Hydrophobic modified powder system nicotine bag and preparation method thereof

Abstract

The invention relates to the technical field of nicotine bags, and discloses a hydrophobic modified powder system nicotine bag and a preparation method thereof, the nicotine bag is prepared from microcrystalline cellulose, hydrophobic fumed silica, nicotine, a humectant, water, an osmotic pressure regulator and other raw materials; the preparation method comprises the following steps: constructing functional particles through ordered steps: mixing microcrystalline cellulose with a high-osmotic-pressure pre-concentrated solution to form wet core particles with a high-osmotic-pressure core; a nicotine flavor agent mixed solution is applied to the surface; and adding hydrophobic fumed silica for coating to form hydrophobic modified particles with a core-shell structure, and mixing and sub-packaging to obtain the nicotine bag. By constructing a specific particle structure of a high osmotic pressure core and a hydrophobic shell, water loss is effectively inhibited, and the storage stability of the product is improved; during use, particles can be driven by osmotic pressure to be quickly disintegrated, so that nicotine and a flavoring agent can be instantly released, and the effect is quick; the powder flowability is improved, and the production efficiency and the product uniformity are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of nicotine pouches, in particular to a hydrophobically modified powder system nicotine pouch and a preparation method thereof. BACKGROUND

[0002] As a new emerging smokeless tobacco product, a nicotine pouch is usually composed of a powder mixture filled in a small bag, which contains nicotine, fillers, flavoring agents and other components, and provides users with an experience of replacing traditional tobacco through oral mucosa absorption to release nicotine. In the prior art, the performance and user experience of the nicotine pouch are highly dependent on the physical and chemical state of its powder system.

[0003] However, the existing nicotine pouch products generally face an inherent contradiction. In order to ensure the comfort and effective delivery of active substances during use, the product needs to maintain a certain moisture and softness, but this also makes it easy to dry and harden during storage and transportation due to water evaporation, resulting in a shortened shelf life of the product and a decreased user experience. The prior art usually adds a large amount of moisture retention agents to delay water loss, but this way has limited effect on improving long-term storage stability and cannot build an efficient water locking structure.

[0004] In addition, the release mechanism of nicotine and flavoring agents in the existing nicotine pouch mainly relies on simple passive diffusion. When the user places the nicotine pouch in the mouth, the active substances slowly dissolve from the powder matrix, and the release rate is slow, resulting in a need to wait for a period of time to feel obvious flavor stimulation and nicotine effect, lacking an instant and fast onset experience, thereby affecting the user's experience of the product.

[0005] At the same time, from the perspective of production and manufacturing, in order to achieve the desired moisture and flavor, various liquid or semi-solid raw materials often need to be added to the powder system. The presence of these components often causes adhesion between powder particles, making the flowability of the entire powder system poor. Poor powder mechanics directly affects the accuracy and efficiency of high-speed quantitative dispensing on the automated production line, easily causing uneven weight of individual products, increasing production costs and quality control difficulty. Therefore, how to develop a nicotine pouch technology that can both long-term retain moisture and quickly release, and is easy to handle during production, is a technical problem to be solved in the field. SUMMARY

[0006] In view of the deficiencies of the prior art, the present application provides a hydrophobically modified powder system nicotine pouch and a preparation method thereof, which solves the problems of poor storage stability of the nicotine pouch, slow release of active substances, and difficulty in efficient and accurate dispensing due to poor powder flowability.

[0007] To achieve the above object, the present application is implemented by the following technical solutions: the present application provides a hydrophobically modified powder system nicotine bag, which adopts the following technical solutions: The powder system is prepared from raw materials including the following components by weight: Microcrystalline cellulose 45-60 parts; hydrophobic fumed silica 1-2 parts; nicotine 3-5 parts; humectant 10-12 parts; water 8-12 parts; osmotic pressure regulator 3-5.5 parts; bulking agent 15-26 parts; sweetener 0.1-1 part; flavoring agent 1.5-2 parts.

[0008] By adopting the above technical solutions, the powder system particles prepared by the present application have a specific core-shell structure, which endows the product with functions in two dimensions of storage stability and instant use.

[0009] In terms of storage stability, the structure realizes water retention through a double mechanism: firstly, the microcrystalline cellulose serves as a porous framework, and the high-osmotic-pressure liquid composed of water, humectant and osmotic pressure regulator is adsorbed inside the microcrystalline cellulose, and the low water activity formed by high-concentration solutes binds water from the thermodynamic level; secondly, the outer layer of the particle is composed of a physical barrier of hydrophobic fumed silica, which hinders the diffusion of water to the external environment, and the double action of this thermodynamic binding and physical barrier endows the product with excellent water retention capacity during storage, i.e. high accelerated stability.

[0010] In terms of instant use, when the nicotine bag is in contact with saliva, the rapid release mechanism of its active substances is triggered: Establishment of osmotic pressure gradient: an osmotic pressure gradient is formed between the high-solute concentration inside the particle and the low-osmotic-pressure saliva environment outside.

[0011] Rapid inflow of water: under the driving of the osmotic pressure gradient, water rapidly penetrates through the hydrophobic shell and enters the interior of the particle.

[0012] Swelling of the framework and destruction of the structure: the inflow of water causes the microcrystalline cellulose serving as the particle framework to rapidly absorb water and swell, and the stress generated by the volume expansion is sufficient to destroy the hydrophobic fumed silica coating structure of the outer layer.

[0013] Rapid release of active substances: once the hydrophobic barrier is destroyed, the active ingredients such as nicotine and flavoring agent originally adsorbed inside and on the surface of the particle are rapidly dissolved and released, changing the release mode of nicotine from the traditional mode limited by slow diffusion to the rapid disintegration release mode driven by osmotic pressure, thereby realizing storage stability while ensuring rapid onset of active substances during use.

[0014] Preferably, the humectant is propylene glycol and glycerol.

[0015] By adopting the technical scheme, propylene glycol and glycerol are both efficient and safe humectants, and the combination use can not only effectively build a high osmotic pressure environment, but also cooperatively improve the touch and moisture of the powder, and help to regulate the release rate of nicotine.

[0016] Preferably, the osmotic pressure regulator comprises at least one organic acid selected from citric acid, malic acid and tartaric acid, and sodium chloride.

[0017] By adopting the technical scheme, sodium chloride as a strong electrolyte can efficiently increase the osmotic pressure, and the introduction of the organic acid not only cooperatively enhances the osmotic pressure effect, but also regulates the pH value of the system, is conducive to the stability of nicotine, and provides moderate flavor stimulation to improve the sensory experience.

[0018] Preferably, the flavoring agent is peppermint oil and spearmint oil.

[0019] By adopting the technical scheme, the combination use of peppermint oil and spearmint oil, which are common flavoring substances in the field, can provide cool and lasting composite aroma, effectively mask the bad taste of nicotine, and improve the user acceptance of the product.

[0020] In a second aspect, the present application provides a preparation method of a hydrophobically modified powder system nicotine bag, comprising the following steps: S1, taking microcrystalline cellulose as a carrier, adding a high osmotic pressure pre-concentrate containing water, a humectant and an osmotic pressure regulator to the microcrystalline cellulose to mix, so that the high osmotic pressure pre-concentrate is absorbed by the microcrystalline cellulose to form a wet core particle with a high osmotic pressure core; S2, applying a nicotine flavoring agent mixture containing nicotine and a flavoring agent to the surface of the wet core particle to form a liquid layer rich in nicotine and a flavoring agent on the surface of the wet core particle; S3, immediately after step S2, adding hydrophobic fumed silica to the wet core particle and mixing, so that the hydrophobic fumed silica is coated outside the liquid layer to form a hydrophobically modified particle; S4, adding a filler and a sweetener to the hydrophobically modified particle and mixing uniformly to obtain a final mixture; S5, dividing the final mixture into non-woven bags at a dosage of 0.4-0.6 grams per bag and heat-sealing to obtain a nicotine bag.

[0021] By adopting the technical scheme, the method of the present application is not simply mixing materials, but constructing a specific functional structure on the particle scale through orderly process steps, and the core mechanism lies in accurately regulating the physical and chemical properties of the particle interface.

[0022] Firstly, in step S1, the porous structure of microcrystalline cellulose is used as a framework to absorb the high-osmotic-pressure pre-concentrate solution containing high-concentration solutes inside, and a functional core of the particle, i.e. a high-osmotic-pressure area, is constructed, which is the power source for subsequent rapid water imbibition and rapid release.

[0023] Then, in step S2, a mixed solution composed of nicotine and an oily flavoring agent is applied to the surface of the wet core particle. Due to the certain interfacial tension between the mixed solution and the hydrophilic core inside, a relatively hydrophobic liquid interfacial layer tends to be formed on the surface of the particle. This step not only loads the active substance, but more importantly, creates a physical basis for the subsequent directional adsorption of the hydrophobic coating material.

[0024] Finally, in step S3, hydrophobic fumed silica is immediately added after the formation of the hydrophobic interfacial layer. Based on hydrophobic interaction, the fine particles of the hydrophobic fumed silica will preferentially adsorb, adhere to and spread on the hydrophobic liquid layer formed in step S2, rather than entering the hydrophilic core inside the particle. Through subsequent high-speed mixing, these silica particles are evenly coated on the outermost layer of the particle to form a physical hydrophobic barrier, i.e. a hydrophobic shell.

[0025] The finally obtained hydrophobically modified particles have the aforementioned core-shell structure, thereby exhibiting excellent powder mechanical properties (such as low rest angle and good flowability characterized by low Hausner ratio) on the macroscopic level, as well as the dual functions of storage stability and rapid release.

[0026] Preferably, before step S1, water, the humectant and the osmotic pressure regulator are mixed to prepare the high-osmotic-pressure pre-concentrate solution. Before step S2, nicotine is mixed with the flavoring agent to prepare the nicotine-flavoring-agent mixed solution.

[0027] By adopting the above technical solution, the liquid components are pre-mixed to ensure that the high-osmotic-pressure pre-concentrate solution and the nicotine-flavoring-agent mixed solution are in a uniform state before being added to the powder, thereby ensuring the consistency of the osmotic pressure of each particle core and the uniform loading of nicotine on the surface of the particle, and improving the quality stability and uniformity of the final product batch.

[0028] Preferably, all steps are carried out in a high-speed mixing granulator, wherein the stirring paddle speed in step S1 is 300-700 rpm until the liquid is completely absorbed, and the stirring paddle speed in step S2 is 400-800 rpm until the spraying of the nicotine-flavoring-agent mixed solution is completed.

[0029] By adopting the above technical solution, the key process parameters in the granulation process are limited. In step S1, a moderate speed is adopted, which is beneficial to the slow and uniform absorption of the liquid by the microcrystalline cellulose, and the formation of a full wet core particle. The step S2 promotes the rotating speed, which helps atomize the oily liquid and uniformly spread on the surface of the particles; and the plurality of steps are continuously completed in the same device, which simplifies the process flow, reduces the material transfer loss, and improves the production efficiency.

[0030] Preferably, in the S3 step, the rotating speed of the mixing paddle is 500-1000 rpm, and the mixing time is 3-10 minutes.

[0031] By adopting the above technical scheme, the high rotating speed of the stirring paddle can provide sufficient shearing force to depolymerize the hydrophobic fumed silica aggregate and uniformly disperse and fix it on the surface of the particles to form a dense and complete coating layer.

[0032] Preferably, in the S4 step, the rotating speed of the mixing paddle is 100-300 rpm, and the mixing time is 5-15 minutes.

[0033] By adopting the above technical scheme, low-speed stirring is adopted in the last mixing step, which aims to uniformly mix the filler and the hydrophobically modified particles while avoiding damage to the formed particle coating structure caused by high-speed shearing, thereby protecting the functionality of the particles.

[0034] Preferably, the hydrophobic fumed silica is added after all the liquid raw materials, the high-osmotic-pressure pre-concentrate, and the nicotine flavoring agent mixing liquid are completely added.

[0035] By adopting the above technical scheme, the key addition time of the hydrophobic fumed silica is specified and emphasized, and this timing is the fundamental guarantee for forming the core-shell structure. If it is added too early, it will be wetted by the hydrophilic high-osmotic-pressure pre-concentrate, thereby losing its hydrophobic surface properties and directional coating ability, and unable to form an effective hydrophobic barrier.

[0036] The present application provides a hydrophobically modified powder system nicotine pouch and a preparation method. It has the following beneficial effects: 1. The present application constructs a high-osmotic-pressure core containing water, humectants, and osmotic pressure regulators, and coats the outside of the particles with hydrophobic fumed silica, establishing a dual moisture retention mechanism of thermodynamic constraint and physical barrier synergy, effectively inhibiting the moisture escape of the product during storage and transportation, ensuring that the nicotine pouch can always maintain the ideal moisture and softness during the shelf life, and improving the storage stability of the product and the sensory experience of the user when opening the pouch.

[0037] 2、The present application changes the release mode of active substances from traditional slow diffusion to rapid disintegration release driven by osmotic pressure by designing the core-shell particle structure. When the product is in contact with saliva, the huge osmotic pressure gradient inside and outside the particle drives water to rapidly penetrate, causing the swelling of microcrystalline cellulose as the skeleton and the destruction of the external hydrophobic coating, thereby releasing nicotine and flavoring agents in a very short time, realizing the rapid effect of active substances, and meeting the needs of users for instant sensory stimulation and effect feedback.

[0038] 3、The present application improves the powder mechanical properties of the final mixture by constructing a hydrophobic fumed silica coating layer on the surface of the particles. The coating layer reduces the friction and adhesion between particles, giving the powder excellent flowability. Good flowability ensures smooth and uniform powder discharge in automated packaging equipment, thereby realizing high-speed and precise quantitative dispensing, improving production efficiency, and ensuring high consistency of the content weight between individual nicotine bag products. DETAILED DESCRIPTION

[0039] The technical solutions in the embodiments of the present application will be described below in conjunction with the preparation examples, examples, comparative examples and test examples of the present application. Obviously, the described examples are only a part of the embodiments of the present application, rather than all the embodiments. Based on the examples in the present application, all other examples obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0040] Preparation Example 1-2: Preparation Example 1: Preparation of high-osmotic-pressure pre-concentrate Pre-concentrate A1: 10.0 parts of purified water, 10.0 parts of propylene glycol, 2.0 parts of sodium chloride and 2.0 parts of citric acid were mixed in a stirring container at room temperature, and stirring was continued until all solid components were completely dissolved, to obtain a clear and uniform solution for standby use.

[0041] Pre-concentrate A2: 12.0 parts of purified water, 5.0 parts of glycerol, 5.0 parts of propylene glycol, 3.0 parts of sodium chloride and 2.5 parts of malic acid were mixed in a stirring container at room temperature, and stirring was continued until all solid components were completely dissolved, to obtain a clear and uniform solution for standby use.

[0042] Preparation Example 2: Preparation of nicotine-flavoring agent mixture Mixture B1: 3.0 parts of nicotine and 2.0 parts of peppermint oil were mixed at room temperature, and stirring was uniform, to obtain a clear oily liquid for standby use.

[0043] Mixture B2: 4.0 parts of nicotine and 1.5 parts of spearmint oil were mixed at room temperature, and stirring was uniform, to obtain a clear oily liquid for standby use.

[0044] Example 1-3: Example 1:

[0045] The present embodiment provides a preparation method of a hydrophobically modified powder system nicotine bag, and the raw materials used therein include, by weight fraction: Microcrystalline cellulose (PH-102) 55.0 parts, mannitol 20.0 parts, nicotine 3.0 parts, propylene glycol 10.0 parts, purified water 10.0 parts, hydrophobic fumed silica 1.5 parts, citric acid 2.0 parts, sodium chloride 2.0 parts, sucralose 0.5 parts, peppermint oil 2.0 parts.

[0046] The method comprises the following steps: First, according to the method of preparing pre-concentrate A1 in Preparation Example 1, 10.0 parts of purified water, 10.0 parts of propylene glycol, 2.0 parts of sodium chloride and 2.0 parts of citric acid are mixed to prepare a high-osmotic pre-concentrate; at the same time, according to the method of mixing liquid B1 in Preparation Example 2, 3.0 parts of nicotine and 2.0 parts of peppermint oil are mixed to prepare a nicotine flavoring agent mixture.

[0047] Put 55.0 parts of microcrystalline cellulose into a high-speed mixing granulator, and slowly spray the high-osmotic pre-concentrate prepared in step (1) into the granulator at a stirring paddle speed of 300-700 rpm, and continue stirring until the liquid is completely absorbed to form wet core granules.

[0048] Increase the stirring paddle speed to 400-800 rpm, and atomize and spray the nicotine flavoring agent mixture prepared in step (1) onto the surface of the wet core granules.

[0049] After the spraying is completed, immediately add 1.5 parts of hydrophobic fumed silica, and mix for 5 minutes at a speed of 500-1000 rpm for coating.

[0050] Reduce the speed to 100-300 rpm, add 20.0 parts of mannitol and 0.5 parts of sucralose, and mix for 10 minutes.

[0051] Take the final mixture out of the mixer, and divide it into non-woven fabric bags at a dosage of 0.5 grams per bag, and heat seal to obtain the finished product. Example 2:

[0052] The present embodiment provides a preparation method of a hydrophobically modified powder system nicotine bag, and the raw materials used therein include, by weight fraction: Microcrystalline cellulose (PH-200) 60.0 parts, mannitol 15.5 parts, nicotine 4.0 parts, propylene glycol 5.0 parts, glycerol 5.0 parts, purified water 12.0 parts, hydrophobic fumed silica 1.0 parts, malic acid 2.5 parts, sodium chloride 3.0 parts, sucralose 0.5 parts, spearmint oil 1.5 parts.

[0053] The method comprises the following steps: First, according to the method of preparing pre-concentrate A2 in Preparation Example 1, 12.0 parts of purified water, 5.0 parts of glycerol, 5.0 parts of propylene glycol, 3.0 parts of sodium chloride and 2.5 parts of malic acid are mixed to prepare a high-osmotic-pressure pre-concentrate; at the same time, according to the method of mixing liquid B2 in Preparation Example 2, 4.0 parts of nicotine and 1.5 parts of spearmint oil are mixed to prepare a nicotine flavoring agent mixture.

[0054] Put 60.0 parts of microcrystalline cellulose into a high-speed mixing granulator, slowly spray the prepared high-osmotic-pressure pre-concentrate into the granulator at a stirring paddle speed of 300-700 rpm, and continue to stir until the liquid is completely absorbed to form wet core granules.

[0055] Increase the stirring paddle speed to 400-800 rpm, and atomize and spray the nicotine flavoring agent mixture prepared in step (1) onto the surface of the wet core granules.

[0056] After spraying is completed, immediately add 1.0 part of hydrophobic fumed silica, and mix for 5 minutes at a speed of 500-1000 rpm for coating.

[0057] Reduce the speed to 100-300 rpm, add 15.5 parts of mannitol and 0.5 parts of sucralose, and mix for 10 minutes.

[0058] Take the final mixture out of the mixer, and pack it into non-woven fabric bags at a dosage of 0.5 grams per bag, and heat seal to obtain the finished product. Example 3:

[0059] The present embodiment provides a method for preparing a hydrophobically modified powder system nicotine bag, which uses raw materials including, by weight: 45.0 parts of microcrystalline cellulose (PH-101), 25.5 parts of mannitol, 5.0 parts of nicotine, 12.0 parts of glycerol, 8.0 parts of purified water, 2.0 parts of hydrophobic fumed silica, 1.5 parts of tartaric acid, 1.5 parts of sodium chloride, 0.5 parts of sucralose, and 2.0 parts of peppermint oil.

[0060] The method comprises the following steps: First, mix 8.0 parts of purified water, 12.0 parts of glycerol, 1.5 parts of sodium chloride and 1.5 parts of tartaric acid to prepare a high-osmotic-pressure pre-concentrate; at the same time, mix 5.0 parts of nicotine and 2.0 parts of peppermint oil to prepare a nicotine flavoring agent mixture.

[0061] Put 45.0 parts of microcrystalline cellulose into a high-speed mixing granulator, slowly spray the prepared high-osmotic-pressure pre-concentrate into the granulator at a stirring paddle speed of 300-700 rpm, and continue to stir until the liquid is completely absorbed to form wet core granules.

[0062] Increase the stirring speed to 400-800 rpm and atomize the nicotine flavoring mixture prepared in step (1) onto the surface of the wet core particles.

[0063] Immediately after spraying, add 2.0 parts of hydrophobic fumed silica and mix at 500-1000 rpm for 5 minutes to coat the product.

[0064] Reduce the speed to 100-300 rpm, add 25.5 parts mannitol and 0.5 parts sucralose, and mix for 10 minutes.

[0065] The final mixture is removed from the mixer, dispensed into non-woven bags at a rate of 0.5 grams per bag, and heat-sealed to obtain the finished product.

[0066] Comparative Examples 1-4: Comparative Example 1: Compared with Example 1, the types and proportions of raw materials used are exactly the same, the difference lies in the preparation method. This comparative example adopts a traditional one-step wet granulation process: all powder materials of microcrystalline cellulose, mannitol, sucralose, hydrophobic fumed silica, citric acid, and sodium chloride are premixed in a mixer; all liquid materials of nicotine, propylene glycol, purified water, and peppermint oil are mixed evenly in another container; then the liquid mixture is added to the powder mixture and granulated by high-speed stirring, and the remaining steps are the same as in Example 1.

[0067] Comparative Example 2: Compared with Example 1, the types and proportions of raw materials used are exactly the same, the difference lies in the preparation method. Although this comparative example uses a step-by-step process, it does not construct a high osmotic pressure core: all dry powders (except hydrophobic fumed silica) such as microcrystalline cellulose, sodium chloride, citric acid, mannitol, and sucralose are premixed; purified water and propylene glycol are mixed and added to the above powder for granulation; then a mixture of nicotine and peppermint oil is added; finally, hydrophobic fumed silica is added and mixed, and the remaining steps are the same as in Example 1.

[0068] Comparative Example 3: Compared with Example 1, the types and proportions of raw materials used are exactly the same. The difference lies in the timing of the addition of hydrophobic fumed silica in the preparation method. In this comparative example, the hydrophobic fumed silica is premixed with microcrystalline cellulose at the very beginning of the process, and then the high osmotic pressure pre-concentrated solution and nicotine flavoring agent mixture are added sequentially according to the subsequent steps of Example 1. The remaining steps are the same as in Example 1.

[0069] Comparative Example 4: The difference compared with Example 1 is that 1.5 parts of hydrophobic fumed silica is replaced by 1.5 parts of hydrophilic fumed silica (e.g. AEROSIL® 200), and all the rest of the raw material ratios and preparation methods are exactly the same as Example 1.

[0070] Test Examples 1-4: Test Example 1: Angle of repose test Purpose of experiment: Evaluate the flowability of powder systems prepared by different processes by measuring the angle of repose.

[0071] Experimental equipment and reagents: Angle of repose tester (fixed funnel method), electronic balance (precision 0.01 g), stopwatch.

[0072] Test samples: Finished powders prepared in Examples 1-3 and Comparative Examples 1-4.

[0073] Experimental steps: 1. Place the angle of repose tester horizontally, fix the funnel so that the lower end is 10.0 cm above the plane of the base plate.

[0074] 2. Accurately weigh 50.0 g of the powder sample to be tested.

[0075] 3. Pour the sample into the fixed funnel at once, let it flow naturally, and form a conical powder pile on the base plate.

[0076] 4. After the powder has completely flowed out and the pile is stable, measure the height of the pile (h) and the diameters of the pile in four different directions using a ruler, and calculate the average radius .

[0077] 5. Calculate the angle of repose (θ) by the formula . ).

[0078] 6. Repeat the measurement three times for each sample, record the data and calculate the average value.

[0079] Experimental data: Table 1. Angle of repose test results of different sample powders

[0080] Conclusion: The angle of repose is a key physical parameter for characterizing the flowability of powders. The test data in Table 1 shows that the powder systems prepared in Examples 1-3 have lower angles of repose than Comparative Examples 1-4.

[0081] The process method of the present application uses a step-by-step and orderly feeding sequence. First, the porous structure of microcrystalline cellulose is used to effectively absorb the liquid phase containing water and humectants inside the particles. Then, the hydrophobic components such as nicotine and liquid flavor are used to form an interfacial transition layer on the surface of the particles. Finally, the hydrophobic silicon dioxide is preferentially adsorbed and coated on the interface layer, so that the surface of the final particles exhibits a physical property of rich hydrophobic silicon dioxide. The surface characteristics reduce the capillary bridging effect and electrostatic adsorption between particles, thereby reducing the cohesion and friction between particles, so that the powder system has a lower rest angle.

[0082] In comparison, the conventional wet process of Comparative Example 1 leads to uniform distribution of liquid components inside and outside the particles, the particle surface is wet and sticky, the cohesion is large, and the flowability is poor. Although Comparative Examples 2 and 3 are operated in steps, they fail to build an effective and functional surface structure. In particular, in Comparative Example 3, the function of the hydrophobic silicon dioxide is destroyed by the subsequent liquid components due to its early addition, resulting in limited improvement in flowability. Comparative Example 4 uses hydrophilic silicon dioxide, which exacerbates water adsorption on the surface of the particles, resulting in the largest rest angle and the worst flowability. Therefore, the specific process sequence of the present application is the key to obtaining a good flowability powder.

[0083] Test Example 2: Hausner Ratio Test Purpose of the experiment: Determine the cohesion and flow characteristics of the powder system prepared by different processes by measuring the Hausner ratio.

[0084] Experimental equipment and reagents: powder tap density instrument, 100 mL graduated cylinder, electronic balance (accuracy 0.01 g). Test samples: finished powders prepared in Examples 1-3 and Comparative Examples 1-4.

[0085] Experimental steps: 1. Accurately weigh 50.0 g of the sample to be tested.

[0086] 2. Slowly and evenly add the sample through the funnel into a clean and dry 100 mL graduated cylinder, avoiding vibration, and record the bulk volume .

[0087] 3. Fix the graduated cylinder containing the sample on the powder tap density instrument.

[0088] 4. Set the vibration frequency to 250 times / min, the vibration amplitude to 3 mm, and the cumulative vibration to 500 times.

[0089] 5. After the vibration is completed, remove the graduated cylinder from the instrument, read and record the tap volume .

[0090] 6. Calculate the Hausner ratio of the sample by the formula: Hausner ratio .

[0091] 7. Each sample was measured in triplicate, and the data was recorded and averaged.

[0092] Experimental data: Table 2. Hausner ratio of different sample powders

[0093] Conclusion: Hausner ratio is a direct measure of the compressibility of the powder, reflecting the inter-particle cohesion and flowability. The test data in Table 2 shows that the Hausner ratios of Examples 1-3 are all close to 1.1, lower than those of Comparative Examples 1-4.

[0094] The preparation method of the present application forms a physical barrier on the surface of the particles by a series of process steps, effectively reducing the polarity and hygroscopicity of the particle surface, weakening the van der Waals force and liquid bridge force between particles, thereby reducing the cohesion between the powder particles. The reduction of cohesion allows the powder to form a relatively tight accumulation in a loose state, with a small difference between the loose volume and the tapped volume, resulting in a lower Hausner ratio.

[0095] The preparation method of Comparative Example 1-4 fails to form the aforementioned effective surface structure. The particle surfaces of Comparative Examples 1 and 4 have high surface energy due to the exposure of liquid components or the presence of hydrophilic silica, resulting in strong inter-particle adhesion and high cohesion of the powder, with a large difference between the loose volume and the tapped volume, and the highest Hausner ratio. The preparation sequence of Comparative Examples 2 and 3 cannot achieve effective surface coating of the hydrophobic agent, and the inter-particle force is weakened but still higher than that of the examples, so the Hausner ratio is also at a higher level. The data shows that the specific process sequence used in the present application is the fundamental reason for reducing the cohesion of the powder system and improving its flow characteristics.

[0096] Test 3: Accelerated stability (water retention) test Purpose of the experiment: To evaluate the water retention capacity of finished products prepared by different processes under accelerated conditions to characterize their storage stability.

[0097] Experimental equipment and reagents: constant temperature and humidity chamber, analytical balance (precision 0.0001 g), tweezers, timer. Test samples: finished product bags prepared by Examples 1-3 and Comparative Examples 1-4.

[0098] Experimental steps: 1. From the finished products of Examples 1-3 and Comparative Examples 1-4, 10 bags were randomly selected from each group as test samples.

[0099] 2. The initial weight of each bag of samples was accurately weighed using an analytical balance and recorded as .

[0100] 3. All samples were single-layered on the tray and placed in a constant temperature and humidity chamber preset at 40±2°C and 25±5% RH. The low humidity environment was intended to accelerate the evaporation of moisture in the samples.

[0101] 4. The samples were taken out at the 7th day, 14th day and 28th day, respectively, and balanced at room temperature for 15 minutes after being taken out to eliminate the influence of temperature on the measurement.

[0102] 5. The weight of the samples at each time point was accurately measured again using the same analytical balance, and recorded as .

[0103] 6. The weight loss percentage of each sample at each time point was calculated according to the formula .

[0104] 7. The average weight loss rate of each group of 10 samples was calculated as the final test result of the group of samples at the corresponding time point.

[0105] Experimental data:

[0106] Table 3. Average weight loss rate of different samples under accelerated conditions

[0107] Conclusion: The accelerated stability test results in Table 3 show that the weight loss rates of the samples of Examples 1-3 are lower than those of all the comparative samples within 28 days.

[0108] The particle structure constructed by the preparation method of the present application has a dual water locking mechanism. One is that a high osmotic pressure concentrate is prepared in advance and is adsorbed by the microcrystalline cellulose core, and the low water activity formed by high concentration solutes thermodynamically binds the migration of water molecules. The other is that the subsequent formation of a hydrophobic silica coating layer on the surface of the particles constitutes a physical barrier, hindering the diffusion of water vapor to the outside world. This internal and external synergistic effect leads to the excellent water retention capacity of the sample of the example.

[0109] The traditional process used in Comparative Example 1 causes the uniform distribution of liquid components inside and outside the particles, without effective barriers, and the water loss is serious. Comparative Example 4 uses hydrophilic silica, which instead accelerates the exchange of water with the external environment, with the highest weight loss rate. The preparation sequence of Comparative Examples 2 and 3 fails to form a complete and functional hydrophobic surface structure, and cannot effectively block water. The water retention performance is between that of the example and Comparative Examples 1 and 4. The data prove that the present application can effectively inhibit the water loss of the product during storage by constructing a high osmotic pressure core and combining an orderly hydrophobic coating process.

[0110] Test 4: In vitro nicotine release rate test Objective: To evaluate and compare the release behavior of nicotine from samples prepared by different processes using in vitro dissolution test.

[0111] Experimental equipment and reagents: Dissolution tester (according to Chinese Pharmacopoeia or USP Apparatus 2, paddle method).

[0112] High-performance liquid chromatography (HPLC) system with ultraviolet detector.

[0113] Analytical balance, syringe, 0.22 μm needle filter.

[0114] Artificial saliva buffer solution (containing phosphate, sodium chloride, etc., adjusted to pH 6.8 ± 0.05).

[0115] Nicotine standard (purity ≥ 99.5%).

[0116] Chromatographic conditions: Chromatographic column: C18 reversed-phase chromatographic column (e.g., 4.6 mm x 250 mm, 5 μm).

[0117] Mobile phase: acetonitrile: water: triethylamine = 10:90:0.2 (v / v / v), adjusted to pH 7.0 with phosphoric acid.

[0118] Flow rate: 1.0 mL / min.

[0119] Detection wavelength: 260 nm.

[0120] Column temperature: 30°C.

[0121] Dissolution conditions and experimental steps: 1. Add 900 mL of artificial saliva buffer solution to each dissolution cup of the dissolution tester, preheat and maintain at 37 ± 0.5°C, start the paddle, and set the rotation speed to 50 rpm.

[0122] 2. Fix one portion of the sample bag to be tested in the sinker basket at the bottom of the dissolution cup.

[0123] 3. Start the timer. At the time points of 1, 2, 5, 10, 15, and 30 minutes, take out 5 mL of the dissolution solution from the dissolution cup.

[0124] 4. After each sampling, immediately supplement 5 mL of the same temperature blank artificial saliva buffer solution to the dissolution cup.

[0125] 5. After filtration with a 0.22 μm filter, inject the sample solution into the HPLC system for analysis to determine the nicotine concentration.

[0126] 6. According to the measured concentration and the labeled amount of nicotine, calculate the cumulative release rate at each time point.

[0127] 7. Each sample set was measured in triplicate and the average cumulative release rate was calculated.

[0128] Experimental data: Table 4. Cumulative release rate of nicotine from different samples in the in vitro dissolution medium

[0129] Conclusion: The in vitro dissolution data show that the nicotine release rate of the samples of Examples 1-3 is faster than that of the samples of Comparative Examples 1-4. Within the first 5 minutes of testing, the cumulative release rate of the samples of Examples has exceeded 70%, while the release rate of all the samples of Comparative Examples is less than 31%.

[0130] The phenomenon is caused by the particle structure built by the preparation process of the present application. The core of the particles of Examples contains high concentrations of salt and humectant, forming a high osmotic pressure area. When the sample is in contact with the dissolution medium with low osmotic pressure, the huge osmotic pressure gradient inside and outside the particle drives the dissolution medium to rapidly penetrate into the core of the particle. The rapid influx of water causes the rapid swelling of the microcrystalline cellulose as the skeleton, which in turn destroys the hydrophobic barrier of the outer layer, allowing the internal adsorbed nicotine to be released rapidly. This process changes the release mechanism of nicotine from diffusion control to a rapid release mode driven by osmotic pressure.

[0131] In contrast, Comparative Example 1, due to the homogeneous mixing of components, the hydrophobic agent is distributed throughout the system, hindering the infiltration of the medium, and the release of nicotine depends on slow passive diffusion. Comparative Examples 2 and 3 fail to build an effective osmotic pressure gradient core or a complete hydrophobic outer shell, and cannot start the release mechanism driven by osmotic pressure. Comparative Example 4 uses hydrophilic silicon dioxide which forms a gel layer after contacting with water, further increasing the diffusion resistance of nicotine, resulting in the slowest release rate. The test results confirm that the osmotic pressure gradient structure built by the specific process sequence of the present application is the key to achieving rapid release of nicotine.

Claims

1. A nicotine bag based on a hydrophobically modified powder system, characterized in that, Made from the following ingredients in parts by weight: 45-60 parts of microcrystalline cellulose; 1-2 parts of hydrophobic fumed silica; Nicotine 3-5 parts; 10-12 parts of moisturizer; 8-12 parts water; 3-5.5 parts of osmotic pressure regulator; 15-26 parts filler; Sweetener 0.1-1 part; Flavoring agent 1.5-2 parts.

2. The nicotine bag of the hydrophobic modified powder system according to claim 1, characterized in that, The humectant is propylene glycol and glycerol.

3. The nicotine bag of the hydrophobic modified powder system according to claim 1, characterized in that, The osmotic pressure regulator comprises at least one organic acid selected from citric acid, malic acid, and tartaric acid, and sodium chloride.

4. The nicotine bag of the hydrophobic modified powder system according to claim 1, characterized in that, The flavoring agents are peppermint oil and spearmint oil.

5. A method for preparing nicotine bags using a hydrophobically modified powder system, characterized in that, Includes the following steps: S1. Using microcrystalline cellulose as a carrier, a high osmotic pressure pre-concentrate containing water, a humectant, and an osmotic pressure regulator is added to the microcrystalline cellulose and mixed, so that the high osmotic pressure pre-concentrate is absorbed by the microcrystalline cellulose to form wet core particles with a high osmotic pressure core. S2. Apply a nicotine flavoring mixture containing nicotine and flavoring agent to the surface of the wet core particles to form a liquid layer rich in nicotine and flavoring agent on the surface of the wet core particles; S3. Immediately after step S2, hydrophobic fumed silica is added to the wet core particles and mixed to coat the liquid layer with the hydrophobic fumed silica, forming hydrophobic modified particles. S4. Add filler and sweetener to the hydrophobic modified particles and mix evenly to obtain the final mixture; S5. The final mixture is dispensed into non-woven bags at a quantitative rate of 0.4-0.6 grams per bag and then heat-sealed to obtain nicotine bags.

6. The method for preparing nicotine bags using a hydrophobic modified powder system according to claim 5, characterized in that, Before step S1, water, the humectant, and the osmotic pressure regulator are mixed to prepare the high osmotic pressure pre-concentrated solution; before step S2, nicotine and the flavoring agent are mixed to prepare the nicotine flavoring agent mixture.

7. The method for preparing nicotine bags using a hydrophobic modified powder system according to claim 5, characterized in that, Steps S1, S2, S3, and S4 are all performed in a high-speed mixing granulator. In step S1, the stirring paddle speed is 300-700 rpm until the liquid is completely absorbed. In step S2, the stirring paddle speed is 400-800 rpm until the nicotine flavoring agent mixture is sprayed.

8. The method for preparing nicotine bags using a hydrophobic modified powder system according to claim 5, characterized in that, In step S3, the mixing impeller speed is 500-1000 rpm, and the mixing time is 3-10 minutes.

9. The method for preparing nicotine bags using a hydrophobic modified powder system according to claim 5, characterized in that, In step S4, the mixing impeller rotates at 100-300 rpm and the mixing time is 5-15 minutes.

10. The method for preparing nicotine bags using a hydrophobic modified powder system according to claim 5, characterized in that, The hydrophobic fumed silica is added only after all liquid raw materials, the high osmotic pressure pre-concentrated solution, and the nicotine flavoring agent mixture have been added.

Images