A method for the preparation of dry-mixed embedded octenyl succinic anhydride starch and a honey embedding process
By preparing porous octenyl succinic starch ester, the problems of complex processes and high equipment costs in the encapsulation of high-viscosity substances have been solved, achieving efficient and stable dry-mix encapsulation effects, which are particularly suitable for high-viscosity substances such as honey.
Patent Information
- Application Number
- CN202510986379.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-17
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2045-07-17
AI Technical Summary
Existing technologies for encapsulating highly viscous materials involve complex processes, high equipment costs, and difficulty in achieving efficient and stable encapsulation results.
A porous octenyl succinate starch ester preparation method was adopted, which involves esterification, enzymatic hydrolysis and spray drying processes. This ester is used for dry mixing and encapsulation of high-viscosity substances such as honey, avoiding high-pressure shearing and spray drying steps, and utilizing the porous structure to achieve efficient adsorption.
It achieves stable encapsulation of high-viscosity substances, simplifies the process, reduces equipment costs, provides good product stability, is suitable for temperature-sensitive substances, and avoids caking under high temperature and high humidity conditions.
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Figure CN120718163B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of preparation of edible modified starch, in particular to a preparation method of octenyl succinic anhydride starch for dry-mix embedding and a honey embedding process. BACKGROUND
[0002] Octenyl succinic anhydride starch, also known as pure glue, generally exists in the form of sodium octenyl succinic anhydride starch, is a safe emulsifying thickener. There are also some reports of porous starch as a new type of organic adsorbent and embedding material, which is widely used in medicine, pesticide, printing, sewage treatment, daily chemical industry, cosmetics and food industry. For example, CN106279450A reports a porous octenyl succinic anhydride starch, which is prepared by hydrolyzing the raw starch milk with enzymes to form pores, and then reacting with octenyl succinic anhydride to obtain porous octenyl succinic anhydride starch. It not only has good adsorption and embedding properties, but also has hydrophilic and lipophilic properties, and good emulsifying performance. CN108409871A reports a method for preparing octenyl succinic anhydride starch by heat treatment-esterification and synergistic enzymatic hydrolysis of alpha amylase. The pre-heat treatment before esterification can partially eliminate the particle structure of the starch, improve the substitution degree and reaction efficiency, and then use alpha amylase to treat the octenyl succinic anhydride starch. However, the product obtained is a raw starch particle with small pore size. These reported modified starch embedding materials usually need to be dissolved, high-pressure homogenized and dried when embedding substances with high viscosity, and the process is relatively complex, requiring high equipment.
[0003] Honey is a viscous, transparent or translucent viscous liquid, and also a natural supplement and sweetener with biological activity. Solid honey powder has high commercial value. The preparation of solid honey powder usually involves embedding with wall materials (such as modified starch, malt dextrin, gum arabic, etc.) and drying by heating, vacuum drying, freeze drying and spray drying. CN108041527A discloses a method for preparing solid honey powder by embedding honey with modified starch. This method needs to dissolve, homogenize, emulsify and spray dry the modified starch when used, and the manufacturer needs to be equipped with high-pressure homogenizer, spray drying tower and other equipment, which increases the investment and inconvenience of the manufacturer.
[0004] Therefore, there is an urgent need for a preparation method of octenyl succinic anhydride starch which is convenient to use, has high embedding efficiency and stable product properties. SUMMARY
[0005] The purpose of this invention is to provide a method for preparing octenyl succinate starch ester for dry blending and embedding, and a honey embedding process. By esterifying starch, enzymatically hydrolyzing it, and treating it with gas, an octenyl succinate starch ester suitable for dry blending and embedding is obtained, thus solving the problems of complex processes and high equipment costs in the embedding of high-viscosity substances mentioned in the background art. This octenyl succinate starch ester can be used for dry blending and embedding of high-viscosity substances such as honey.
[0006] To achieve the above objectives, the present invention provides the following technical solution:
[0007] A method for preparing octenyl succinic acid starch ester for dry mixing and embedding is characterized by: firstly, preparing starch milk at a solid-liquid ratio of 1:1.5 to 1:2, esterifying and gelatinizing it with octenyl succinic anhydride, adding amylase for enzymatic hydrolysis, using 0.25 to 4.50 IU of amylase per gram of starch, treating for 2 to 6 hours, adding a gas-generating agent, and spray drying to obtain the finished octenyl succinic acid starch ester.
[0008] Preferably, the amylase is any one of α-amylase, β-amylase, and glucoamylase.
[0009] Preferably, the pH of the esterification treatment is maintained at 8.9-9.2.
[0010] Preferably, the esterification treatment temperature is 35-36°C.
[0011] Preferably, the pH of the enzyme treatment is 5.0-5.2.
[0012] Preferably, the gas-generating agent is any one of ammonium carbonate and ammonium bicarbonate or a combination thereof.
[0013] Preferably, the starch is one or any combination of waxy corn starch, tapioca starch, potato starch, corn starch, glutinous rice starch, and wheat starch.
[0014] A honey encapsulation process involves adding honey to octenyl succinate starch ester prepared by the above-mentioned method for dry-mixing and encapsulation, followed by dry-mixing and encapsulation to prepare solid honey powder.
[0015] Preferably, the mass ratio of the octenyl succinic acid starch ester to honey is 150:80-130.
[0016] Compared with the prior art, the beneficial effects of the present invention are:
[0017] The octenyl succinate starch prepared by the method provided by the application can be directly used to embed high viscosity substances such as honey, flavor oil, syrup and lecithin in powder form through dry mixing, thereby saving the steps of conventional high-pressure shearing and spray drying, and having small investment, convenient use and good product stability. The obtained product is free-flowing powder and will not form paste or agglomerate. When needed, the product can be directly used in powder form or mixed into other foods. Since the spray drying process is omitted in the embedding process, the product can also be used to embed high-temperature sensitive substances and will not be hardened under high-temperature and high-humidity conditions. BRIEF DESCRIPTION OF DRAWINGS
[0018] Figure 1 Product photos of the modified starch dry-mixed and embedded honey prepared in Examples 1-4;
[0019] Wherein, a, Example 1; b, Example 2; c, Example 3; d, Example 4.
[0020] Figure 2 Product photos of the modified starch dry-mixed and embedded honey prepared in Examples 5-8;
[0021] Wherein, a, Example 5; b, Example 6; c, Example 7; d, Example 8.
[0022] Figure 3 Product photos of the modified starch dry-mixed and embedded honey prepared in Examples 9-12;
[0023] Wherein, a, Example 9; b, Example 10; c, Example 11; d, Example 12.
[0024] Figure 4 Product photos of the modified starch dry-mixed and embedded honey prepared in Comparative Examples 1-3;
[0025] Wherein, a, Comparative Example 1; b, Comparative Example 2; c, Comparative Example 3. DETAILED DESCRIPTION
[0026] The technical solutions in the embodiments of the application will be described below in conjunction with the following embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the protection scope of the application.
[0027] The application provides a technical scheme: a preparation method of a dry-mixed embedded octenyl succinate starch ester, characterized by: first, starch milk is prepared according to a solid-liquid ratio of 1:1.5-1:2, esterification treatment is performed on the starch milk by using octenyl succinic anhydride, gelatinization is performed, and enzymatic hydrolysis treatment is performed by adding amylase, the amylase is used in an amount of 0.25-4.50 IU of enzyme per gram of starch, after 2-6 hours of treatment, a gas-producing agent is added, and the finished product octenyl succinate starch ester is obtained by spray drying.
[0028] Among them, the solid-liquid ratio of the starch milk refers to the mass of the starch and the volume of the water, and the ratio ensures that the starch particles are fully dispersed to form a uniform suspension. Enzymatic hydrolysis refers to the process of hydrolyzing starch molecular chains by using amylase, which can be realized by using a constant-temperature water bath oscillator to maintain the reaction temperature, and the molecular weight reduction amplitude is adjusted by controlling the enzyme activity unit and the action time. The gas-producing agent refers to a substance that decomposes to produce gas at high temperature, which releases gas to form a porous structure during the spray drying process.
[0029] Specifically, after the starch milk is introduced with a hydrophobic group through esterification reaction, gelatinization treatment is performed to fully stretch the starch molecular chains. The amylase selectively cuts the alpha-1,4 glycosidic bond under a specific pH condition to reduce the molecular weight and improve the solubility, while retaining a long enough molecular chain to maintain the emulsifying performance. After the enzymatic hydrolysis product is mixed with the gas-producing agent, in the high-temperature environment in the spray drying tower, the gas produced by the decomposition of the gas-producing agent forms a microporous structure inside the starch particles. This porous structure makes the material have a high specific surface area and adsorption capacity. When the material is dry-mixed with a high-viscosity substance (such as honey), the porous surface can quickly adsorb the viscous substance, and the starch molecules with a moderate molecular weight form a stable embedding system through hydrogen bonding.
[0030] Further, the amylase is any one of alpha-amylase, beta-amylase, and glucoamylase. By selecting amylases with different action modes, the breaking mode of the starch molecular chain is targetedly regulated. Alpha-amylase realizes rapid molecular weight reduction by randomly cutting internal bonds, beta-amylase realizes accurate control of chain length by gradually hydrolyzing the non-reducing end, and glucoamylase realizes viscosity optimization of the system by completely hydrolyzing to generate monomers. This selective regulation makes the molecular weight distribution of the starch ester adjustable according to actual needs, which can not only avoid the negative impact of the excessively large molecular weight of natural starch on the stability of the emulsion, but also retain necessary branched chain structures to maintain the embedding performance, so as to balance the material properties while simplifying the dry-mixing process.
[0031] Further, the pH of the esterification treatment is maintained at 8.9-9.2. When the pH value is lower than 8.9, the degree of hydrolytic activation of octenyl succinic anhydride is insufficient, resulting in a decrease in the esterification reaction rate and uneven distribution of the degree of substitution; when the pH value exceeds 9.2, the starch granule surface will swell significantly and even rupture, causing the molecular chain to break disorderly. By precisely controlling the pH in the range of 8.9-9.2, the active sites formed by the effective ring-opening of the anhydride can be ensured, and the integrity of the crystal structure of the starch granule can be maintained, so that the substitution reaction preferentially occurs in a specific area on the surface of the granule. This directional esterification makes the distribution of hydrophobic groups on the molecular chain of the product exhibit a gradient characteristic, providing a necessary amphiphilic structure basis for the formation of a stable emulsion in the subsequent dry mixing embedding process. The octenyl succinic acid starch ester obtained finally has uniform distribution of substituent groups and stable emulsifying properties, and can be directly used for dry mixing embedding of high-viscosity honey without additional emulsification treatment.
[0032] Further, the temperature of the esterification treatment is 35-36℃. When the reaction temperature is controlled at 35-36℃, the swelling degree of the starch granule is limited within a controllable range, and its crystal structure is not irreversibly destroyed, which is conducive to the subsequent directional cutting of the starch molecular chain by enzymatic hydrolysis. The temperature condition cooperates with the alkaline pH environment to make the esterification reaction rate of octenyl succinic anhydride reach the best balance point, avoiding both the increase in side reactions caused by excessively high temperature and the decrease in reaction efficiency caused by insufficient temperature. Within this temperature range, the hydroxyl activity of the starch molecular chain is effectively activated, while the diffusion rate of octenyl succinic anhydride matches the reaction activity, forming a uniform esterification product. This temperature control effectively avoids batch differences caused by temperature fluctuations, and the octenyl succinic acid starch ester prepared finally has stable emulsifying properties and embedding capacity, and is particularly suitable for the processing needs of viscosity materials in the dry mixing embedding process.
[0033] Further, the pH of the enzyme treatment is 5.0-5.2. After the starch milk is subjected to esterification treatment, the reaction system is precisely adjusted to a weakly acidic environment with a pH of 5.0-5.2. This pH range puts the active sites of the amylase in the best protonation state, promoting the binding efficiency of the enzyme and the starch molecular chain, while maintaining the integrity of the tertiary structure of the enzyme molecule. Under this condition, the hydrolysis rate of the α-1,4 glycosidic bond of the starch chain and the stability of the enzyme molecule reach a dynamic balance, avoiding both enzyme deactivation caused by excessively strong acidity and the generation of side reaction products under neutral conditions, ensuring controllable degradation of the starch molecular weight. This provides an intermediate product with stable physicochemical properties for the subsequent uniform dispersion of the gas generating agent and the spray drying process.
[0034] Further, the gas generating agent is any one or a combination of ammonium carbonate and ammonium bicarbonate. Ammonium carbonate decomposes into carbon dioxide and ammonia gas upon heating, and ammonium bicarbonate decomposes into carbon dioxide, ammonia gas, and water vapor upon heating. These gases form a uniform pore structure inside the material, enabling the starch ester carrier to adsorb viscous substances. The choice of gas generating agent is based on its decomposition temperature matching the spray drying process, avoiding the introduction of foreign chemical residues, and ensuring the safety of food-grade applications.
[0035] Specifically, during the spray drying stage, the gases generated by the decomposition of ammonium carbonate or ammonium bicarbonate are encapsulated in the starch ester matrix, forming a honeycomb-like pore structure. When ammonium carbonate is used as the gas generating agent, it produces a larger amount of gas upon decomposition, making it suitable for scenarios requiring higher porosity. The release of gas from ammonium bicarbonate is relatively gradual, preventing the pore structure from expanding excessively and causing the carrier to break. When used in combination, the gas generation rate can be controlled by adjusting the ratio, for example, when mixed in a 1:1 mass ratio, both the pore generation efficiency and the prevention of excessive local gas pressure damaging the carrier structure can be maintained. The resulting porous structure directly enhances the adsorption capacity of viscous substances such as honey, eliminating the need for forced dispersion through high-pressure homogenization equipment. The porous carrier structure formed increases the honey adsorption capacity to more than 1.5 times that of conventional modified starch, with an embedding efficiency of more than 92%, and without the need for specialized equipment such as high-pressure homogenizers, making it particularly suitable for small and medium-sized food processing enterprises.
[0036] Further, the starch is one or any combination of waxy corn starch, cassava starch, potato starch, corn starch, glutinous rice starch, and wheat starch.
[0037] Among them, waxy corn starch refers to a variety of corn starch with a high amylopectin content of more than 95%. It can be extracted by wet milling process from natural waxy corn. Its high amylopectin structure is conducive to forming a loose and porous network structure. Cassava starch refers to the starch extracted from cassava tubers. It can be prepared by crushing, filtering, and precipitating processes. Its low protein content can reduce the interfacial interference during emulsification. Potato starch refers to starch granules separated from potato tubers. It can be obtained by centrifugal separation. Its larger particle size helps to improve the uniformity of gas generating agent dispersion. Corn starch refers to the starch extracted from ordinary corn by wet processing. It can be obtained by soaking, crushing, and separation processes. Its moderate ratio of amylose to amylopectin can balance the hydrophilic and lipophilic properties. Glutinous rice starch refers to the starch extracted from glutinous rice. It can be prepared by alkali leaching process. Its high viscoelasticity helps to maintain the integrity of the embedding structure. Wheat starch refers to the starch separated from wheat endosperm. It can be extracted by dough washing method. Its unique granular morphology is conducive to improving the adsorption capacity.
[0038] Specifically, by selecting specific types of starch or combinations thereof, the molecular structural properties of different starches are utilized to synergistically optimize the performance of the esterification product. The high-branched structure of waxy corn starch creates uniform porosity during enzymatic hydrolysis, the low impurity content of cassava starch ensures the efficiency of esterification reactions, and the particle size differences of potato starch complement the distribution of gas-forming agents. When multiple starches are used in combination, such as waxy corn starch mixed with cassava starch at a mass ratio of 1:1, their branched structures and low protein characteristics work together to make the esterification product have both high adsorption capacity and low interfacial tension. The porous structure formed in this way can directly adsorb honey molecules during dry mixing without the need to destroy the starch structure through a dissolution step, and the optimized hydrophilic-lipophilic balance value allows the embedding system to form a stable interface during solid-state mixing.
[0039] A honey embedding process using the octenyl succinate starch ester prepared by the above-mentioned method for dry-mixed embedding, adding honey to it, dry-mixed embedding, and preparing a solid honey powder.
[0040] The octenyl succinate starch ester has a porous surface and emulsifying properties. During mixing with honey, the starch ester particles adsorb honey components through the pores, and the surface ester groups interact with the polar substances in the honey to form a stable coating structure. Mechanical forces during mixing cause the starch ester to be uniformly dispersed in the honey, forming a micro-morphology in which the continuous phase wraps the dispersed phase. The final solid powder fixes the honey components through the film-forming action of the starch ester, avoiding the loss of volatile substances caused by high-temperature drying in traditional processes.
[0041] Further, the mass ratio of octenyl succinate starch ester to honey is 150:80-130. Dry-mixed embedding refers to a process in which solid materials are coated through mechanical mixing in a non-dissolved state, and can be specifically carried out by mixing in a blender or mixer at room temperature. This process avoids liquid homogenization and forms a composite structure through physical adsorption between solid particles.
[0042] Specifically, the microporous structure of the starch ester can effectively adsorb sugars and active substances in honey, and its surface hydrophobic groups form stable bonds with honey components. The lower limit of this ratio ensures that the starch ester carrier has sufficient adsorption capacity, preventing clumping caused by excessive honey; the upper limit ensures the embedding rate of active ingredients in honey, preventing the loss of effective substances. During mixing, the starch ester particles and honey form a uniformly dispersed system under the action of shear force, without the need for high-pressure homogenization to achieve sufficient contact between the embedding material and the core material.
[0043] In some embodiments, the mass ratio of the octenyl succinate starch and the honey can be 150:100, for example, 150 grams of the starch ester and 100 grams of the honey are put into a mixer and mixed at 200 revolutions per minute for 30 minutes at 25°C. After mixing, the material is sieved to obtain a solid honey powder with good fluidity.
[0044] The application realizes effective embedding of high-viscosity honey under solid-state mixing conditions, avoids the destruction of bioactive components of honey caused by high-temperature or high-pressure treatment, and solves the problem of uneven mixing caused by high viscosity of honey in traditional processes. The formed solid powder has a stable physical structure and is not easy to absorb moisture and cake during storage.
[0045] The application will be further described in detail below with reference to the examples, but the embodiments are not limited thereto.
[0046] Example 1
[0047] 1000g of waxy corn starch (absolute dry) is prepared into starch milk according to a solid-liquid ratio of 1:1.5, and then sprayed and gelatinized after esterification treatment with 3% (dry weight of starch, the same below) octenyl succinic anhydride. Enzymatic treatment is performed with α-amylase, and the usage is 0.25 IU of enzyme per gram of starch. After 2 hours of treatment, the mixture is cooled to room temperature, 50g of ammonium carbonate gas agent is added, and the mixture is spray dried at an inlet temperature of 280°C and an outlet temperature of 90°C. After sieving, the octenyl succinate starch product is obtained. 150g of the octenyl succinate starch product is added to a mixer, 80g of honey is slowly added, and stirring is continued until all the honey is absorbed into the powder. As shown in FIG. a, a non-caking powder product is obtained. Figure 1
[0048] Example 2
[0049] 1000g of waxy corn starch (absolute dry) is prepared into starch milk according to a solid-liquid ratio of 1:1.5, and then sprayed and gelatinized after esterification treatment with 3% octenyl succinic anhydride. Enzymatic treatment is performed with α-amylase, and the usage is 1.50 IU of enzyme per gram of starch. After 2 hours of treatment, the mixture is cooled to room temperature, 50g of ammonium bicarbonate gas agent is added, and the mixture is spray dried at an inlet temperature of 280°C and an outlet temperature of 90°C. After sieving, the octenyl succinate starch product is obtained. 150g of the octenyl succinate starch product is added to a mixer, 85g of honey is slowly added, and stirring is continued until all the honey is absorbed into the powder. As shown in FIG. b, a non-caking and uniform powder product is obtained. Figure 1
[0050] Example 3
[0051] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:1.5, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with α-amylase, with the enzyme usage amount of 2.50 IU enzyme per gram of starch, and the treatment time of 4 hours. After the treatment, the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added. The mixture was spray-dried at the inlet air temperature of 280°C and the outlet air temperature of 90°C, and then sieved to obtain the octenyl succinic anhydride starch ester product. As shown in FIG. 1a, 150g of the octenyl succinic anhydride starch ester product was added into a mixer, and then 90g of honey was slowly added and continuously stirred until all the honey was absorbed into the powder, to obtain the non-caking and uniform powder product. Figure 1 c.
[0052] Example 4
[0053] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:1.5, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with α-amylase, with the enzyme usage amount of 3.00 IU enzyme per gram of starch, and the treatment time of 4 hours. After the treatment, the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added. The mixture was spray-dried at the inlet air temperature of 280°C and the outlet air temperature of 90°C, and then sieved to obtain the octenyl succinic anhydride starch ester product. As shown in FIG. 1d, 150g of the octenyl succinic anhydride starch ester product was added into a mixer, and then 95g of honey was slowly added and continuously stirred until all the honey was absorbed into the powder, to obtain the non-caking and uniform powder product. Figure 1 d.
[0054] Example 5
[0055] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with β-amylase, with the enzyme usage amount of 3.00 IU enzyme per gram of starch, and the treatment time of 4 hours. After the treatment, the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added. The mixture was spray-dried at the inlet air temperature of 280°C and the outlet air temperature of 90°C, and then sieved to obtain the octenyl succinic anhydride starch ester product. As shown in FIG. 1c, 150g of the octenyl succinic anhydride starch ester product was added into a mixer, and then 107g of honey was slowly added and continuously stirred until all the honey was absorbed into the powder, to obtain the non-caking and uniform powder product. Figure 2 a.
[0056] Example 6
[0057] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then treated with 3% octenyl succinic anhydride for esterification, and then jet-paste, and then treated with β-amylase for enzymatic hydrolysis, and the amount of use was 3.00 IU of enzyme per gram of starch, and the treatment was performed for 6 hours, and then the mixture was cooled to room temperature, and then 25 g of ammonium carbonate and 25 g of ammonium bicarbonate were added as gas agents, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then sieved to obtain octenyl succinic anhydride starch ester finished product. 150 g of the octenyl succinic anhydride starch ester finished product was added into a mixer, and then 121 g of honey was slowly added, and then stirring was continuously performed until all the honey was absorbed into the powder, and then a non-caking uniform powder finished product was obtained, as shown in Figure 2 b.
[0058] Example 7
[0059] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then treated with 3% octenyl succinic anhydride for esterification, and then jet-paste, and then treated with β-amylase for enzymatic hydrolysis, and the amount of use was 4.00 IU of enzyme per gram of starch, and the treatment was performed for 5 hours, and then the mixture was cooled to room temperature, and then 30 g of ammonium carbonate and 20 g of ammonium bicarbonate were added as gas agents, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then sieved to obtain octenyl succinic anhydride starch ester finished product. 150 g of the octenyl succinic anhydride starch ester finished product was added into a mixer, and then 129 g of honey was slowly added, and then stirring was continuously performed until all the honey was absorbed into the powder, and then a non-caking uniform powder finished product was obtained, as shown in Figure 2 c.
[0060] Example 8
[0061] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then treated with 3% octenyl succinic anhydride for esterification, and then jet-paste, and then treated with β-amylase for enzymatic hydrolysis, and the amount of use was 4.50 IU of enzyme per gram of starch, and the treatment was performed for 5 hours, and then the mixture was cooled to room temperature, and then 50 g of ammonium carbonate was added as a gas agent, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then sieved to obtain octenyl succinic anhydride starch ester finished product. 150 g of the octenyl succinic anhydride starch ester finished product was added into a mixer, and then 106 g of honey was slowly added, and then stirring was continuously performed until all the honey was absorbed into the powder, and then a non-caking uniform powder finished product was obtained, as shown in Figure 2 d.
[0062] Example 9
[0063] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with glucose amylase, with the use amount of 4.50 IU enzyme per gram of starch, for 6 hours. After the treatment, the mixture was cooled to room temperature, 50g ammonium bicarbonate gas agent was added, and the mixture was spray dried at an inlet temperature of 280°C and an outlet temperature of 90°C. The product of octenyl succinic acid starch ester was obtained after sieving. 150g of the product of octenyl succinic acid starch ester was added into a mixer, 92g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder. As shown in FIG. a, the non-caking uniform powder product was obtained. Figure 3 a, the non-caking uniform powder product was obtained.
[0064] Example 10
[0065] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with glucose amylase, with the use amount of 4.50 IU enzyme per gram of starch, for 3 hours. After the treatment, the mixture was cooled to room temperature, 50g ammonium bicarbonate gas agent was added, and the mixture was spray dried at an inlet temperature of 280°C and an outlet temperature of 90°C. The product of octenyl succinic acid starch ester was obtained after sieving. 150g of the product of octenyl succinic acid starch ester was added into a mixer, 90g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder. As shown in FIG. b, the non-caking uniform powder product was obtained. Figure 3 b, the non-caking uniform powder product was obtained.
[0066] Example 11
[0067] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then jet-paste after esterification treatment with 3% octenyl succinic anhydride, and then enzymatic treatment with glucose amylase, with the use amount of 4.50 IU enzyme per gram of starch, for 4 hours. After the treatment, the mixture was cooled to room temperature, 50g ammonium bicarbonate gas agent was added, and the mixture was spray dried at an inlet temperature of 280°C and an outlet temperature of 90°C. The product of octenyl succinic acid starch ester was obtained after sieving. 150g of the product of octenyl succinic acid starch ester was added into a mixer, 87g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder. As shown in FIG. c, the non-caking uniform powder product was obtained. Figure 3 c, the non-caking uniform powder product was obtained.
[0068] Example 12
[0069] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:2, and then was treated with 3% octenyl succinic anhydride to form esterification, and then was jet-pasteized, and then was treated with glucoamylase, and the amount of enzyme used was 4.50 IU per gram of starch, and the treatment time was 6 hours, and then the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then the product was sieved to obtain octenyl succinic anhydride starch ester. 150g of the octenyl succinic anhydride starch ester product was added to a mixer, and 82g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder, and then the product was obtained, as shown in FIG. a, and the product was a non-caking uniform powder. Figure 3 d, and the product was a non-caking uniform powder.
[0070] Comparative Example 1
[0071] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:1.5, and then was treated with 3% octenyl succinic anhydride to form esterification, and then was jet-pasteized, and then was treated with alpha-amylase, and the amount of enzyme used was 0.15 IU per gram of starch, and the treatment time was 2 hours, and then the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then the product was sieved to obtain octenyl succinic anhydride starch ester. 150g of the octenyl succinic anhydride starch ester product was added to a mixer, and 80g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder, and then the product was obtained, as shown in FIG. a, and the product was a non-caking uniform powder. Figure 4 a, and the product was a non-caking uniform powder.
[0072] Comparative Example 2
[0073] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk with solid-liquid ratio of 1:1.5, and then was treated with 3% octenyl succinic anhydride to form esterification, and then was jet-pasteized, and then was treated with alpha-amylase, and the amount of enzyme used was 5.5 IU per gram of starch, and the treatment time was 2 hours, and then the mixture was cooled to room temperature, and then 50g ammonium carbonate gas agent was added, and then the mixture was spray-dried at an inlet temperature of 280°C and an outlet temperature of 90°C, and then the product was sieved to obtain octenyl succinic anhydride starch ester. 150g of the octenyl succinic anhydride starch ester product was added to a mixer, and 80g of honey was slowly added, and the stirring was continued until all the honey was absorbed into the powder, and then the product was obtained, as shown in FIG. b, and the product was a non-caking uniform powder. Figure 4 b, and the product was a non-caking uniform powder.
[0074] Comparative Example 3
[0075] 1000g waxy corn starch (absolute dry basis) was prepared into starch milk according to the solid-liquid ratio of 1:1.5, and then was treated with 3% octenyl succinic anhydride for esterification, and then was jet gelatinized, and then was treated with α-amylase for enzymatic hydrolysis, and the amount of use was 0.25 IU of enzyme per gram of starch, and the treatment lasted for 2 hours, and then the product was cooled to room temperature, and then was spray dried at an inlet air temperature of 280°C and an outlet air temperature of 90°C, and then was sieved to obtain octenyl succinic acid starch ester product. 150g of the octenyl succinic acid starch ester product was added into a mixer, and then 80g of honey was slowly added, and then the stirring was continued until all the honey was absorbed into the powder, and then the product was obtained. Figure 4 As shown in FIG. c, the product particles were uneven, and the phenomenon of caking occurred.
[0076] Comparative Example 4
[0077] Referring to patent CN108409871A, 1000g waxy corn starch (absolute dry basis) was prepared into starch milk according to the solid-liquid ratio of 1:1.5, and then was treated with 3% octenyl succinic anhydride for esterification, and then was jet gelatinized, and then was treated with α-amylase for enzymatic hydrolysis, and the amount of use was 0.25 IU of enzyme per gram of starch, and the treatment lasted for 2 hours, and then the product was cooled to room temperature, and then was spray dried at an inlet air temperature of 280°C and an outlet air temperature of 90°C, and then was sieved to obtain octenyl succinic acid starch ester product. 150g of the octenyl succinic acid starch ester product was added into a mixer, and then 80g of honey was slowly added, and then the stirring was continued until all the honey was absorbed into the powder, and then the product was obtained. Figure 4 As shown in FIG. d, the product particles were uneven, and the phenomenon of caking occurred.
[0078] For the octenyl succinic acid starch ester prepared in Comparative Examples 1-4, since the product did not have sufficient pore structure to adsorb liquid, the liquid was excessively retained on the surface of the starch particles, and the phenomenon of caking occurred.
[0079] Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacements to some of the technical features, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A honey encapsulation process, characterized in that: First, a starch slurry is prepared at a solid-liquid ratio of 1:1.5 to 1:
2. It is then esterified and gelatinized with octenyl succinic anhydride, followed by enzymatic hydrolysis with amylase at a dosage of 0.25 to 4.50 IU per gram of starch. After treatment for 2 to 6 hours, a gas-generating agent is added, and the mixture is spray-dried to obtain the finished octenyl succinic anhydride starch ester. Honey is then added, and the mixture is dry-mixed and encapsulated to prepare solid honey powder. The gas-generating agent is any one of ammonium carbonate or ammonium bicarbonate, or a combination thereof.
2. The honey encapsulation process according to claim 1, characterized in that: The amylase is any one of α-amylase, β-amylase, or glucoamylase.
3. The honey encapsulation process according to claim 1, characterized in that: The pH of the esterification treatment is maintained at 8.9-9.
2.
4. The honey encapsulation process according to claim 1, characterized in that: The esterification treatment is performed at a temperature of 35-36°C.
5. The honey encapsulation process according to claim 1, characterized in that: The pH of the enzymatic hydrolysis treatment is 5.0-5.
2.
6. The honey encapsulation process according to claim 1, characterized in that: The starch is one of waxy corn starch, tapioca starch, potato starch, corn starch, glutinous rice starch, wheat starch, or any combination thereof.
7. The honey encapsulation process according to claim 1, characterized in that: The mass ratio of the octenyl succinic starch ester to honey is 150:80-130.
Citation Information
Patent Citations
Preparation method of porous starch octenyl succinate
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