Buccal product and preparation method thereof

Abstract

The embodiment of the invention provides a buccal product and a preparation method thereof, the buccal product provided by the embodiment of the invention comprises an active agent, the active agent comprises modified starch, and the surface of the modified starch is provided with pores; the solubility of the modified starch in water at 25 + / -2 DEG C is less than 0.01 g per 100 g of water, and the solubility in water at 40 + / -2 DEG C is less than or equal to 0.5 g per 100 g of water; the active substance is loaded on the modified starch. According to the buccal product prepared by using the modified starch with pores in the surface as the carrier to load the active substance, the buccal cigarette product can effectively improve the problems that the mouth discomfort is easily generated, the content of effective components is insufficient, and the effective components are easily volatilized and deteriorated due to poor taste and insufficient load capacity of the carrier material in the buccal cigarette product.

Description

Technical Field

[0001] This application belongs to the field of oral tobacco technology, specifically relating to an oral tobacco product and its preparation method. Background Technology

[0002] Oral tobacco products allow smokers to absorb active ingredients directly through the oral mucosa, helping them alleviate cravings. Compared to regular tobacco products, they reduce the intake of harmful substances such as tar and carbon monoxide, making them a healthier option for smokers trying to quit.

[0003] Oral cigarette products based on related technologies are prone to causing discomfort due to poor taste of the carrier material, and their insufficient load-bearing capacity can easily lead to insufficient content of effective ingredients, affecting customer experience. At the same time, the effective ingredients are prone to volatilization or oxidation. Summary of the Invention

[0004] The technical problem to be solved by this application is to provide a mouth-held product and its preparation method, so as to improve the problems of oral discomfort, insufficient content of effective ingredients, and easy volatilization and deterioration of effective ingredients in existing mouth-held tobacco products due to poor taste and insufficient load-bearing capacity of carrier materials.

[0005] To address the aforementioned problems, this application provides the following technical solution:

[0006] This application discloses a mouth-held article comprising an active agent, said active agent including:

[0007] The modified starch has a porous surface; the modified starch has a solubility of less than 0.01 g / 100 g water in water at 25℃±2℃, and a solubility of less than or equal to 0.5 g / 100 g water in water at 40℃±2℃.

[0008] An active substance, wherein the active substance is loaded onto the modified starch.

[0009] Furthermore, in the oral product, the modified starch has hydrophobic groups.

[0010] Furthermore, in the oral product, the hydrophobic group includes at least one of lipo group, acetyl group, ester group, and dialdehyde group.

[0011] Furthermore, in the oral product, the modified starch surface has pores with a diameter of 0.1 to 3 μm.

[0012] Furthermore, in the oral product, the porosity of the modified starch surface is 55-65%.

[0013] Furthermore, in the oral product, the modified starch surface has pores with a depth of 3 to 50 μm.

[0014] Furthermore, in the oral product, the modified starch has a specific surface area of ​​30-40 m². 2 / g.

[0015] Furthermore, in the oral product, the activator further includes a coating attached to the surface of the modified starch.

[0016] Furthermore, in the oral product, the coating includes at least one of flavoring, sugar alcohol filler, binder, sweetener, plasticizer, solvent, and pH adjuster.

[0017] Furthermore, in the oral product, the active substance includes at least one of nicotine and tobacco extract.

[0018] Further, the active agent, by weight, comprises:

[0019] Modified starch 10-30 parts, sugar alcohol filler 35-72.2 parts, binder 0-6 parts, sweetener 0.2-1.5 parts, plasticizer 0-3 parts, pH adjuster 0.5-5 parts, flavoring 5-20 parts, antioxidant 0.1-2 parts, nicotine agent 4-15 parts.

[0020] Furthermore, the oral product also includes a bag, and the active agent is filled in the bag.

[0021] This application also proposes a method for preparing a mouth-held product, used to prepare the mouth-held product as described above, the method comprising:

[0022] A modified starch with a porous surface is provided, wherein the modified starch has a solubility of less than 0.01 g / 100 g water in water at 25℃±2℃ and a solubility of less than or equal to 0.5 g / 100 g water in water at 40℃±2℃.

[0023] Active substances are loaded onto the modified starch to form a dry powder, thereby obtaining a lozenge.

[0024] Furthermore, in the preparation method described above, the modified starch with porous surface is prepared using one of the following methods (I) to (II):

[0025] (I) Enzymatic hydrolysis of starch using amylase;

[0026] (II) Using free radical polymerization, starch is grafted and copolymerized with porogens and acrylic monomers.

[0027] Furthermore, in the preparation method, the amylase includes at least one of glucanase, dextranase, glucosylamylase, glycosylation enzyme, and α-amylase;

[0028] The pore-forming agent includes at least one of sodium bicarbonate and polyethylene glycol, and the acrylic monomer includes at least one of acrylic acid and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS).

[0029] Furthermore, in the preparation method, after providing the modified starch with porous surface, the method further includes:

[0030] A modifier having a hydrophobic group is added to the modified starch, and the hydrophobic group is controlled to undergo a substitution reaction with the hydroxyl groups in the modified starch.

[0031] Furthermore, in the preparation method, after loading the active substance onto the modified starch to form dry powder, the method further includes:

[0032] The coating solution is sprayed onto the dry powder using a fluidized bed granulation method to obtain an active agent with a fluidized bed coating.

[0033] Compared with the prior art, the embodiments of this application have the following advantages:

[0034] In this embodiment of the application, the oral product provided includes an active agent, which includes: modified starch, the modified starch having pores on its surface and having a solubility of less than 0.01 g / 100 g water at 25℃±2℃ and a solubility of less than or equal to 0.5 g / 100 g water at 40℃±2℃; and an active substance loaded on the modified starch. Modified starch with a porous surface has a fine texture and good adsorption properties, enabling it to uniformly adsorb active substances, resulting in a smoother and more mellow taste in oral products, thus reducing irritation and improving the user experience. Simultaneously, the porous structure of the modified starch surface not only allows for more efficient adsorption of more active substances and control of their release rate, thereby increasing the content of active ingredients and providing a more consistent absorption experience, but also effectively protects the active substances and prevents their volatilization and oxidation, extending the product's shelf life and ensuring a stable and lasting flavor during use. Modified starch is insoluble in water and can maintain the integrity of its porous structure in aqueous solutions, ensuring stable loading of active substances and continuous release. Furthermore, starch, as a natural polymer material, is safe, non-toxic, and biodegradable, making it more environmentally friendly and healthier. Therefore, the oral products made using modified starch with a porous surface as a carrier to load active substances in this application embodiment can effectively improve the problems in oral tobacco products caused by poor taste and insufficient loading capacity of the carrier material, leading to oral discomfort, insufficient content of active ingredients, and easy volatilization and deterioration of active ingredients.

[0035] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and do not limit this application. Attached Figure Description

[0036] Figure 1 This is a schematic diagram of the active agent structure in the oral product provided in the embodiments of this application;

[0037] Figure 2 This is a flowchart of the preparation method of the oral article provided in the embodiments of this application;

[0038] Figure 3 Here is a scanning electron microscope image of porous starch in an embodiment of this application;

[0039] Figure 4 This is a comparison curve of the nicotine dissolution ratio in oral products in the embodiments and comparative examples of this application. Detailed Implementation

[0040] To make the above-mentioned objectives, features and advantages of this application more apparent and understandable, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0041] The terms "first" and "second" in the specification and claims of this application may explicitly or implicitly include one or more of the features. In the description of this application, unless otherwise stated, "multiple" means two or more. Furthermore, "and / or" in the specification and claims indicates at least one of the connected objects, and the character " / " generally indicates that the preceding and following objects are in an "or" relationship.

[0042] The inventors discovered that traditional oral tobacco products typically use traditional carrier materials such as microcrystalline cellulose, which have a rough taste, are highly irritating, and can easily cause discomfort. At the same time, traditional carrier materials have limited loading capacity for tobacco extracts and flavorings, which may result in insufficient content of active ingredients. In addition, active ingredients such as nicotine and flavorings in traditional oral nicotine products are prone to volatilization or oxidation, which can easily lead to a short shelf life and decreased performance.

[0043] To address the aforementioned issues, relevant technical measures include adding humectants, lubricants, sweeteners, and antioxidants during the production process to improve the rough texture. Additionally, optimizing particle size can further enhance the mouthfeel. The amount of coating is used to control the oxidation or volatilization of the active ingredient, nicotine. Drying or sealing the powder to control moisture content helps maintain product stability. While humectants and lubricants (such as glycerin and propylene glycol) can improve the moisture content of the smoke, excessive use can lead to an overly sticky mouthfeel, negatively impacting the user experience. Sweeteners and flavorings, while masking the harsh taste of tobacco, may cause taste fatigue with prolonged use, reducing product appeal. Antioxidants (such as BHT and BHA), although commonly used food additives, may pose potential health risks with long-term intake, failing to meet modern consumers' demand for natural and healthy products. Furthermore, mixing multiple additives can lead to chemical reactions, affecting product stability and flavor. Additionally, uneven particle size distribution can cause inconsistencies in taste and release performance, uneven coating thickness, and uneven coating liquid distribution, all of which can negatively impact product quality.

[0044] In response to the above problems, such as Figure 1 As shown, an embodiment of this application provides a mouth-sucking product comprising an active agent 20, the active agent 20 comprising: modified starch 11, the modified starch having pores 13 on its surface, the modified starch having a solubility of less than 0.01 g / 100 g water at 25℃±2℃ and a solubility of less than or equal to 0.5 g / 100 g water at 40℃±2℃; and an active substance 12, the active substance 12 being loaded onto the modified starch 11.

[0045] The modified starch mentioned above may include one or more of the following: modified corn starch, tapioca starch, potato starch, wheat starch, barley starch, and mung bean starch. It not only has pores on its surface, but is also insoluble in water.

[0046] Among them, the modified starch with porous surface has a delicate texture and good adsorption performance, which can uniformly adsorb active substances, making the taste of oral products more mellow and smooth, thereby reducing irritation and improving the user experience. At the same time, the porous structure of the modified starch surface can not only more efficiently adsorb more active substances and control their release rate, thereby increasing the content of effective ingredients in the product and providing a more consistent active substance absorption experience, but also effectively protect the active substances and prevent their volatilization and oxidation, extending the product's shelf life and ensuring that the flavor of the product remains stable during use. The solubility of modified starch in water at 25℃±2℃ is less than 0.01g / 100g water, and the solubility in water at 40℃±2℃ is less than or equal to 0.5g / 100g water, which allows the modified starch to maintain the integrity of its porous structure in aqueous solution, ensuring stable loading of active substances and thus continuous release of active substances. In addition, starch itself, as a natural polymer material, is safe, non-toxic, and biodegradable, making it more environmentally friendly and healthier.

[0047] In this embodiment, the oral products made by using modified starch with porous surfaces as a carrier to load active substances can fundamentally solve the key problems of traditional oral products in terms of taste, release of active substances, stability, flavor retention, hygroscopicity, drug loading, and environmental friendliness. It can significantly improve product quality and user experience, while meeting the needs of modern consumers for health, environmental protection, and personalization.

[0048] Therefore, the oral products provided in this application can effectively improve the problems in oral tobacco products, such as poor taste and insufficient load-bearing capacity of the carrier material, which easily cause oral discomfort, insufficient content of effective ingredients, and easy volatilization and deterioration of effective ingredients.

[0049] In some embodiments, the modified starch surface has pores with a diameter of 0.1–3 μm, which can not only meet the physical adsorption requirements of active substances, but also effectively improve drug encapsulation efficiency and control release rate. The pore diameter can be one of or any combination of 0.1 μm, 0.2 μm, 0.5 μm, 0.6 μm, 0.8 μm, 1.0 μm, 1.2 μm, 1.5 μm, 2 μm, and 3 μm.

[0050] In this embodiment, the pores on the surface of the modified starch can be uniformly distributed on the surface and inside of the particles, extending from the surface to the inside of the particles to form through channels, and can maintain the structural integrity of the pores in aqueous solution to ensure that the active substances are deeply loaded.

[0051] In the embodiments of this application, the particle size of the modified starch can be 20 to 200 μm, for example, one or any two of 20 μm, 30 μm, 50 μm, 80 μm, 100 μm, 150 μm, and 200 μm, so that the modified starch has a good lubricating effect and a delicate taste.

[0052] In this embodiment, the gaps on the surface make the modified starch more readily biodegradable. In some embodiments, the modified starch surface has pores with a depth of 3–50 μm, allowing the pores to penetrate deep into the center of the starch granules, forming a unique channel structure and high adsorption capacity. This protects the active substances to achieve a sustained-release effect and also makes the starch texture softer, smoother, and more delicate, reducing irritation and improving the user experience.

[0053] In this embodiment, the modified starch with pores on its surface has a large specific surface area and porosity, which can efficiently adsorb and load active ingredients such as nicotine and fragrances, thereby increasing the content of active ingredients in the product.

[0054] In one embodiment, the porosity of the modified starch surface is 55-65%, and the pores are uniformly distributed on the starch surface, which can effectively improve the adsorption capacity and specific surface area while ensuring the structural stability of starch as a carrier.

[0055] In one embodiment, the specific surface area of ​​the modified starch is 30–40 m². 2 / g, which can combine high adsorption rate and active material loading efficiency, while improving the dissolution and release of active materials. Optionally, the specific surface area of ​​the starch can be 30m². 2 / g、32m 2 / g、35m 2 / g、38m 2 / g、40m 2 The range of values ​​in / g, either one or both.

[0056] In this embodiment, the adsorption and release characteristics of the modified starch surface pores can be customized by adjusting the porosity and surface modification, thereby meeting the needs of different users for the release rate and flavor of active substances such as nicotine, and thus achieving personalized needs.

[0057] In some embodiments, the modified starch has hydrophobic groups, which enables the starch to maintain the structural integrity of its pores in aqueous solution, ensuring stable loading of the active substance and thus continuously releasing the active substance.

[0058] In some embodiments, the hydrophobic group includes at least one of lipo group, acetyl group, ester group, and dialdehyde group, which can effectively improve the hydrophobicity of starch while maintaining a better taste.

[0059] In this embodiment, the active substance includes at least one of nicotine preparations and tobacco extracts. It not only dissolves rapidly in the oral cavity, releasing active substances to help smokers alleviate withdrawal symptoms, but also readily adheres to the starch surface, achieving a long-lasting and continuous stimulating effect. The active substance may also include substances with specific medical properties; such as caffeine, theophylline, capsaicin, and vitamins.

[0060] In some implementations, the tobacco extract can be adjusted according to the flavor of the oral product, and can be flue-cured tobacco extract, cigar tobacco extract, burley tobacco extract, sun-cured tobacco extract, Zimbabwe extract, etc. Nicotine agents include nicotine, nicotine salts, etc., which can provide physiological satisfaction.

[0061] In some embodiments, the activator also includes an antioxidant loaded on the modified starch, wherein the antioxidant, such as ascorbic acid, can inhibit the oxidation reaction of nicotine, vegetable oils or flavorings, prevent rancidity, discoloration or deterioration, slow down component degradation, and maintain product stability and flavor consistency.

[0062] In some implementations, such as Figure 1 As shown, the activator 20 also includes a coating 14 attached to the surface of the modified starch. The modified starch surface in this embodiment has pores, making the coating easier to adhere, and since most starch is nearly spherical, the coating thickness is more easily achieved.

[0063] In some embodiments, the coating includes at least one of flavoring, sugar alcohol filler, binder, sweetener, plasticizer, solvent, and pH adjuster.

[0064] Flavorings can improve taste and flavor, mask the smell of chemicals such as tobacco or nicotine, and enhance the user experience. At the same time, flavorings such as mint and spicy spices can stimulate the oral mucosa, promote saliva secretion, help nicotine be released faster and absorbed through the mouth, and enhance the effect. In addition, the diverse flavors of flavorings (such as coffee, chocolate, cinnamon, etc.) can meet the preferences of different consumers and increase the product's appeal.

[0065] Among them, the porous structure of starch surface can effectively adsorb and protect flavorings, prevent them from volatilizing and oxidizing, extend the shelf life of the product, and ensure that the flavor of the product is stable and long-lasting during use.

[0066] Among them, the aforementioned sugar alcohol fillers can effectively fill the surface of active substances and fragrances, prolonging their duration of action. Sugar alcohol fillers can include substances such as xylitol, mannitol, lactitol, erythritol, isomaltitol, and sorbitol.

[0067] The aforementioned adhesive not only binds nicotine, flavorings, and other powders or granules into a uniform solid (such as in small packets or tablets), preventing loosening or breakage and thus maintaining the product's shape and structure, but also allows for the slow release of nicotine and flavor substances by adjusting the dissolution rate. This avoids excessive oral irritation or an overly strong taste caused by a large release at once. Furthermore, by controlling the type and proportion of the adhesive, the smoke can remain in the mouth for a longer period, enhancing the user experience. In addition, the adhesive binds fine particles into a smooth texture, preventing a gritty or uncomfortable feeling during use. It also helps nicotine, flavorings, pH adjusters, and other ingredients to be evenly distributed in the product, ensuring consistent dosage in every serving.

[0068] Among them, the sweeteners mentioned above can mask the bitter or irritating taste of nicotine, tobacco or plant fiber, enhancing the palatability of the product; at the same time, sweeteners can also enhance the sense of pleasure, making the product closer to the experience of snacks or candy, reducing the resistance to use; in addition, sweeteners work synergistically with flavorings to enhance the expression of flavors such as fruit and mint.

[0069] Among them, the plasticizers mentioned above can increase the softness and elasticity of oral products, prevent the products from drying and cracking, and can also adjust the dissolution rate of nicotine and flavorings by adjusting the porosity of the material.

[0070] The solvents mentioned above can help fat-soluble or water-soluble components such as nicotine and fragrances to be evenly dispersed in the matrix, and can also enhance the permeability of nicotine through the oral mucosa.

[0071] Among them, pH adjusters can not only neutralize the irritation of acidic components and reduce the burning sensation in the mouth, but also maintain a slightly alkaline environment. Nicotine is in a non-ionic state in an alkaline environment (pH 8-9), which is not only not easy to degrade, but also easier to be absorbed through the oral mucosa, thus enhancing bioavailability and extending shelf life.

[0072] In some embodiments, the adhesive may include at least one of polyvinyl alcohol (PVA), hydroxypropyl methylcellulose, sodium carboxymethyl cellulose, gum arabic, xanthan gum, and gelatin; the sweetener may include at least one of sucralose, acesulfame potassium, aspartame, and neotame; the pH adjuster may include at least one of sodium bicarbonate, sodium carbonate, and calcium carbonate; and the plasticizer may include at least one of propylene glycol, polyethylene glycol, and glycerin. These components not only increase the softness and elasticity of oral products such as cigarette smokers, but also lock in moisture, prevent the product from hardening, and extend its shelf life.

[0073] In this embodiment, the modified starch with porous surface serves as a highly efficient carrier. The presence of its pore structure can reduce the use of plasticizers or stabilizers such as antioxidants and preservatives. At the same time, because the modified starch has high adsorption capacity, it can reduce the use of adhesives and reduce the odor of active substances, thereby reducing the use of flavoring agents.

[0074] In some embodiments, the oral article comprises, by weight, parts of:

[0075] Modified starch 10-30 parts, sugar alcohol filler 35-72.2 parts, binder 0-6 parts, sweetener 0.2-1.5 parts, plasticizer 0-3 parts, pH adjuster 0.5-5 parts, flavoring 5-20 parts, antioxidant 0.1-2 parts, nicotine agent 4-15 parts.

[0076] In some embodiments, the oral product may further include 8 to 20 parts by weight of solvent.

[0077] In some embodiments, the oral product provided in this application is a mouth bag, including a bag body, an active agent is filled in the bag body, and the bag body is permeable to saliva.

[0078] The bag can be a fiber bag, and it is treated with pure water, sodium alginate solution, sodium hyaluronate solution, hydroxypropyl methylcellulose solution, etc. to maintain the humidity of the oral product.

[0079] In some embodiments, the shape of the oral product can be irregular, such as cylindrical, granular, strip-shaped, sheet-like, filament-like, or spherical, and can be adjusted according to different design requirements.

[0080] The oral products provided in this application can effectively improve the key issues of traditional oral cigarettes in terms of taste, nicotine release, stability, flavor retention, hygroscopicity, drug loading, and environmental friendliness. They can significantly improve product quality and user experience, while meeting the needs of modern consumers for health, environmental protection, and personalization.

[0081] This application provides a method for preparing a mouth-held product, such as... Figure 2 As shown, steps 201 to 202 are included:

[0082] Step 201: Provide modified starch with porous surface, wherein the modified starch has a solubility of less than 0.01g in water at 25℃±2℃ and a solubility of less than or equal to 0.5g in water at 40℃±2℃.

[0083] In this step, pores are formed on the surface of starch using biological, chemical, or physical methods, and the solubility of starch in water at 25℃±2℃ is controlled to be less than 0.01g / 100g water, and the solubility in water at 40℃±2℃ is less than or equal to 0.5g / 100g water. This results in a fine starch texture, good adsorption performance, and the ability to maintain the structural integrity of the pores in aqueous solution, which facilitates the stable loading of subsequent active substances.

[0084] Step 202: Load the active substance onto the modified starch to form a dry powder, thereby obtaining a mouth-held product.

[0085] In this step, active substances are loaded onto the starch surface by means of solution soaking, coating or spraying equipment, and then dried by drying / freeze-drying to obtain oral products.

[0086] Because modified starch has pores on its surface, using it as a carrier allows for the secure loading of active substances into these pores, resulting in a smoother, more mellow mouthfeel, reducing irritation and enhancing the user experience. Furthermore, the porous structure of the modified starch surface not only allows for more efficient adsorption of active substances and control of their release rate, thereby increasing the content of active ingredients and providing a more consistent absorption experience, but also effectively protects the active substances from volatilization and oxidation, extending the product's shelf life and ensuring a stable and lasting flavor during use. The modified starch has a solubility of less than 0.01g / 100g water at 25℃±2℃ and less than 0.5g / 100g water at 40℃±2℃, making it insoluble in water. This allows it to maintain the integrity of its pore structure in aqueous solutions, ensuring stable loading of active substances and continuous release. In addition, starch itself, as a natural polymer, is safe, non-toxic, and biodegradable, making it more environmentally friendly and healthier.

[0087] Therefore, the oral products provided in this application can effectively improve the problems of oral tobacco products, such as poor taste and insufficient load-bearing capacity of the carrier material, which easily cause oral discomfort and insufficient content of effective ingredients.

[0088] In some embodiments, step 201 above includes step 211:

[0089] Step 211: Use amylase to enzymatically hydrolyze starch.

[0090] In this embodiment, amylase and other enzymes are used to enzymatically hydrolyze natural starches such as corn starch, cassava starch, potato starch, wheat starch, barley starch, and mung bean starch, causing voids to appear in the internal structure of the starch and forming porous starch with pores on the surface.

[0091] In some possible embodiments, the amylase described above includes at least one of glucanase, dextranase, glucosylamylase, glycosylation enzyme, and α-amylase.

[0092] In some embodiments, step 201 above includes step 212:

[0093] Step 212: Using free radical polymerization, starch is grafted and copolymerized with porogens and acrylic monomers.

[0094] In this embodiment, acrylic monomers are grafted onto starch using a free radical polymerization method with a porogen to synthesize a starch-based macroporous superabsorbent polymer. The pore size, depth, and porosity of the starch surface pores can be controlled by the porogen.

[0095] In some embodiments, the pore-forming agent includes at least one of sodium bicarbonate and polyethylene glycol, which can form pores with a diameter of 0.5 to 1.5 μm, a depth of 3 to 50 μm, and a porosity of 55 to 65% on the starch surface. The pores are uniformly distributed on the starch surface, which can effectively improve the adsorption capacity and specific surface area while ensuring the structural stability of starch as a carrier.

[0096] In one embodiment, the specific surface area of ​​the starch is 30-40 m². 2 / g can combine high adsorption rate and active material loading efficiency, while improving the dissolution and release of active materials.

[0097] In some embodiments, the aforementioned acrylic monomers include at least one of acrylic acid and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS). The hydrophobic groups of the acrylic monomers can form covalent bonds with the starch molecular chains, thereby changing their surface properties and functions, forming a hydrophobic structure on the porous starch surface, and forming chemical bonds on the starch molecules through a reaction. The starch main chain serves as the backbone, and the grafted hydrophobic branches exist in the form of side chains, forming a comb-like topological structure of "main chain-branch chain", which can further improve hydrophobic properties and improve taste.

[0098] In some embodiments, after providing the modified starch with a porous surface, step 103 is further included:

[0099] A modifier having a hydrophobic group is added to the modified starch, and the hydrophobic group is controlled to undergo a substitution reaction with the hydroxyl groups in the modified starch.

[0100] In this embodiment, considering that starch is a biosynthesized semi-crystalline particle composed of two types of dextran, amylose and amylopectin, and that both dextran are composed of α-D-glucose units, and that there are three active hydrophilic hydroxyl groups (-OH) on C2, C3 and C6 of the glucose molecule, starch can be chemically modified to make it hydrophobic.

[0101] Hydrophobic modification of starch can be achieved by blocking or introducing functional groups.

[0102] In some embodiments, hydrophobic groups can be substituted with hydroxyl groups in starch through esterification, etherification, crosslinking, grafting, and condensation reactions to achieve chemical modification of starch, thereby improving the hydrophobicity of starch. The starch then becomes modified starch with hydrophobic groups and a crosslinked network structure, which enables the starch to maintain the integrity of the pore structure in aqueous solution, ensuring stable loading of active substances and thus continuously releasing active substances.

[0103] For example, hydrophobic groups can be grafted onto starch by reacting the hydroxyl groups (-OH) in starch molecules with acid anhydrides or acyl chlorides to form ester bonds (-O-CO-R); or by reacting the hydroxyl groups in starch molecules with reagents such as propylene oxide or chloroacetic acid to form ether bonds (-OR).

[0104] For example, during the esterification reaction, the reaction between the hydroxyl groups (-OH) of starch and the carboxyl groups (-COOH) in the esterifying agent is controlled, and the reaction equation is as follows:

[0105]

[0106] In some embodiments, the hydrophobic groups include at least one of lipo groups, acetyl groups, ester groups, and dialdehyde groups, which can effectively improve the hydrophobicity of starch while also providing a better taste.

[0107] For example, long-chain alkyl groups can be introduced through octenyl succinic anhydride esterification; acetyl groups and ester groups can be introduced by generating starch acetate through acetylation; and there are also complex groups, such as acrylates and dialdehyde groups.

[0108] In some implementations, step 202 includes:

[0109] By loading active substances and antioxidants onto the surface of the modified starch, and then loading at least one of flavorings, sugar alcohol fillers, binders, sweeteners, plasticizers, solvents, and pH adjusters, the oral product is obtained.

[0110] In this embodiment, active substances and antioxidants are first loaded onto the starch surface, and then flavorings, sugar alcohol fillers, binders, sweeteners, plasticizers, solvents, pH adjusters, etc. are loaded onto the starch surface using methods such as dip coating and spray granulation. This not only ensures that more active substances are loaded in the pores of the starch surface, but also allows antioxidants to fully contact the active substances, effectively protecting the active substances and preventing their volatilization and oxidation, thus extending the shelf life of the product.

[0111] The solvent mentioned above can specifically be deionized water.

[0112] In some embodiments, step 202 specifically includes: dissolving the active substance and antioxidant in a solvent to obtain a butyl salt solution; and drying the starch in the butyl salt solution under vacuum after standing to obtain a dry powder.

[0113] In some embodiments, after loading the active substance onto the modified starch to form dry powder, step 202 further includes: spraying the coating solution onto the dry powder using a fluidized bed granulation method to obtain an active agent with a fluidized bed coating.

[0114] In this embodiment, after obtaining the modified starch dry powder loaded with active substances, a coating solution including flavoring, binder, sweetener, plasticizer, solvent and pH adjuster is sprayed onto the starch surface by spray granulation to form a fluidized coating. This ensures that more active substances are loaded in the pores of the starch surface, effectively protects the active substances and prevents them from volatilizing and oxidizing, and extends the shelf life of the product.

[0115] In some embodiments, after obtaining the surfactant with a fluidized coating, step 202 further includes:

[0116] The active agent and sugar alcohol filler are mixed and then filled into a bag to obtain a lozenge.

[0117] In step 202 above, the formulas for each component, by mass percentage, are as follows:

[0118] Starch 10-30%, sugar alcohol fillers 35-72.2%, binders 0-6%, sweeteners 0.2-1.5%, plasticizers 0-3%, solvents 8-20%, pH adjusters 0.5-5%, flavorings 5-20%, antioxidants 0.1-2%, nicotine 4-15%.

[0119] To make the inventive objectives, technical solutions, and beneficial effects of this application clearer, the application is further described below with reference to embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of this application.

[0120] The present application will be described in detail below through embodiments.

[0121] Test methods

[0122] (1) Adsorption rate test of butyrate and flavoring:

[0123] Prepare nicotine ethanol solution with a concentration of 1 mg / mL and flavor ethanol solution with a concentration of 0.5 mg / mL. Weigh 0.5 g of the sample and add it to 10 mL of nicotine solution to ensure full contact. Stir with a magnetic stirrer at 37 °C for 2 h to allow the adsorption reaction to reach equilibrium. Then, centrifuge the mixture and take the supernatant to determine the nicotine content by HPLC.

[0124] Meanwhile, another sample was weighed and added to 10 mL of fragrance solution, and the adsorption experiment and determination were carried out in the same way.

[0125] Based on the nicotine and flavor content before and after adsorption, the adsorption capacity of porous starch and microcrystalline cellulose for nicotine and flavor is calculated; the adsorption capacity can be calculated using the following formula:

[0126] Nicotine adsorption rate = (nicotine content in the solution before adsorption - nicotine content in the solution after adsorption) / (nicotine content in the solution before adsorption) × 100%;

[0127] Fragrance adsorption rate = (fragrance content in the solution before adsorption - fragrance content in the solution after adsorption) / (fragrance content in the solution before adsorption) × 100%.

[0128] (2) Single-weight stability test:

[0129] After the formulation was prepared, a single-weight stability test was conducted when the product was bagged. The oral cigarette sample was designed to weigh 0.4g per bag, and the single-weight stability was verified using a 1 / 10,000 electronic balance.

[0130] (3) Nicotine content test:

[0131] The test was performed using HPLC-Aglient GC8890. The reagents were isopropanol (chromatographic grade) and ethanol (chromatographic grade); the standards were nicotine standard solution in isopropanol and n-heptadecane (internal standard).

[0132] (4) Nicotine dissolution ratio test:

[0133] The tests were performed using an Agilent 708-DS dissolution meter.

[0134] (5) Product stability test

[0135] The samples were sealed and stored in a box, and then an environmental accelerated test was conducted using a programmable temperature and humidity test chamber. The environmental test conditions were set as follows: temperature 50℃, humidity 90%, and placement time 5 days. The moisture content of the samples was then tested using a Japanese KEM 710S-ADP611 instrument, and the degree of color change of the samples after the environmental test was examined using a 3nhT7020 spectrophotometer.

[0136] (6) Product taste evaluation:

[0137] A comparative taste evaluation was conducted on the samples, mainly based on four dimensions: taste, aroma, irritation, and physiological sensation.

[0138] Examples 1-3

[0139] Oral products were prepared according to the formulations shown in Table 1 and the following preparation process:

[0140] (1) Weigh out nicotine tartrate and ascorbic acid according to the formula ratio and dissolve them in deionized water. Stir for 0.5 hours to obtain nicotine tartrate solution.

[0141] (2) Weigh out the carrier porous starch with a particle size of 100 μm, a pore size of 0.1 to 3 μm, a pore depth of 3 to 50 μm and a porosity of 50% according to the formula ratio, add it to the buty salt solution, continue to stir with a stirrer for 2 hours to ensure that the porous starch is completely adsorbed, and then let it stand for 1 hour to obtain wet powder.

[0142] (3) Spread the above wet powder evenly on the drying tray, close the drying chamber, start the vacuum pump to the target vacuum degree (-0.09MPa), then slowly raise the temperature to the set temperature of 40℃, and then keep it warm for 2 hours. After drying, turn off the heating, keep the vacuum state and cool naturally to below 30℃, slowly release the vacuum, take out the sample and put it into a sealed bag to obtain dry powder.

[0143] (4) Weigh out the flavoring, pH adjuster, sweetener sucralose, binder hydroxypropyl methylcellulose, and plasticizer polyethylene glycol and dissolve them completely in the solvent deionized water. Stir for 1 hour to obtain the flavoring coating solution.

[0144] (5) The above dry powder is placed on a fluidized bed, and the above fragrance coating solution is sprayed onto the dry powder to coat it with fragrance using a fluidized granulation method to obtain active agent granules; wherein, the inlet air temperature of the fluidized bed is controlled at 60-70℃, the material temperature is controlled at 35-40℃, the spraying rate is 6-10mL / min, the fan speed is 800-1600 rpm, and the moisture content is controlled to be less than 5%.

[0145] (6) Mix the activator particles with mannitol and erythritol, and mix for 0.5 hours using a three-dimensional mixer to obtain the finished powder.

[0146] (7) The finished powder is packaged in non-woven fabric, boxed, and plastic sealed using a mouth-holding cigarette sealing bag machine.

[0147] Table 1

[0148] Example 1 Example 2 Example 3 Raw material name Formula ratio (%) Formula ratio (%) Formula ratio (%) Porous starch 15.0％ 30.0％ 10.0％ Mannitol 28.0％ 18.0％ 38.0％ Erythritol 20.0％ 17.0％ 18.8％ Sucralose 1.0％ 1.5％ 0.5％ Hydroxypropyl methylcellulose 2.0％ 4.0％ 0.2％ polyethylene glycol 1.0％ 2.0％ 0.0％ Deionized water 15.0％ 10.0％ 15.0％ Sodium bicarbonate 1.5％ 1.0％ 1.0％ Grape flavoring 10.0％ 10.0％ 10.0％ ascorbic acid 0.5％ 0.5％ 0.5％ Nicotine tartrate salts 6.0％ 6.0％ 6.0％

[0149] Comparative Examples 1-3

[0150] Oral products were prepared according to the formulations shown in Table 2 and the following preparation process:

[0151] (1) Weigh out nicotine tartrate, ascorbic acid (antioxidant), and hydroxypropyl methylcellulose (binder) according to the formula ratio and dissolve them in deionized water. Stir for 2 hours to obtain nicotine tartrate coating solution.

[0152] (2) Weigh the sweetener sucralose and grape flavoring according to the formula ratio, and stir with a mixer for 1 hour to ensure that the sucralose is completely dissolved in the flavoring liquid to obtain the flavoring solution.

[0153] (3) Weigh out 100 μm carrier microcrystalline cellulose according to the proportion and place it on a fluidized bed. Coat the dry powder with the above butyrate coating solution by fluidized granulation to obtain activator granules. The inlet air temperature of the fluidized bed is controlled at 60-70℃, the material temperature is controlled at 35-40℃, the spraying rate is 6-10 mL / min, the fan speed is 800-1600 rpm, and the moisture content is controlled to be less than 5%.

[0154] (4) Mix the active agent particles with mannitol and erythritol, and mix for 0.5 hours using a three-dimensional mixer to obtain a filler mixture.

[0155] (5) The above-mentioned filler mixture is placed on a fluidized bed, and the above-mentioned fragrance solution is sprayed onto the filler mixture by fluidized granulation to obtain fluidized fragrance granules; wherein, the inlet air temperature of the fluidized bed is controlled at 50-60℃, the material temperature is controlled at 30-35℃, the spraying rate is 4-8mL / min, the fan speed is 800-1600 rpm, and the moisture content is controlled to be less than 5%.

[0156] (6) Mix the coating granules and flavor granules and mix them for 1 hour using a three-dimensional mixer to obtain the finished powder.

[0157] (7) The finished powder is packaged in non-woven fabric, boxed, and plastic sealed using a mouth-holding cigarette sealing bag machine.

[0158] Table 2

[0159]

[0160]

[0161] The adsorption rates of butyrate and fragrance were tested on the carriers in Example 1 and Comparative Example 1, respectively, and the tests were repeated 5 times. The results are shown in Table 3.

[0162] In addition, scanning electron microscopy was performed on the carrier in Example 1, and the results are as follows: Figure 3 As shown.

[0163] Table 3

[0164]

[0165] As can be seen from Table 3, microcrystalline cellulose has very little adsorption of nicotine or fragrance because its surface and interior are smooth and lack pores. In contrast, porous starch has a large number of tiny pores on its surface and interior, which allows it to adsorb and store active substances in solutions containing nicotine or fragrance, thus maintaining the stability of the active substances and reducing volatilization.

[0166] The products prepared in each embodiment and comparative example were subjected to single-weight stability tests, and the tests were repeated 5 times. The results are shown in Table 4.

[0167] Table 4

[0168]

[0169]

[0170] As can be seen from Table 4, the stability of each formulation is good, with a deviation fluctuation of 0.4±10%.

[0171] The nicotine content of the products prepared in each example and comparative example was tested. The actual nicotine contents of Examples 1-3 and Comparative Examples 1-3 were 19.67 mg / g, 19.78 mg / g, 19.34 mg / g, 18.91 mg / g, 19.03 mg / g, and 19.27 mg / g, respectively, with a loss of ±10%, indicating that the preparation process has good stability.

[0172] The results of nicotine dissolution ratio tests of the products prepared in each embodiment and comparative example are shown in Table 5 and 5, respectively. Figure 4 As shown.

[0173] Table 5

[0174]

[0175] The nicotine dissolution curves in Examples 1-3 showed that the porous starch oral nicotine release rate was slower than that of the microcrystalline cellulose oral nicotine release control group in the initial stage (1-10 minutes). This slowed nicotine release reduced irritation to the oral mucosa. Furthermore, in the middle stage (10-30 minutes), the porous starch oral nicotine continued to release nicotine slowly, effectively extending the duration of use. In contrast, the microcrystalline cellulose oral nicotine released almost all of its nicotine within 10 minutes. These results indicate that porous starch, due to its internal pores, stores and stabilizes nicotine, effectively controlling the nicotine release rate, resulting in more uniform nicotine release and maintaining nicotine stability. This not only improves the user experience but also reduces nicotine waste and provides a more comfortable taste.

[0176] The products prepared in each embodiment and comparative example were subjected to product stability tests. The color difference test was repeated 3 times. The results of the moisture content and color difference test are shown in Tables 6 and 7, respectively.

[0177] Table 6

[0178]

[0179] As can be seen from Table 2, adding too high a proportion of porous starch increases the water absorption capacity of the product, which can easily lead to higher moisture content after environmental testing.

[0180] Table 7

[0181]

[0182] As shown in Table 7, the color difference ΔE of porous starch oral smoke is less than 3, indicating that porous starch oral smoke has good stability after environmental testing. Oral smoke using porous starch as a carrier has better stability than microcrystalline cellulose oral smoke during long-term storage.

[0183] The taste evaluation of the products prepared in each embodiment and comparative example is shown in Table 8.

[0184] Table 8

[0185]

[0186] Rating instructions: The rating scale is 0.5 points, with 5 points being very satisfied, 4 points being satisfied, 3 points being average, 2 points being dissatisfied, and 1 point being very poor.

[0187] In summary, the oral products prepared by introducing porous starch as a carrier have the following advantages:

[0188] (1) Due to the presence of pores, porous starch has high adsorption capacity and high loading efficiency, which can effectively control the release rate of nicotine, make the release of nicotine more uniform, maintain the stability of nicotine, reduce nicotine oxidation, and extend the product's service life.

[0189] (2) The nano-sized porous starch has a uniform pore distribution, which ensures that nicotine and flavor molecules are evenly dispersed in the carrier, avoiding the irritation caused by excessive local concentration. This not only improves the user experience but also reduces the waste of nicotine. At the same time, it can maintain the stability of the flavor and reduce the loss of aroma.

[0190] (3) Porous starch can control the slow release and long-lasting release of smoke in the mouth. Nicotine and flavor molecules are combined through physical adsorption (van der Waals forces, capillary action) and weak chemical bonds (hydrogen bonds), and can be gradually desorbed in the moist environment of the oral cavity, thus prolonging the use time.

[0191] (4) Porous starch mouthwash has a soft feel in the mouth and no gritty feeling, avoiding the rough texture of traditional carriers (such as cellulose). The porous structure can absorb the bitterness and irritating smell of nicotine, improving the taste acceptance.

[0192] (5) Reasonably adjusting the proportion of porous starch in the oral tobacco formula can effectively control the product's moisture content, water absorption rate, and taste.

[0193] Although preferred embodiments of the present application have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the embodiments of the present application.

[0194] The above provides a detailed description of an oral product and its preparation method provided in this application. Specific examples have been used to illustrate the principles and implementation methods of this application. The description of the above embodiments is only for the purpose of helping to understand the method and core ideas of this application. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the ideas of this application. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A mouth-held product, characterized in that, Includes an active agent, said active agent comprising: The modified starch has a porous surface; the modified starch has a solubility of less than 0.01 g / 100 g water in water at 25℃±2℃, and a solubility of less than or equal to 0.5 g / 100 g water in water at 40℃±2℃. An active substance, wherein the active substance is loaded onto the modified starch.

2. The oral article according to claim 1, characterized in that, The modified starch has hydrophobic groups.

3. The oral article according to claim 2, characterized in that, The hydrophobic group includes at least one of aliphatic, acetyl, ester, and dialdehyde groups.

4. The oral article according to claim 1, characterized in that, The modified starch surface has pores with a diameter of 0.1–3 μm and a depth of 3–50 μm; and / or, the porosity of the modified starch surface is 55–65%; and / or, the specific surface area of ​​the modified starch is 30–40 m². 2 / g.

5. The oral article according to claim 1, characterized in that, The activator also includes a coating attached to the surface of the modified starch, the coating comprising at least one of flavoring, binder, sweetener, plasticizer, and pH adjuster.

6. The oral article according to claim 1, characterized in that, The oral product further includes at least one of flavorings, sugar alcohol fillers, binders, sweeteners, plasticizers, pH adjusters, and antioxidants; and / or, the active substance includes at least one of nicotine preparations and tobacco extracts.

7. The oral article according to claim 6, characterized in that, The oral product, by weight parts, comprises: Modified starch 10-30 parts, sugar alcohol filler 35-72.2 parts, binder 0-6 parts, sweetener 0.2-1.5 parts, plasticizer 0-3 parts, pH adjuster 0.5-5 parts, flavoring 5-20 parts, antioxidant 0.1-2 parts, nicotine agent 4-15 parts.

8. The oral article according to any one of claims 1 to 7, characterized in that, The oral product also includes a bag, and the active agent is filled in the bag.

9. A method for preparing a mouth-held product, characterized in that, The method for preparing the oral article as described in any one of claims 1 to 8 comprises: A modified starch with a porous surface is provided, wherein the modified starch has a solubility of less than 0.01 g / 100 g water in water at 25 °C ± 2 °C and a solubility of less than or equal to 0.5 g / 100 g water in water at 40 °C ± 2 °C. Active substances are loaded onto the modified starch to form a dry powder, thereby obtaining a lozenge.

10. The preparation method according to claim 9, characterized in that, After loading the active substance onto the modified starch to form a dry powder, the process further includes: The coating solution is sprayed onto the dry powder using a fluidized bed granulation method to obtain an active agent with a fluidized bed coating.

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