant under number N735, will be mixed with 25,500g of tap water to form 30,000g of starch-water mixture, with a starch concentration of approximately 15% by weight.

[0195] - Stir the mixture in a mixing tank for 15 minutes at room temperature.

[0196] - The starch slurry is pumped through a starch cooker at a flow rate of 500 g / min, and the heating temperature is 140℃~150℃.

[0197] - Discharge the gelled starch slurry into a pressure vessel;

[0198] Continue cooking the starch slurry in the pressure vessel to 175°C and maintain for 45 minutes.

[0199] - Flash distill the product into a flash tank and cool the distilled solution to 80°C using a cooling coil.

[0200] - The product is purified with 0.1%~0.3% activated carbon for 45 minutes and then passed through a filter press.

[0201] - Spray-dry the solution at an inlet temperature of 190°C and an outlet temperature of 90°C.

[0202] Sample Analysis

[0203] Solubility measurement (MERDGN 1002EN)

[0204] - Collect 45 ml of sample in a 50 ml centrifuge tube at room temperature.

[0205] Centrifuge the sample at 3000g for 5 minutes.

[0206] Collect the supernatant and weigh it.

[0207] - Dry the supernatant at 130°C for two hours until constant weight is achieved.

[0208] - Cool and dry the supernatant in a desiccator for 1 hour at room temperature.

[0209] - Calculate solubility by answering the following questions:

[0210] 100 * m * (M+P) / (P1 * P)

[0211] Where: M = mass of water, P = mass of starch, P1 = mass of supernatant, m = mass of dried residue.

[0212] - For accuracy, repeat the measurement twice.

[0213] P and M refer to the masses of water and starch in the sample, respectively. These were measured before spray drying.

[0214] Dextran equivalent and carbohydrate distribution measurement

[0215] - Determine the dextran equivalent (DE) of the pilot sample using any method well-known in the art. (MERDGN 1005EN)

[0216] - Carbohydrate distribution was determined by HPLC with a double silver column.

[0217] Viscosity measurement

[0218] - Dissolve the pilot product in deionized (DI) water at room temperature to form a solution with a concentration of 45% w / w;

[0219] The viscosity of the solution was measured using a Brookfield II viscometer with a #21 spindle at 15°C, according to the manufacturer's specifications.

[0220] - The temperature of the solution is controlled by a circulating water bath.

[0221] Results and discussion

[0222] Dextrin equivalents and carbohydrate distribution

[0223] Dextrin equivalent (DE) and carbohydrate distribution (DP) are important information about the characteristics of pilot-scale products.

[0224] Labeled as soluble starch, the product must be soluble in cold water (approximately 20°C) and also contain low concentrations of DP1 and DP2. For feasibility studies, the current requirements for the product are: DE≈12, and DP1 + DP2 < 5%.

[0225] Table 1 shows the DE and DP measurements of different batches of pilot-scale products. Commercial maltodextrin with DE12 (from the applicant's commercialized GLUCIDEX) ® The DE and DP results of 12) are also included in the table for comparison.

[0226] Table 1. Results of DE and DP measurements

[0227]

[0228] The results showed that the DE value of the pilot product was about 11, ranging from 10.9 to 11.1; and the DP1+DP2 concentration was about 4%-5% (between 4.28% and 4.88%).

[0229] The DP distribution of the pilot product is similar to that of the reference sample.

[0230] solubility

[0231] Another important characteristic parameter is solubility. Soluble starch should have sufficiently high solubility in cold water in order to be used as a substitute for maltodextrin.

[0232] Viscosity

[0233] Viscosity directly affects product suitability and processability; it also reflects the impact of processing conditions on the final product. Currently, the viscosity of commercial DE12 samples is used as a reference. Comparative studies...

[0234] The data is shown in Table 2 below. :

[0235]

[0236] *ND: Undetermined, because maltodextrin does not contain starch (iodine test does not show a blue color).

[0237] It is clear that the highly soluble pea starch of the present invention is functionally maltodextrin and structurally starch.

[0238] Example 2. Comparison of GLUCIDEX in flavor ingredient packaging ® Evaluation of 12 Highly Soluble Pea Starch

[0239] The purpose here is to compare the soluble pea starch of Example 1 with GLUCIDEX in terms of flavor encapsulation function. ® 12.

[0240] One major application of maltodextrin is as a cost-effective alternative to gum arabic in film-forming wall materials used to encapsulate oils / flavors during spray drying.

[0241] One potential solution is to dissolve an equivalent amount of glucose into the target maltodextrin, which is expected to have similar functionality in this application. Previous work has tested soluble starch samples on a pilot-scale in spray-drying applications. For this purpose, orange oil was used as a commonly used test flavoring in spray-drying applications, leading to the development of a basic spray-dried flavoring formulation. To ensure a functional baseline, the literature was consulted to determine the optimal levels of maltodextrin relative to gum arabic, wall material relative to core material, and solids relative to water. Additionally, optimal input and output temperatures were selected to maximize oil retention without breaking the encapsulated flavoring shell.

[0242] Soluble starch samples were compared with maltodextrin control samples using routine analyses, including color, pH, particle size, and solution viscosity (before and after homogenization). Since a key function of spray-dried flavor compounds is anti-oxidation, oxidation studies were performed at different temperatures, while monitoring peroxide value and free fatty acids, to observe whether the soluble starch samples exhibited similar or better oxidative stability than the maltodextrin control samples.

[0243] Table 3: Preparation and Processing Procedures

[0244]

[0245] Table 4 :

[0246]

[0247] program :

[0248] 1) Water by weight. Heat to 60°C while mixing at 2000 rpm using a Silverson high-shear mixer with a fine mesh screen.

[0249] 2) Slowly add glucide × 12 and gum arabic while increasing the mixer speed from 2000 -> 4000 -> 6000 -> 9000 rpm for 15 minutes, or until fully dispersed.

[0250] 3) Add orange oil at 9000 rpm for 5 minutes until a coarse emulsion is formed.

[0251] 4) Homogenize at 500 bar in a two-stage high-pressure homogenizer (stage 1 450, stage 2 50).

[0252] 5) Transfer the homogenized solution to a pot and heat it to 60°C while stirring the pot at 250 rpm.

[0253] 6) Pump the solution into a GEA mobile small pilot-scale spray dryer and spray dry it at an input temperature of 185°C and an output temperature of 90°C.

[0254] Analysis program

[0255] color

[0256] Equipment: Konica Minolta CM-5 colorimeter

[0257] Test conditions: D65 / 10°

[0258] Measurement scale: CIELAB scale

[0259] 1) Connect the colorimeter and perform white plate calibration.

[0260] 2) Place the flat portion of the sample on the 30mm equipment opening to completely cover the color measurement area.

[0261] 3) Place the sample on the colorimeter and press "Measure".

[0262] 4) Once the color measurement has been performed, repeat steps 3-4 for a total of 3 measurements, changing the position of the plant-based cheese sample to record more representative color measurements.

[0263] 5) Record the average of the three color measurements.

[0264] 6) Compare the ΔE* values ​​between the three samples to see if there are any perceptible color differences between them.

[0265] AE size:

[0266] • <= 1.0: Imperceptible to the human eye

[0267] •1-2: Can be detected through close observation

[0268] •2-10: Easily noticeable

[0269] •11-49: More similar colors than opposite colors

[0270] •100: Colors completely opposite

[0271] Solids % / Moisture % (Oven dried)

[0272] Equipment: VWR forced-ventilation oven, chemical desiccator with Dri-Rite, analytical balance, 43mm aluminum pan (for drying and storage), oven gloves and clamps. Test conditions: Oven temperature and time 100℃, 24 hours; desiccator time 1 hour. Measurement scale / unit: wet basis moisture content (%)

[0273] 1) Obtain dried aluminum discs from the dryer using Dri-Rite.

[0274] 2) Place the aluminum pan on the analytical balance and record the weight in grams (P), then tare the balance.

[0275] 3) Add about 4 grams of sample to the aluminum pan and record the weight of both the aluminum pan and the sample (W1) – this is part of the initial weight.

[0276] 4) Weigh three samples of each test variable. Label each sample with a unique label to track weight changes.

[0277] 5) Add the samples to the baking tray and place them in a VWR forced ventilation oven set to 100°C for 24 hours (place them on the bottom rack to prevent the fan from blowing the powder around).

[0278] 6) After 24 hours, grab the oven gloves and clamps, then carefully remove the sample from the oven and transfer it to a desiccator containing Dri-Rite.

[0279] 7) Allow the sample to dry further in the desiccator for at least 1 hour, then remove it.

[0280] 8) Weigh each aluminum pan with a unique label and record the weight—this weight is part of the final weight (W2).

[0281] 9) Calculate the wet basis moisture content (%) for each sample using the following equation:

[0282] Moisture content % (wet weight) = [[(W1 - P) - (W2 - P)] / (W1 - P)] * 100

[0283] Density / Specific Gravity - Uncompacted

[0284] Equipment: Analytical balance, 250mL graduated cylinder, funnel, and density cup (50cm³ volume) of a 1800-type film thickness meter.

[0285] Test conditions: Sample temperature 20℃-23℃

[0286] Measurement scale / unit: specific gravity (g / mL)

[0287] Powder-based measurements :

[0288] 1) Place a 250mL graduated cylinder on the analytical balance and tare the balance.

[0289] 2) Using a funnel, fill the graduated cylinder approximately to the 200mL to 220mL mark with the powder sample.

[0290] 3) Record the weight (in grams) displayed on the analytical balance and the volume (in mL) in the graduated cylinder.

[0291] 4) Divide the weight (g) by the recorded volume (mL) to obtain the specific gravity (g / mL).

[0292] 5) Perform this test three times for each powder sample.

[0293] Liquid-based measurement :

[0294] 1) Place the 50cm³ Elcometer density cup on the analytical balance and tare the balance (cover the density cup).

[0295] 2) Remove the lid from the density cup and fill the cup with the liquid sample near the top edge of the container.

[0296] 3) Replace the lid on the density cup and gently press it down to allow excess liquid to drain from the container.

[0297] 4) Thoroughly clean the sides of the sealed density cup with paper towels.

[0298] 5) Record the weight (in grams) shown on the analytical balance and the volume (in mL) of the density cup containing the sample (i.e., 50 mL).

[0299] 6) Divide the weight (g) by the recorded volume (mL) to obtain the specific gravity (g / mL).

[0300] 7) Perform this test three times for each liquid sample.

[0301] Density / Specific Gravity - Tapped (Powder Measurement)

[0302] Equipment: Analytical balance, 250mL graduated cylinder, funnel, and quantumcrime ® AUTOTAP AT-6

[0303] Test conditions: Sample temperature 20℃-23℃, 1300 light taps.

[0304] Measurement scale / unit: specific gravity (g / mL)

[0305] 1) Place a 250mL graduated cylinder on the balance and tare the balance.

[0306] 2) Using a funnel, fill the graduated cylinder approximately to the 200mL to 220mL mark with the powder sample.

[0307] 3) Record and analyze the weight (in grams) displayed on the balance.

[0308] 4) Cover the top of the graduated cylinder tightly with your hand and turn the graduated cylinder back and forth 6-7 times.

[0309] 5) Slowly straighten the measuring cylinder to ensure the powder bed surface is level and avoid tapping the powder (causing compression).

[0310] 6) Clamp the measuring cylinder firmly onto the platform of the Autotap AT-6.

[0311] 7) Set the number of taps to 1300. Press Start on your device.

[0312] 8) Once the process is complete, record the final volume (mL) in the graduated cylinder.

[0313] 9) Divide the weight (g) by the final volume (mL) to obtain the tap density-specific gravity (g / mL).

[0314] 10) Perform this test three times for each powder sample.

[0315] Particle size distribution

[0316] Equipment: Malvern Mastersizer 3000, Malvern Hydro EV, 500mL beaker and deionized water

[0317] Test conditions: Sample temperature 20℃-23℃

[0318] Measurement scale / unit: particle size distribution (μm)

[0319] 1) Turn on the Malvern Mastersizer 3000. Allow the sample to equilibrate to room temperature (~20℃-23℃).

[0320] 2) Fill a 500mL beaker with deionized water and place it under the Malvern Hydro EV device.

[0321] 3) Run the SOP (spray-dried orange oil) for the experiment and name each run.

[0322] 4) Edit the SOP and input the average density and refractive index of the sample to be tested.

[0323] 5) Allow the machine to measure the background light, then add the sample to the device. Typically, the device is ready once the background light reading stabilizes between 0mV and -50mV.

[0324] 6) Add the sample dropwise (slowly) to the 500mL beaker until it reaches the green area in the bar displayed on the computer (this indicates that enough sample has been added for analysis). Then, click the Start button to begin the analysis.

[0325] 7) The device will automatically collect 5 sets of measurements.

[0326] 8) Once completed, the system will automatically enter cleaning mode, requiring three changes of deionized water before testing individual samples.

[0327] 9) Repeat the test on additional samples.

[0328] pH test

[0329] Equipment: Hannah HI11312 pH meter, Halo pH probe and buffer solutions (pH 4.01, 7.00, 10.01)

[0330] Test conditions: Sample temperature 23℃±5℃

[0331] Measurement scale / unit: Measurement of electrode voltage (mV) relative to pH: -log [H + ]. H + (or H3O) + ) = free hydrogen ions

[0332] pH range: 1.00 (acidic) - 14.00 (alkaline)

[0333] 1) Turn on the pH meter and Bluetooth probe (make sure the probe is connected).

[0334] 2) Unscrew the probe and remove the electrode filling hole cap from the probe.

[0335] 3) Calibrate the pH probe by immersing approximately 1 / 3 of its length in a buffer solution. Begin calibrating the probe with a pH 7.00 buffer solution, then a pH 4.01 buffer solution, and finally a pH 10.01 buffer solution. a. Allow the probe to stabilize at the reading for at least 30 seconds before confirming the calibration point.

[0336] b. Ideally, the pH calibration slope under normal testing conditions will be 98%-102%, and the pH calibration slope for food-fortified products will be 99.5%-100.5%.

[0337] 4) After calibration, begin reading the pH value of the sample at a temperature close to room temperature (23°C). Allow the pH reading to stabilize at a certain point for at least 30 seconds before recording the measurement.

[0338] Viscosity-RVA Viscometer

[0339] Equipment: RVA 4500 viscometer with Julabo F12-ED refrigerated / heated circulator, plastic paddle, and aluminum can.

[0340] Test conditions: incubation temperature 20℃, mixing speed 160rpm, holding time 10 minutes, sample weight 28g.

[0341] Measurement scale / unit: viscosity (cP)

[0342] 1) Simultaneously connect the RVA viscometer and the F12-ED water circulator.

[0343] 2) The viscometer is calibrated by attaching the plastic paddle to the coupling and zeroing the viscosity.

[0344] 3) Powder mixture application: Before starting the test, wait at least 15 minutes to allow the protein shake solution to reach equilibrium.

[0345] 4) Run the application’s desired program, which uses a temperature setpoint of 20°C, a mixing rate of 160 rpm, a holding time of 10 minutes, and a sample weight of 28 g.

[0346] 5) Add 28g of sample to the aluminum can.

[0347] 6) Insert the plastic paddle into the filled tank and slide both parts together into the RVA motor coupling (you should hear a click when the plastic slot is locked in the coupling).

[0348] 7) Once the equipment displays "Test ready", press the RVA column into the RVA viscometer to begin the test.

[0349] 8) Once the test is complete, record the final viscosity reading (cP).

[0350] 9) Perform this test twice for each sample.

[0351] Total fat - acid hydrolysis

[0352] The method is based on AOAC official method 996.06, fats in food (total fat, saturated fat and unsaturated fat).

[0353] surface fat

[0354] The method was based on AOAC official method 963.15, Soxhlet extraction method for fats in cocoa bean products, and JAOAC 28,482 (1945); 33, 342 (1950); 34, 442 (1951); 53, 490 (1970).

[0355] Free fatty acids

[0356] Method: Based on the official AOAC method (965.33).

[0357] Peroxide value

[0358] Method: Based on AOAC official method 940.28

[0359] Oxidation Research Procedures

[0360] 1) Pack 20g of spray-dried flavoring into a small metal bag, seal it securely, and label it.

[0361] 2) Measure the control sample of orange oil into a glass bottle and seal it with a rubber seal.

[0362] 3) The samples were separated and placed under four different test conditions to create different oxidation levels.

[0363] a.C1: Freezing conditions (-112℉ / -80℃), control.

[0364] b.C2: Ambient temperature (20℃ / 68℉), RH 40%.

[0365] c.C3: Accelerated conditions (100℉, 37.78℃), RH 60%. Environmental conditions equivalent to 1 week = 1 month.

[0366] d.C4: Accelerated conditions (130℉, 54.44℃), RH 60%. Environmental conditions equivalent to 3 months of work in 1 week.

[0367] 4) Samples from conditions C3 and C4 are taken weekly and frozen at -112℉ / -80℃. Samples from C1 and C2 are taken monthly and frozen at -112℉ / -80℃. At this temperature, further oxidation is assumed to be stopped. Assuming an average shelf life of 18 months, samples are taken according to the following timeline:

[0368] a.C1: Weekly sampling over 18 months (72 weeks), or until the test is discontinued.

[0369] b.C2: Weekly sampling over 18 months (72 weeks), or until the test is discontinued.

[0370] c.C3: Extraction over 4 months (18 weeks). 1 week = 1 month.

[0371] d.C4: Extract 2 months (9 weeks). 1 week = 3 months.

[0372] 5) Once extracted and frozen, the sample is thawed at room temperature and the peroxide value and free fatty acids are measured.

[0373] The samples were compared to observe whether the spray-dried sample contained soluble starch and whether it was equivalent to the sample dried using GLUCIDEX. ® 12. Spray-dried samples were examined to determine if they were suitable spray-dried flavor analogs that underwent acceptable oxidation within the average shelf life of spray-dried flavor compounds. Although different compounds exhibited varying off-odor intensities at different oxidation levels, peroxide values ​​were generally <10 meq-20 meq, indicating the absence of rancid off-odors.

[0374] Analysis results

[0375] Homogenized emulsion (target 45% solids) :

[0376] Solids%, gravimetric analysis at 100°C, 24 hours.

[0377] The measured solids of emulsions with soluble batches Experiment-01 and Experiment-02 were slightly higher than those with GLUCIDEX. ® The control emulsion is 12. This may occur during the homogenization step, in which subsequent runs are better timed to reduce dilution during transfer of the solution to and from the homogenizer.

[0378] Samples of liquid orange oil were spray-dried to observe their volatile content. Almost all orange oil is volatile (~97%) and will contribute to the moisture content in emulsions and spray-dried flavorings.

[0379] Using GLUCIDEX ® 12. No significant differences were observed in the stained micrographs (stained with 0.1N iodine solution) of the homogenized emulsions of experimental batch-01 and experimental batch-02, except in the GLUCIDEX images at 40x magnification. ® Few dense starch molecules were observed in the 12 emulsions.

[0380] Table 5: Colors :

[0381]

[0382] When AE > 2, with GLUCIDEX ® Compared to the control emulsion (batch 12), the homogenized emulsions containing soluble starch in batches Experiment-01 and Experiment-02 were "distinguished at a glance." These samples tended to be darker, slightly redder, and less yellow. This color difference is likely due to residual carbon from the soluble starch production process, and it was even more pronounced in earlier soluble starch test samples. This color difference may persist throughout the spray drying process, but it is not a major issue at this point, as filtration during industrial production is likely more efficient and results in less color variation.

[0383] Table 6: Density / Specific Gravity

[0384]

[0385] A slight increase in the specific gravity of the homogenized emulsion was observed in both soluble pea starch batch experiments-01 and-02. For soluble pea starch batch experiment-01, this difference was negligible, while for soluble pea starch batch experiment-02, the difference was slightly increased.

[0386] This difference can be explained by the increase in solids observed in both soluble starch samples, which is likely due to less dilution during the homogenization step of processing, and this difference is expected to disappear when the spray-dried flavor is restored to a similar solids level.

[0387] Table 7: pH

[0388]

[0389] The pH of soluble starch emulsions is similarly slightly lower than that of emulsions containing GLUCIDEX. ® The homogenized emulsion of the control (12). This may be due to the initial pH of the soluble starch sample being higher than that of GLUCIDEX. ® The levels were 12 lower, and the two soluble pea starch samples had higher solids levels.

[0390] Table 8: Viscosity

[0391]

[0392] On day 0, the viscosity of the homogenized emulsion was measured at a similar time point (approximately 4 hours after initial production). This was compared with that using GLUCIDEX. ® Compared to emulsion 12, the viscosity of the emulsion containing soluble starch increased significantly. This is not surprising, as early samples of soluble starch showed significant sedimentation, which increased the viscosity of their corresponding emulsions. Surprisingly, the increase in viscosity was even greater between emulsions containing soluble pea starch in batches Experiment-01 and Experiment-02. Since these are two similar batches of the same product, comparable analytical characteristics were expected. The emulsion in batch Experiment-02 containing soluble starch had a slightly higher solids level than the emulsion in batch Experiment-01; however, this degree of viscosity difference was not expected. To observe whether this effect is consistent, the viscosity of the reconstituted emulsions will be compared to see if this effect persists.

[0393] One potential problem with higher viscosity is that if the viscosity is too high, manufacturing issues may arise, such as difficulty in pumping the product into the spray dryer. This viscosity difference was observed during pilot-scale processing, where an increased pumping flow rate was required for the emulsion containing soluble starch in batch Experiment-02. While this effect was significant during processing, it did not cause any problems with the spray drying process itself. (Compared to products with GLUCIDEX) ® Compared to the control emulsion of 12, the viscosity increase of the emulsion with soluble starch in batch experiment-01 did not show a significant difference during processing.

[0394] Table 9: Particle Size Distribution

[0395]

[0396] The homogenized emulsions from batches Experiment-01 and Experiment-02 containing soluble starch were compared with those containing GLUCIDEX. ® There were overall differences in particle size between the homogenized emulsions of sample 12. Both samples showed slight increases in Dx50 and Dx90 due to their higher particle size (approximately 10 μm), while those with GLUCIDEX... ® The emulsion of grade 12 has particles in the higher fraction range of approximately 1.0 µm. Soluble starch batch experiment-01 and control GLUCIDEX. ® The average particle size of batch 12 was similar, while the average particle size of batch 02 of soluble starch was lower because the proportion of particles in the 100 μm range was slightly higher in the first two emulsions.

[0397] Reconstituted emulsion (45% solids) :

[0398] Solids%, gravimetric analysis at 100°C, 24 hours.

[0399] Table 10 :

[0400]

[0401] To observe whether the differences observed in the spray-dried samples persisted in the homogenized emulsion, all three spray-dried powders were restored to approximately 45% solids, the same level as during their initial processing / spray drying. Moisture measurements were performed on these samples, revealing similar solids levels, equivalent to those observed in the homogenized emulsion with soluble starch in batch Experiment-02.

[0402] Under a microscope, the restored emulsion was observed in GLUCIDEX. ® No significant differences were observed between 12 and soluble starch E9827-1&3.

[0403] Table 11: Colors :

[0404]

[0405] Similar to the homogenized emulsion, the reconstituted emulsion exhibits similarities to that with GLUCIDEX. ® The color difference of the control emulsion was 12, but it had the same solids level, though the difference was slightly more pronounced. Both soluble starch emulsions were better than those with GLUCIDEX. ®The control emulsion of 12 was deeper, redder, and less yellow. With ΔE < 1, there was no perceptible color difference between the emulsions with soluble starch batch experiment-01 and the emulsions with soluble starch batch experiment-02.

[0406] Table 12: Density / Specific Gravity

[0407]

[0408] When restored to similar solid levels, the density differences of the samples become equal and statistically similar.

[0409] Table 13: pH

[0410]

[0411] When restored to a similar solid level, it has GLUCIDEX ® The pH difference between the emulsions of batches 12 and soluble starch, Experiment-01 and Experiment-02, was equal to a difference of up to 0.4 pH, which has minimal or no effect during processing or application.

[0412] Table 14: Viscosity

[0413]

[0414] The viscosity of the reconstituted emulsion was measured at similar times to that of the homogenized emulsion (approximately 4 hours after day 0 and day 1 of production). Like the homogenized emulsion, it was compared with the emulsion containing GLUCIDEX. ® Compared to the emulsion of 12, the soluble starch sample showed a greater increase in viscosity. Therefore, there is a potential problem of greater sedimentation after spray drying. However, this is only a concern in applications where a large amount of spray-dried flavoring is used in the emulsion and the emulsion is stored for extended periods.

[0415] However, unlike the homogenized emulsion, the viscosity on day 0 was statistically significantly different from that on day 0 when it exhibited GLUCIDEX. ® The 12-component control emulsion was similar. At the same solids level, GLUCIDEX... ® 12 and soluble starch appeared to have similar viscosities during initial processing. Also, unlike the homogenized emulsions, both soluble starch emulsions showed similar day 0 viscosity and a similar increase to their day 1 viscosity, unlike the larger increase observed in the homogenized emulsion with soluble starch batch experiment-02. The small difference in solids levels leading to the significant increase in homogenized emulsion, or the spray drying process eliminating any sedimentation differences between the two samples, suggests this is likely due to the spray drying process eliminating any differences in solidification between them.

[0416] Table 15: Particle Size Distribution

[0417]

[0418] With GLUCIDEX ® The reconstituted emulsion of batch 12 differed in particle size distribution from soluble starch batches Experiment-01 and Experiment-02 and their homogenized emulsions. The Dx(50) of the soluble starch emulsion was slightly increased, but its Dx(90) was slightly lower than that of GLUCIDEX. ® 12 emulsions, because particles in the 100µm range have a lower fraction. This also helps to reduce the median particle size of emulsions containing soluble starch.

[0419] Spray-dried orange oil powder:

[0420] Solids%, gravimetric analysis at 100°C, 24 hours

[0421] Table 16 :

[0422]

[0423] The spray-dried orange oil samples had similar water content to each other, and were similar to those with GLUCIDEX. ® Compared to spray-dried orange oil of grade 12, spray-dried orange oil samples with soluble starch have a comparable slightly higher water content.

[0424] Table 17: Total Fat %

[0425]

[0426] The amount of orange oil present in each orange oil sample can be calculated by calculating the amount of fat present in the orange oil itself, as well as the amount of fat present in the spray-dried orange oil sample. (This is in contrast to the method described by GLUCIDEX.) ® Compared to the spray-dried orange oil of batches 12 (Experiment-01 and Experiment-02), the spray-dried orange oil samples with soluble starch had slightly lower but statistically similar amounts of orange oil. Each sample had a calculated amount of approximately 45% orange oil.

[0427] Table 18: Surface Oil

[0428]

[0429] To ensure that the orange oil is completely protected by the wall material, the surface oil of the spray-dried flavoring was measured to observe how much of the total orange oil was coated on the spray-dried wall material rather than being encapsulated by the material itself.

[0430] Each sample contained less than 1% calculated surface orange oil, compared to samples with GLUCIDEX. ® Compared to the control spray-dried orange oil of batch 12, the spray-dried orange oil batches -01 and -02, containing soluble starch, had slightly higher levels of surface oil. These substances comprised less than 0.5% of the total orange oil coated on the surface of the spray-dried powder, relative to the amount encapsulated by the wall material. This implies that all three samples exhibited good encapsulation of the orange oil and likely provided good oxidative protection for the orange oil itself.

[0431] Table 19: Colors

[0432]

[0433] When ΔE>2, with GLUCIDEX ® A noticeable color difference remained between the spray-dried orange oil of batches 12 and those with soluble starch E9827-1 and 3. The spray-dried orange oils of batches Experiment-01 and Experiment-02 with soluble starch exhibited a deeper, redder, and yellower flavor profile compared to the control samples, which appeared brighter and whiter. However, this difference was significantly reduced compared to their corresponding homogenized and reconstituted emulsions. Since most applications tend to use low levels of flavorings and other coloring agents, this level of difference carries a low risk of causing significant color variations in application. Additionally, as previously mentioned, for homogenized emulsions, more efficient filtration should be employed in industrial production, which would reduce the presence of GLUCIDEX. ® The color difference between the emulsion of 12 and the emulsion of soluble starch.

[0434] Table 20: Volume Density

[0435]

[0436] The spray-dried orange oil samples had similar bulk densities and exhibited GLUCIDEX. ® The bulk density of spray-dried orange oil (batch 12) and soluble starch (batch 02) was statistically similar. The bulk density of spray-dried orange oil (batch 01) with soluble starch was slightly lower than the other two samples. Therefore, the bulk density of GLUCIDEX-containing orange oil was significantly lower. ® The bulk density of spray-dried orange oil varied between batches of spray-dried flavorings containing soluble starch.

[0437] Table 21: Tap Density

[0438]

[0439] For tap density, GLUCIDEX ® The spray-dried orange oil of batch 12 was statistically similar to that of batch 01 with soluble starch. The spray-dried orange oil of batch 02 with soluble starch was slightly higher than the other two samples. Therefore, the orange oil with GLUCIDEX... ® The difference in tap density of spray-dried orange oil of 12 is within the range of batch variation for spray-dried flavorings containing soluble starch.

[0440] Table 22: Particle Size Distribution

[0441]

[0442] The particle size distribution of spray-dried orange oil containing soluble starch E9827-1 is close to that of orange oil containing GLUCIDEX. ® The spray-dried orange oil had a particle size of 12, and the Dx10, Dx50, Dx90, and average particle size were all slightly smaller than those with GLUCIDEX. ® 12 spray-dried orange oil. This indicates that at least one batch is related to GLUCIDEX. ® 12. Compare with similar spray-dried soluble starches.

[0443] Oxidation study results—1 month

[0444] Condition C1 (freezing) and Condition C2 (environmental conditions)

[0445] Free fatty acid concentration :

[0446] Table 23 :

[0447]

[0448] Table 24 :

[0449]

[0450] Table 25: Peroxide Value

[0451]

[0452] Table 26 :

[0453]

[0454] At one month, samples were taken under both frozen (C1) and room temperature (C2) conditions, and the concentration of free fatty acids and peroxide value were tested. Based on the data, both frozen and room temperature conditions showed similarly low levels of free fatty acids, indicating that little or no free fatty acid production occurred under ambient or frozen conditions. Spray-dried orange oil from batches Experiment-01 and Experiment-02 with soluble starch showed better performance than orange oil with GLUCIDEX. ® The spray-dried orange oil at 12 had a slightly higher concentration of free fatty acids, indicating that some of the free fatty acids were provided by the soluble starch itself.

[0455] For peroxide value, it has GLUCIDEX ® The spray-dried flavor compounds of 12 and soluble starch exhibited minimal to undetectable oxidation. The control orange oil itself showed a certain level of basal oxidation observed under C1 freezing conditions, which was slightly higher than in the ambient condition sample. This indicates that GLUCIDEX... ® Both 12 and soluble starch contribute some initial level of protection.

[0456] Condition C3: 37.8℃, RH 60%

[0457] Free fatty acid concentration

[0458] Table 27 :

[0459]

[0460] Table 28: Peroxide Value

[0461]

[0462] At one month, C3 accelerated conditions showed a slight increase in free fatty acids in all samples. This was observed with orange oil and those containing GLUCIDEX. ® Compared to the spray-dried flavor compound and orange oil itself, the spray-dried sample with soluble starch (very similar to those under frozen and ambient conditions) showed a higher baseline level of free fatty acids. However, the concentration of free fatty acids remained fairly consistent over four weeks, indicating an increase of approximately 0.20%, which is similar to that of orange oil and only slightly higher than that with GLUCIDEX. ® 12 spray-dried sample.

[0463] Regarding peroxide value, all spray-dried samples showed only a slight increase to approximately 1.0, while the control orange oil exhibited a much higher degree of oxidation. Although different compounds may produce noticeable oxidative off-odors at different oxidation levels, a peroxide value <10 is generally considered unoxidized. Under 4 weeks of C3 conditions (equivalent to approximately 4 months of environmental conditions), the orange oil was considered oxidized, while the control orange oil with GLUCIDEX... ® 12. Spray-dried flavorings of soluble starch are considered unoxidized and have similar protection.

[0464] Condition C4: 54.4℃, RH 60%

[0465] Free fatty acid concentration

[0466] Table 29 :

[0467]

[0468] Table 30: Peroxide Value

[0469]

[0470] At one month, C4 conditions were similar to C3 conditions, with a slight increase in free fatty acids in all samples. This was compared to orange oil and those with GLUCIDEX. ® Compared to spray-dried flavor compounds and orange oil itself, spray-dried samples with soluble starch (very similar to other environmental conditions) showed higher baseline levels of free fatty acids. However, the concentration of free fatty acids remained fairly consistent over four weeks, indicating an increase of approximately 0.20–0.3%, which is only slightly higher than that of orange oil and those with GLUCIDEX. ® 12 spray-dried sample.

[0471] Regarding peroxide value, all spray-dried samples showed only a slight increase to approximately 1.0, while the control orange oil exhibited a much higher degree of oxidation. Although different compounds may produce noticeable oxidative off-odors at different oxidation levels, a peroxide value <10 is generally considered unoxidized. Under 4 weeks of C4 conditions (equivalent to approximately 12 months of environmental conditions), the orange oil was considered oxidized, while the control orange oil with GLUCIDEX... ® 12. Spray-dried flavorings of soluble starch are considered unoxidized and have similar protection.

[0472] in conclusion

[0473] With GLUCIDEX ®Compared to batch 12, soluble starch batches Experiment-01 and Experiment-02 exhibited similar processability during spray drying. Major problems may arise if the resulting emulsion is kept for up to 24 hours, indicating a difference compared to batches with GLUCIDEX. ® Compared to the control (12), significant sedimentation and increased viscosity were observed in the emulsion containing soluble starch. This did not significantly affect the spray drying of the current soluble starch sample.

[0474] The resulting emulsion is similar to GLUCIDEX. ® 12. The biggest difference is color, which may be addressed in industrial-scale production through more efficient filtration.

[0475] The resulting spray-dried orange oil containing soluble starch showed similar powder properties to GLUCIDEX. ® 12 Similar oil encapsulation rates.

[0476] At 1 month, the oxidative protection of spray-dried soluble starch samples appeared to be equivalent to GLUCIDEX. ® 12 samples.

[0477] One month after the oxidative stability study, the soluble starch sample appears to be an equivalent alternative to 12DE maltodextrin in spray drying applications.

[0478] Example 3: Preparation of soluble pea starch with high DS and high temperature

[0479] Materials and equipment

[0480] • Raw material: Natural pea starch N735 (commercialized by the applicant)

[0481] • A commercially available starch / jet cooker (also known as a laboratory starch cooker) by Bottom Line Process Technologies, Inc.

[0482] • Pressure cooker: Parr Pressure Reactor 8500

[0483] • Refining and spray drying equipment

[0484] Process, guiding procedures and operating conditions

[0485] process :

[0486] Pea starch and water are mixed in a mixing tank, liquefied by passing through a starch / jet cooker, and further heat-treated in a pressure reactor. After cooking, the solution is refined and then spray-dried to form soluble pea starch powder.

[0487] Booting procedures and operating conditions :

[0488] The steps and related operating conditions for the bootloader are listed below:

[0489] - 9000g of pea starch, commercialized by the applicant under number N735, will be mixed with 21,000g of tap water to form 30,000g of starch-water mixture, with a starch concentration of approximately 30% by weight.

[0490] - Stir the mixture in a mixing tank for 15 minutes at room temperature.

[0491] - The starch slurry is pumped through the starch cooker at a flow rate of 500g / min and the heating temperature is 140℃~150℃.

[0492] - Discharge the gelled starch slurry into a pressure vessel.

[0493] Continue cooking the starch slurry in the pressure vessel to 180°C and maintain for 10-15 minutes.

[0494] - Flash distill the product into a flash tank and cool the distilled solution to 80°C using a cooling coil.

[0495] - The product is purified with 0.1%~0.3% activated carbon for 45 minutes and then passed through a filter press.

[0496] - Spray-dry the solution at an inlet temperature of 190°C and an outlet temperature of 90°C.

[0497] Sample Analysis

[0498] Solubility measurement (MERDGN 1002EN)

[0499] - Collect 45 ml of sample in a 50 ml centrifuge tube at room temperature.

[0500] Centrifuge the sample at 3000g for 5 minutes.

[0501] Collect the supernatant and weigh it.

[0502] - Dry the supernatant at 130°C for two hours until constant weight is achieved.

[0503] - Cool and dry the supernatant in a desiccator for 1 hour at room temperature.

[0504] - Calculate solubility by answering the following questions:

[0505] 100 * m * (M+P) / (P1 * P)

[0506] Where: M = mass of water, P = mass of starch, P1 = mass of supernatant, m = mass of dried residue.

[0507] - For accuracy, repeat the measurement twice.

[0508] Dextran equivalent and carbohydrate distribution measurement

[0509] - Determine the dextran equivalent (DE) of the pilot sample using any method well-known in the art. (MERDGN 1005EN)

[0510] - Carbohydrate distribution was determined by HPLC with a double silver column.

[0511] Viscosity measurement

[0512] - Dissolve the pilot product in deionized (DI) water at room temperature to form a solution with a concentration of 45% w / w.

[0513] The viscosity of the solution was measured using a Brookfield II viscometer with a #21 spindle at 15°C. Measurements were performed according to the manufacturer's specifications.

[0514] - The temperature of the solution is controlled by a circulating water bath.

[0515] Results and discussion

[0516] Dextrin equivalents and carbohydrate distribution

[0517] Dextrin equivalent (DE) and carbohydrate distribution (DP) are important information about the characteristics of pilot-scale products.

[0518] Table 31 shows the DE and DP measurements of different batches of pilot-scale products. Commercial maltodextrin with DE12 (from the applicant's commercialized GLUCIDEX) ® The DE and DP results of 12) are also included in the table for comparison.

[0519] Table 31. Results of DE and DP measurements

[0520]

[0521] The results showed that the DE value of the pilot product was about 11, ranging from 9.5 to 12.2; and the DP1+DP2 concentration was about 4%-6% (between 4.8% and 5.7%).

[0522] The DP distribution of the pilot product is similar to that of the reference sample.

[0523] solubility

[0524] Another important characteristic parameter is solubility. Soluble starch should have sufficiently high solubility in cold water in order to be used as a substitute for maltodextrin.

[0525] Viscosity

[0526] Viscosity directly affects product suitability and processability; it also reflects the impact of processing conditions on the final product. Currently, the viscosity of commercial DE12 samples is used as a reference.

[0527] Comparative study

[0528] The data is shown in Table 32 below. :

[0529]

[0530] *ND: Undetermined, because maltodextrin does not contain starch (iodine test does not show a blue color).

[0531] It is also clear here that the highly soluble pea starch of the present invention is functionally maltodextrin and structurally starch.

Claims

1. A highly soluble leguminous starch having: - an oligosaccharide content of DP 1 and 2 of less than 10% by weight, preferably less than 7% by weight, - an oligosaccharide content of DP 3 to 20 of between 30% and 40% by weight, - a water solubility of more than 95% by weight, more preferably more than 98% by weight, - a viscosity of less than 500 cP, more preferably less than 200 cP, and characterized in that: - by 13 an a-1,4 / a-1,6 ratio of between 23 and 32% determined by C NMR.

2. The highly soluble starch according to claim 1, wherein the starch is a pea or a broad bean starch.

3. A method of preparing a highly soluble starch, comprising the steps of: - preparing a starch slurry, - gelatinizing the starch slurry, - cooking the gelatinized starch, - refining the hot decomposition solution thus obtained with activated carbon, filtering and evaporating, and - drying the concentrated solution to obtain a powder product.

4. The method according to claim 3, wherein the starch is a native leguminous starch.

5. The method according to claim 4, wherein the starch is a pea or a broad bean starch.

6. The method according to any one of claims 3 to 5, wherein the starch slurry is prepared by adding the starch in powder form in water to reach an initial starch water mixture, wherein the starch in the initial starch water mixture represents 10% to 35% by weight, more preferably 15% to 30% by weight, relative to the total weight of the starch water mixture.

7. The method according to any one of claims 3 to 6, wherein the gelatinization is performed by steam cooking, jet cooker cooking, cooking on a roller, cooking in a kneader / extruder system, followed by drying, for example in an oven, by hot air on a fluidized bed, on a rotating roller, by atomization, by extrusion or by lyophilization.

8. The method according to any one of claims 3 to 7, wherein the gelatinization of the starch is performed continuously in a jet cooker at a temperature between 140°C and 150°C.

9. The method according to any one of claims 3 to 8, wherein the cooking of the gelatinized starch is performed at a temperature of up to 175°C at a pressure of between 1.43 bar and 12.55 bar, more preferably at a pressure of between 4.16 bar and 8.94 bar.

10. The method according to any one of claims 3 to 8, wherein the cooking of the gelatinized starch is performed at a temperature of up to 180°C at a pressure of between 9 bar and 9.5 bar.

11. The method according to any one of claims 3 to 10, wherein the cooked solution is refined with activated carbon, filtered and evaporated, and dried to powder form using a dryer such as a roller dryer, a flash dryer, a spray dryer, a freeze dryer.

12. The method according to claim 11, wherein the decocted solution is dried into powder form using a spray dryer, with inlet temperatures between 150°C to 250°C, more preferably between 170°C to 190°C; and outlet temperatures between 60°C to 120°C, more preferably between 80°C to 90°C.

13. Use of the highly soluble legume starch according to claim 1 or 2 as a substitute for maltodextrin in food applications.

14. Use of the highly soluble legume starch according to claim 1 or 2 as a substitute for maltodextrin for the preparation of baked goods, sauces and dressings, dairy products and beverages, more specifically as carrier for flavor encapsulation, for the formulation of fat free vinaigrettes and for the preparation of powdered beverage formulations.

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