Anti-caking and easily-stored polygonatum sibiricum powder and preparation process thereof

Abstract

The present application relates to the technical field of traditional Chinese medicine processing, and specifically relates to a kind of anti-caking easy-to-store rhizoma polygonati powder and its preparation process, which sequentially includes raw material selection, washing, slicing, curing, drying, low-temperature wall-breaking ultrafine grinding, anti-caking treatment, low-temperature sterilization, nitrogen-filled packaging and storage steps.Curing and drying control moisture content to be less than or equal to 5%, low-temperature grinding (pulverizer material tank temperature is -15 to -10℃) in a constant temperature 22℃ environment, cell wall (membrane) breaking rate reaches more than 95%, anti-caking can be achieved by adding 0.2%-0.5% anti-caking agent or premixing 10%-20% poria cocos / maltodextrin freeze-drying, and after cobalt-60 irradiation sterilization, PET / AL / PE aluminum foil composite bag is used for nitrogen-filled packaging.The present application can store rhizoma polygonati powder for 18-24 months without obvious caking, the retention rate of active ingredients is greater than or equal to 86%, the process is simple, the cost is controllable, and the present application is suitable for industrial production, and a method for repairing hardened rhizoma polygonati powder is also provided.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine processing technology, specifically to a powder of Polygonatum rhizome that is easy to store and prevents clumping, and its preparation process. Background Technology

[0002] Polygonatum, a traditional Chinese medicine, possesses the effects of tonifying qi and nourishing yin, strengthening the spleen and moistening the lungs, and benefiting the kidneys and replenishing essence. Its main active ingredients are polysaccharides and saponins, which are highly favored by consumers. With the modernization of traditional Chinese medicine and the industrialization of food processing, Polygonatum powder is widely used in pharmaceuticals, health products, and food due to its convenient consumption and rapid absorption. However, Polygonatum itself contains a relatively high amount of polysaccharides and starch, which, after being processed into powder, easily absorb moisture from the air, causing the powder particles to stick together and clump. This not only affects the appearance and flowability of the product but also leads to microbial growth, causing quality deterioration and shortening the shelf life.

[0003] Current processes for preparing Polygonatum sibiricum powder commonly suffer from incomplete drying, excessively high temperatures during pulverization, and simplistic packaging. This results in noticeable clumping within 12 hours of pulverization and discoloration and off-taste within 3 months, severely impacting product quality and market competitiveness. While some manufacturers have attempted to alleviate clumping by adding anti-caking agents or improving drying methods, these approaches often suffer from drawbacks such as excessive anti-caking agent dosage, uneven drying, and unscientific process parameters. These either fail to effectively solve the clumping problem or damage the active ingredients of Polygonatum sibiricum, affecting its efficacy and safety. Furthermore, existing processes have stringent storage requirements and generally short shelf lives, typically not exceeding 12 months, making them unsuitable for industrial production and market distribution. Therefore, there is an urgent need to develop an anti-caking, easily stored Polygonatum sibiricum powder and its preparation process to overcome the shortcomings of current applications. Summary of the Invention

[0004] The purpose of this invention is to provide a non-caking and easily stored Polygonatum powder and its preparation process, so as to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] A caking-resistant and easily stored Polygonatum powder, wherein the moisture content of the Polygonatum powder is ≤5%, and it contains an anti-caking component;

[0007] The Polygonatum powder is packaged in nitrogen-filled packaging, and the packaging material is a composite packaging material that is oxygen-barrier, moisture-proof, and light-proof.

[0008] As a further aspect of the present invention: the anti-caking component is a food-grade anti-caking agent, and the amount added is 0.2%-0.5% of the mass of the pulverized Polygonatum powder;

[0009] Alternatively, the anti-caking component may be a functional excipient, and the amount added is 10%-20% of the mass of the Polygonatum odoratum raw material before maturation.

[0010] As a further aspect of the present invention: the content retention rate of Polygonatum polysaccharides in the Polygonatum powder is ≥86%, and the content retention rate of Polygonatum saponins is ≥88%.

[0011] A process for preparing Polygonatum sibiricum powder that is easy to store and prevents caking includes raw material pretreatment, aging and drying, pulverization, sterilization and packaging steps, and also includes an anti-caking treatment step;

[0012] Among them, the moisture content of the material after aging and drying is ≤5%;

[0013] The pulverization is a low-temperature pulverization, carried out in a clean environment with a constant temperature of 22℃ and a relative humidity of <45%.

[0014] The sterilization process employs cobalt-60 irradiation.

[0015] The packaging is nitrogen-filled, using composite packaging materials that are oxygen-barrier, moisture-proof, and light-proof, with a nitrogen replacement rate of ≥99%.

[0016] As a further aspect of the present invention: the anti-caking treatment involves adding a food-grade anti-caking agent to the Polygonatum sibiricum granules before low-temperature pulverization and mixing them evenly;

[0017] The food-grade anti-caking agent is selected from one or more of silicon dioxide, tricalcium phosphate, sodium aluminosilicate, microcrystalline cellulose, and maltodextrin.

[0018] As a further aspect of the present invention: the anti-caking treatment is to mix the Polygonatum sibiricum raw material and functional excipients evenly before vacuum freeze-drying before aging and drying;

[0019] The functional excipients are Poria cocos powder or maltodextrin.

[0020] As a further aspect of the present invention: the ripening and drying includes a steaming step, and after steaming, it is dried at a low temperature until the moisture content is ≤5%;

[0021] The low-temperature drying method is selected from one of the following: heat pump drying, vacuum freeze drying, and microwave drying.

[0022] As a further aspect of the present invention: the low-temperature pulverization adopts a low-temperature ultrafine pulverizer with a built-in cooling system, the material tank temperature is -15 to -10℃, the pulverizer speed is 15000-20000r / min, and the feeding speed is 5-10kg / h.

[0023] As a further aspect of the present invention, the irradiation dose for cobalt-60 irradiation sterilization is 5-10 kGy.

[0024] As a further aspect of the present invention, it also includes a repair step for caking Polygonatum sibiricum powder: the caking Polygonatum sibiricum powder is dried at a low temperature of 50-55℃, placed in a vacuum freeze dryer for 24 hours, placed in a low temperature wall-breaking pulverizer for pulverizing for 10 minutes, and then anti-caking components are added and mixed evenly, and then repacked with nitrogen.

[0025] Compared with the prior art, the beneficial effects of the present invention are:

[0026] This invention adopts a systematic anti-caking solution, which addresses the technical problem of moisture absorption and clumping of Polygonatum powder from five dimensions: water control at the source, humidity control in the environment, temperature control in the process, physical isolation, and air isolation. The Polygonatum powder still shows no obvious clumping after 18-24 months of storage and has good fluidity.

[0027] This invention strictly controls the process parameters at each stage, especially the ripening, drying, and low-temperature cell wall breaking and ultra-fine pulverization stages, which can retain the effective components such as polysaccharides and saponins in Polygonatum to the greatest extent, avoid degradation of the effective components, and ensure the efficacy and quality of Polygonatum powder. At the same time, the cobalt-60 irradiation low-temperature sterilization and nitrogen-filled packaging effectively inhibit the growth of microorganisms, prevent the deterioration of the quality of Polygonatum powder, and extend the shelf life.

[0028] The process of this invention is scientific and reasonable, easy to operate, and all required equipment are conventional equipment in the field of Chinese herbal medicine processing. No new special equipment is needed, production costs are controllable, and it is suitable for large-scale industrial production. The amount of anti-caking agent added complies with national standards, is safe for consumption, and natural anti-caking solutions can be selected according to needs to meet different market demands.

[0029] This invention provides an effective treatment method for caking Polygonatum powder, which can restore the quality and flowability of Polygonatum powder, reduce product waste, and improve resource utilization. At the same time, the storage requirements are relatively relaxed, which facilitates market circulation and storage management. Attached Figure Description

[0030] Figure 1 This is a flowchart illustrating the preparation process of the anti-caking and easily stored Polygonatum powder in this embodiment of the invention. Detailed Implementation

[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0032] The specific implementation of the present invention will be described in detail below with reference to specific embodiments.

[0033] Please see Figure 1This invention provides an anti-caking and easily stored Polygonatum powder and its preparation process, including two preparation process routes: Route 1 is a process of adding anti-caking agents after preparation, which achieves anti-caking through full-process control of "source water control - environmental humidity control - process temperature control - physical isolation - air isolation", resulting in high efficacy retention and low production cost; Route 2 is a premixed excipient freeze-drying process, which further enhances the anti-hygroscopic ability by adding functional excipients before pulverization and synergistic freeze-drying, suitable for the needs of high-end natural products. Polygonatum powder prepared by both process routes can maintain excellent flowability and efficacy during a storage period of 18-24 months.

[0034] I. Process Route 1: Preparation Process of Polygonatum Powder with Post-Addition Anti-caking Agent

[0035] This process includes eight steps in sequence: raw material selection, cleaning and slicing, maturation and drying, low-temperature cell wall breaking and ultra-fine pulverization, anti-caking treatment, low-temperature sterilization, nitrogen-filled packaging and storage, as detailed below:

[0036] 1. Raw Material Selection: Select high-quality Polygonatum rhizomes that are free from rot, pests, and mechanical damage. Manually remove surface impurities, soil, and rotten parts before use. This step reduces the risk of microbial contamination and quality deterioration from the source, which is crucial to ensuring the basic quality of Polygonatum powder.

[0037] 2. Cleaning and slicing: Place the selected Polygonatum rhizome into a soaking tank / vessel, add clean water and soak for 10-20 minutes to initially soften the surface soil; then transfer it to a high-pressure spray cleaning machine and rinse with 0.3-0.5MPa high-pressure water flow to efficiently remove surface mud, impurities and residual dirt. After cleaning, drain the water.

[0038] After draining, place the Polygonatum rhizome into a slicer and cut it into uniform thin slices with a thickness of 3-5mm. This thickness ensures that the subsequent cooking is uniform and the drying is thorough, while also improving the pulverization efficiency and avoiding uneven particle size during the pulverization process.

[0039] 3. Cooking and drying: Place the sliced ​​Polygonatum sibiricum into a steamer and steam it with saturated steam provided by a steam boiler for 30-60 minutes.

[0040] This steaming time can fully promote the conversion of effective components such as Polygonatum polysaccharides and Polygonatum saponins inside Polygonatum, while inactivating enzymes such as polyphenol oxidase and amylase in the raw materials, preventing the degradation of effective components during subsequent processing, and killing some microorganisms on the surface and inside of the raw materials, reducing the pressure of subsequent sterilization.

[0041] After steaming, the Polygonatum slices are immediately transferred to a low-temperature drying device, with the drying temperature controlled at 40-65℃, and dried continuously until the moisture content of the Polygonatum slices is ≤5%, preferably controlled at 4%-6%. The dried Polygonatum slices are then pulverized into Polygonatum particles of approximately 10 mesh. The low-temperature drying device can be a heat pump drying room, a vacuum freeze dryer, or a microwave dryer, with a heat pump drying room being preferred due to its energy efficiency, high performance, and controllable temperature, which maximizes the preservation of the quality and active ingredients of Polygonatum.

[0042] If using traditional methods, a "nine-steaming and nine-drying" process can be employed. Each steaming process uses 0.1 MPa saturated steam for 30 minutes. Each drying process takes place in a clean, well-ventilated drying area at 25-30℃ and relative humidity ≤60%, until the moisture content of the Polygonatum slices reaches 10%-12%. This steaming and drying process is repeated nine times, with the final drying stage ensuring the moisture content of the Polygonatum slices is ≤5%, guaranteeing thorough steaming and drying, and uniform drying. Uneven drying is the main cause of subsequent clumping in Polygonatum powder; therefore, this step requires strict control of drying temperature and time to ensure that the moisture content of each slice meets the standard.

[0043] 4. Low-Temperature Cell Wall Breaking and Ultrafine Grinding: The grinding operation is carried out in a clean workshop with a constant temperature of 22℃ and a relative humidity of <45% to prevent moisture from the environment from entering the Polygonatum powder. A low-temperature ultrafine pulverizer with a built-in cooling system is used. The dried Polygonatum granules are fed into the pulverizer. The material tank temperature is -15 to -10℃, the pulverizer speed is 15000-20000 r / min, and the feeding speed is 5-10 kg / h.

[0044] In some embodiments of the present invention, the material temperature can be controlled at -20°C using a cryogenic cooling system, further reducing the risk of softening and sticking of Polygonatum polysaccharides. Low-temperature pulverization prevents the heat generated during pulverization from causing the Polygonatum powder to heat up and absorb moisture, while also preventing the degradation of the effective components of Polygonatum due to high temperatures. The pulverized product yields Polygonatum powder with a uniform particle size of approximately 100 mesh.

[0045] 5. Anti-caking treatment: Add food-grade anti-caking agent to the pulverized Polygonatum powder and mix using a mixer for 10-15 minutes to ensure that the anti-caking agent and Polygonatum powder are evenly mixed. The amount of anti-caking agent added is 0.2%-0.5% of the weight of Polygonatum powder, preferably 0.3%.

[0046] The food-grade anti-caking agent is selected from one or more of silicon dioxide, tricalcium phosphate, sodium aluminosilicate, microcrystalline cellulose, and maltodextrin, with silicon dioxide (micronized silica gel) being preferred. It has a strong ability to adsorb free water and can form a uniform isolation film on the surface of Polygonatum powder particles, effectively preventing particles from sticking together and clumping.

[0047] For a natural and environmentally friendly approach, a natural anti-caking solution can be adopted, incorporating 10%-20% Poria cocos by weight of Polygonatum odoratum powder. Its porous structure adsorbs free water and blocks inter-particle contact, achieving a synergistic anti-caking effect without affecting the flavor and efficacy of Polygonatum odoratum. The addition of anti-caking agents must strictly comply with the provisions of the "National Food Safety Standard for the Use of Food Additives" (GB 2760-2024) and be clearly labeled on the product label.

[0048] 6. Low-temperature sterilization: The Polygonatum sibiricum powder is sterilized using cobalt-60 irradiation, with the irradiation dose controlled at 5-10 kGy. This method, with its low temperature and strong penetrating power, effectively kills the total bacterial count, molds, yeasts, and other microorganisms in the Polygonatum sibiricum powder without damaging its active ingredients or affecting product quality. It is a commonly used sterilization method for Chinese medicinal herb powders. After sterilization, the microbiological indicators of the Polygonatum sibiricum powder must meet the relevant requirements of the national food safety standards and the 2025 edition of the Chinese Pharmacopoeia.

[0049] 7. Nitrogen-filled packaging: Food-grade aluminum foil composite bags with a PET / AL / PE structure are used as inner packaging. This packaging has excellent oxygen barrier, moisture-proof, and light-proof properties, and can effectively block the entry of external air, moisture, and light.

[0050] Using an automatic packaging machine equipped with nitrogen gas replacement function, the Polygonatum powder is packaged into bags according to specifications. The air inside the bags is then extracted, and high-purity nitrogen (purity ≥99.9%) is introduced, with a nitrogen replacement rate ≥99%. Subsequently, heat sealing is performed at a temperature of 150-170℃, a heat sealing time of 2-3 seconds, and a heat sealing pressure of 0.2-0.3MPa to ensure a tight heat seal without any air or powder leakage.

[0051] For the 25kg large packaging, cardboard drums are used as the outer packaging, with PE bags lined inside to prevent deformation from stacking. Small packaging can be designed according to market demand, and all use nitrogen-filled packaging to further prevent the Polygonatum powder from oxidizing, absorbing moisture and clumping.

[0052] 8. Storage: Store the packaged Polygonatum powder in a cool, dry and well-ventilated warehouse with a temperature of ≤25℃ and a relative humidity of ≤60%. The warehouse should be protected from light, moisture, insects and rodents, and should avoid direct sunlight and humid environments.

[0053] The first-in, first-out principle is adopted during storage, the stacking height does not exceed 5 layers, and the product status is checked every 3 months to ensure that the Polygonatum powder maintains excellent quality during the 18-24 month storage period.

[0054] 9. Repairing Clumping: If the Polygonatum powder clumps during storage, the following methods can be used to repair it: Mechanically break up the clumped Polygonatum powder, pass it through an 80-100 mesh sieve, and gently crush it to remove large clumps; Place the treated Polygonatum powder in a low-temperature drying device at 50-55℃ and dry it for 2-4 hours to further remove free moisture; After cooling to room temperature, re-crush and sieve it, add 0.3% silica and mix evenly, then re-dry and repackage it to restore the flowability and quality of the Polygonatum powder.

[0055] II. Process Route 2: Preparation Process of Lyophilized Polygonatum Powder with Premixed Excipients

[0056] This process reduces the hygroscopicity of Polygonatum powder from the source by adding functional excipients before drying, combined with vacuum freeze-drying technology, resulting in better anti-caking effects. The specific steps are as follows:

[0057] 1. Raw material pretreatment: Select mature and high-quality Polygonatum tubers, and pretreat them by washing, steaming and removing impurities to produce nine-times-processed Polygonatum granules for later use.

[0058] 2. Quantitative mixing: Weigh out the Polygonatum granules and functional anti-caking excipients according to the specified ratio. The functional anti-caking excipients are Poria cocos powder or maltodextrin, and the amount added is 10%-20% of the mass of Polygonatum granules. Put both into a mixer and mix at a speed of 20-30 r / min for 15-20 min to ensure uniform mixing.

[0059] 3. Vacuum freeze-drying: Place the uniformly mixed material into a vacuum freeze dryer, pre-freeze to below -40℃, keep at this temperature for 2 hours, then sublimate and dry under a vacuum of ≤10Pa for 24 hours, and finally desorb and dry until the moisture content of the material is ≤3%. Vacuum freeze-drying can retain the effective components of Polygonatum to the greatest extent, while making the material form a porous and loose structure, reducing the adhesion between powder particles.

[0060] 4. Low-temperature cell wall breaking ultrafine pulverization: In a constant temperature clean room, a low-temperature ultrafine pulverizer with a built-in cooling system is used to pulverize the dried material. The pulverizer speed is 15000-20000r / min, the feeding speed is 5-10kg / h, the material tank temperature is controlled at -15 to -10℃ during the pulverization process, and the pulverization time is 8min to obtain uniformly sized Polygonatum odoratum powder.

[0061] 5. Sieving and sieving: Pass the crushed Polygonatum powder through a 100-mesh sieve to remove large particles and ensure uniform particle size.

[0062] 6. The cobalt-60 irradiation sterilization dose is 5 kGy, and the microbiological indicators after sterilization meet the national standards.

[0063] 7. Nitrogen-filled packaging: Food-grade aluminum foil composite bags with an aluminum-coated PET / AL / PE structure (aluminum foil layer thickness ≥7μm) are used as inner packaging. An automatic packaging machine with nitrogen filling and replacement function is used to extract the air from the bag and fill it with high-purity nitrogen (purity ≥99.9%), achieving a nitrogen replacement rate ≥99%, followed by a tight heat seal. 25kg sizes are packaged in cardboard drums lined with PE bags to prevent deformation from stacking.

[0064] 8. Storage: Store the packaged Polygonatum powder in a cool, dark warehouse under the same conditions as in process route one.

[0065] Example 1: Preferred Example of Process Route

[0066] (1) Raw material selection: Select high-quality Polygonatum tubers that are free from rot, pests and diseases and mechanical damage, and manually remove surface impurities, soil and rotten parts for later use.

[0067] (2) Cleaning and slicing: Place the selected Polygonatum rhizome into a soaking tank, add water and soak for 15 minutes to soften the surface soil; then transfer it to a high-pressure spray cleaning machine and rinse with 0.4MPa high-pressure water flow to remove surface mud and impurities, and drain the water; put the drained Polygonatum rhizome into a slicer and cut it into uniform thin slices with a thickness of 4mm.

[0068] (3) Cooking and drying: Place the slices of Polygonatum into a steamer and steam for 45 minutes using a steam boiler to provide saturated steam. After steaming, transfer them to a heat pump drying room and control the drying temperature at 50°C. Continue drying until the moisture content of the slices of Polygonatum is 4.5%, and then crush them into Polygonatum granules of about 10 mesh.

[0069] (4) Low-temperature cell wall breaking ultrafine grinding: In a clean workshop with a constant temperature of 22℃ and a relative humidity of 40%, a low-temperature ultrafine grinding machine with its own cooling system is used. The grinding machine speed is controlled at 18000r / min, the feeding speed is 7kg / h, the material tank temperature is -15 to -10℃, the material temperature is 18℃, and after grinding, it is passed through a 100-mesh sieve to obtain uniformly sized Polygonatum powder.

[0070] (5) Anti-caking treatment: Add 0.3% food-grade 15% maltodextrin to the polygonatum powder and mix for 12 minutes using a mixer to ensure uniform mixing.

[0071] (6) Low temperature sterilization: Cobalt-60 irradiation sterilization is used with an irradiation dose of 7kGy. After sterilization, the total number of colonies is ≤100cfu / g and the number of molds and yeasts is ≤10cfu / g, which meets the national standard.

[0072] (7) Nitrogen-filled packaging: PET / AL / PE structure aluminum foil composite bags are used as inner packaging. The air inside the bag is extracted by an automatic packaging machine with nitrogen filling and replacement function, and nitrogen with a purity of 99.9% is filled in. The nitrogen replacement rate is 99.2%, the heat sealing temperature is 160℃, the heat sealing time is 2.5s, and the heat sealing is tight. The outer packaging is a carton, with 10 bags per carton and 500g per bag.

[0073] (8) Storage: Place the packaged Polygonatum powder in a cool, dry and ventilated warehouse with a temperature of 20°C and a relative humidity of 55%, and store it according to the first-in, first-out principle.

[0074] The Polygonatum powder prepared in this embodiment has good flowability, an angle of repose of 32°, and no clumping. After 24 months of storage, there is still no obvious clumping, the color is uniform, and there is no discoloration or off-flavor. The Polygonatum polysaccharide content retention rate is 91.2%, and the microbiological indicators meet the relevant requirements of GB2760-2024 and the 2025 edition of the Chinese Pharmacopoeia.

[0075] Example 2: Process Route - Nine Steaming and Nine Sun-drying Example

[0076] (1) Raw material selection: Select high-quality Polygonatum tubers that are free from rot and pests, remove impurities and rotten parts manually, and set aside.

[0077] (2) Cleaning and slicing: Put the Solomon's seal tuber into the soaking tank and soak for 10 minutes. Then transfer it to a high-pressure spray cleaning machine to remove surface mud and impurities and drain the water. Put it into a slicer and cut it into uniform thin slices with a thickness of 3 mm.

[0078] (3) Curing and drying: The “nine steaming and nine drying” process is adopted. Each steaming uses 0.1MPa saturated steam for 30 minutes. Each drying is carried out in a clean and ventilated drying area with a temperature of 28℃ and a relative humidity of 55% until the moisture content of the Polygonatum slices is 11%. The steaming and drying steps are repeated nine times in total. The last drying is carried out until the moisture content of the Polygonatum slices is 5%, and then crushed into Polygonatum granules of about 10 mesh.

[0079] (4) Low-temperature cell wall breaking ultra-fine pulverization: In a clean workshop with a constant temperature of 22℃ and a relative humidity of 42%, a low-temperature ultra-fine pulverizer is used, with a rotation speed of 16000r / min, a feeding speed of 6kg / h, and a material tank temperature of -15 to -10℃. After pulverization, the material passes through a 100-mesh sieve.

[0080] (5) Anti-caking treatment: Add 20% Poria cocos to Polygonatum powder and mix for 10 minutes to ensure even mixing.

[0081] (6) Low temperature sterilization: Cobalt-60 irradiation sterilization is used, with an irradiation dose of 5 kGy. After sterilization, the microbial indicators meet the national standards.

[0082] (7) Nitrogen-filled packaging: PET / AL / PE structure aluminum foil composite bags are used as inner packaging, filled with nitrogen gas with a purity of 99.9%, nitrogen replacement rate of 99.1%, and heat-sealed tightly; 25kg specifications are packaged in cardboard drums lined with PE bags.

[0083] (8) Storage: Store Polygonatum powder in a warehouse at a temperature of 22°C and a relative humidity of 58%.

[0084] The Polygonatum powder prepared in this embodiment showed no clumping after 18 months of storage, indicating excellent quality. The retention rate of Polygonatum saponins was 88.7%, which meets relevant standards.

[0085] Example 3: Process Route 1 - Vacuum Drying Example

[0086] (1) Raw material selection: Select Polygonatum tubers that are free from disease, pests and rot, remove impurities, and set aside.

[0087] (2) Cleaning and slicing: Soak the Polygonatum tuber for 20 minutes, rinse with high pressure spray, drain and cut into 5mm thick slices.

[0088] (3) Cooking and drying: After steaming for 60 minutes, transfer to a vacuum dryer, control the drying temperature at 45℃, dry until the moisture content of the Polygonatum slices is 4%, and pulverize into Polygonatum granules of about 10 mesh.

[0089] (4) Low-temperature cell wall breaking ultrafine grinding: In a clean workshop with a constant temperature of 22℃ and a relative humidity of 44%, low-temperature ultrafine grinding is carried out, with a rotation speed of 19000r / min, a feeding speed of 8kg / h, and a material temperature of 19℃. After grinding, the material is passed through a 100-mesh sieve.

[0090] (5) Anti-caking treatment: Add 0.5% tricalcium phosphate, mix for 15 minutes, and mix evenly.

[0091] (6) Low temperature sterilization: Cobalt-60 irradiation sterilization, irradiation dose 10kGy, sterilization qualified.

[0092] (7) Nitrogen-filled packaging: inner packaging is aluminum foil composite bag, nitrogen-filled and heat-sealed, and outer packaging is paper drum.

[0093] (8) Storage: Store in a warehouse at a temperature of 25°C and a relative humidity of 60%.

[0094] The Polygonatum powder prepared in this embodiment showed no clumping after 20 months of storage, exhibited stable quality, and retained 89.5% of the Polygonatum polysaccharide content.

[0095] Example 4: Process Route 1 - Lower Limit of Drying Temperature Example

[0096] The only difference between this embodiment and embodiment 1 is that the drying temperature in step (3) is 40°C, and the drying is carried out until the moisture content of the Polygonatum slices is 4.8%.

[0097] The Polygonatum powder prepared in this embodiment showed no obvious clumping after 24 months of storage, the Polygonatum polysaccharide content retention rate was 92.1%, and the microbial indicators were qualified.

[0098] Example 5: Process Route 1 - Upper Limit of Drying Temperature Example

[0099] The only difference between this embodiment and embodiment 1 is that the drying temperature in step (3) is 65°C, and the drying is carried out until the moisture content of the Polygonatum slices is 4.2%.

[0100] The Polygonatum powder prepared in this embodiment showed no obvious clumping after 24 months of storage, the Polygonatum polysaccharide content retention rate was 88.3%, and the microbial indicators were qualified.

[0101] Example 6: Process Route 1 - Lower Limit Example of Chemical Anti-caking Agent

[0102] The only difference between this embodiment and Embodiment 1 is that the amount of silicon dioxide added in step (5) is 0.2%.

[0103] The Polygonatum powder prepared in this embodiment showed no obvious clumping after 22 months of storage, the Polygonatum polysaccharide content retention rate was 90.8%, and the microbial indicators were qualified.

[0104] Example 7: Upper Limit of Chemical Anti-caking Agent in Process Route 1

[0105] The only difference between this embodiment and Embodiment 1 is that the amount of silicon dioxide added in step (5) is 0.5%.

[0106] The Polygonatum powder prepared in this embodiment showed no clumping after 24 months of storage, exhibited excellent flowability, retained 90.5% of the Polygonatum polysaccharide content, and met the microbial indicators.

[0107] Example 8: Process Route 1 - Lower Limit Example of Natural Anti-caking Agent

[0108] The only difference between this embodiment and embodiment 1 is that 3% of wood ear powder is added in step (5) to replace silicon dioxide.

[0109] The Polygonatum powder prepared in this embodiment showed no clumping after 18 months of storage, had a natural flavor, retained 89.1% of the Polygonatum polysaccharide content, and met the microbial indicators.

[0110] Example 9: Example of the upper limit of natural anti-caking agents in process route one

[0111] The only difference between this embodiment and embodiment 1 is that 5% of Poria cocos powder is added in step (5) to replace silicon dioxide.

[0112] The Polygonatum powder prepared in this embodiment showed no clumping after 20 months of storage, the Polygonatum polysaccharide content retention rate was 88.6%, and the microbial indicators were qualified.

[0113] Example 10: Process Route 1 - Cementation Repair Example

[0114] Take 1 kg of Polygonatum odoratum powder that has slightly caking after 24 months of storage in Example 1, and process it as follows: break up the caking Polygonatum odoratum powder mechanically, pass it through a 100-mesh sieve, and remove large lumps by light crushing; put the processed Polygonatum odoratum powder into a low-temperature drying device at 52°C and dry it for 3 hours; after cooling to room temperature, crush it again and pass it through a 100-mesh sieve, add 0.3% silica and mix evenly, and repackage it with nitrogen.

[0115] After processing, the flowability of Polygonatum powder returned to its initial state, with an angle of repose of 33°. The pass rate through a 100-mesh sieve was 98.5%, and the polysaccharide content retention rate was 89.7%. After repackaging and storage for 12 months, there was no re-caking phenomenon.

[0116] Example 11: Process Route Two - Low-Dose Poria Cocos Example

[0117] (1) Raw material pretreatment: Select mature and high-quality Polygonatum tubers, and pretreat them by washing, steaming and removing impurities to make nine-times processed Polygonatum granules for later use.

[0118] (2) Quantitative mixing: Weigh 500g of Polygonatum granules, add 50g of Poria cocos powder (10% by mass), put them into a mixer, and mix at a speed of 25r / min for 18min to ensure uniform mixing.

[0119] (3) Vacuum freeze drying: The uniformly mixed material is placed in a vacuum freeze dryer, pre-frozen to -45℃, kept warm for 2 hours, and then sublimated and dried under a vacuum of 8 Pa for 24 hours. The material is then desorbed and dried until the moisture content is 2.8%.

[0120] (4) Low-temperature cell wall breaking ultrafine grinding: In a clean workshop with a constant temperature of 22℃ and a relative humidity of 40%, a low-temperature ultrafine grinding machine is used, with a rotation speed of 18000r / min, a feeding speed of 7kg / h, a material tank temperature of -15 to -10℃, and a grinding time of 8min to obtain uniformly sized Polygonatum powder.

[0121] (5) Screening the powder: Pass the crushed Polygonatum powder through a 100-mesh sieve to remove coarse particles.

[0122] (6) Nitrogen-filled packaging: Aluminum-coated PET / AL / PE aluminum foil composite bags (aluminum foil layer thickness 7μm) are used as inner packaging, filled with nitrogen gas with a purity of 99.9%, nitrogen replacement rate of 99.3%, and heat-sealed tightly.

[0123] (7) Storage: Store in a cool, dark warehouse.

[0124] The Polygonatum powder prepared in this embodiment has a uniform and loose texture, good particle dispersibility, an angle of repose of 30°, and no moisture absorption or clumping after 24 months of sealed storage at room temperature. The content retention rate of Polygonatum polysaccharides is 87.9%.

[0125] Example 12: High-dose Poria cocos example using process route two

[0126] The only difference between this embodiment and embodiment 11 is that the amount of Poria cocos powder added in step (2) is 100g (20% by mass).

[0127] The Polygonatum powder prepared in this embodiment has excellent flowability, an angle of repose of 28°, and further improved moisture resistance. It has a loose texture and no clumping or hardening problems during long-term storage. After 24 months of storage, the Polygonatum polysaccharide content retention rate is 86.5%.

[0128] Example 13: Low-dose maltodextrin example from process route two

[0129] The only difference between this embodiment and embodiment 11 is that 50g of maltodextrin (10% by mass) is added in step (2) to replace the Poria cocos powder.

[0130] The Polygonatum powder prepared in this embodiment is fine and dry, with a repose angle of 31°. It does not clump after 24 months of sealed storage, and the Polygonatum polysaccharide content retention rate is 88.2%.

[0131] Example 14: High-dose maltodextrin example from process route two

[0132] The only difference between this embodiment and embodiment 11 is that 100g of maltodextrin (20% by mass) is added in step (2) to replace the Poria cocos powder.

[0133] The Polygonatum powder prepared in this embodiment has the best anti-caking and storage resistance. The powder remains loose for a long time and shows no caking or hardening after 24 months of storage. The Polygonatum polysaccharide content retention rate is 87.1%.

[0134] Comparative Example 1: Pure Polygonatum odoratum powder (without anti-caking agent, process route 1)

[0135] The only difference between this comparative example and Example 1 is that no anti-caking agent is added in step (5).

[0136] The pure Polygonatum powder prepared in this comparative example showed obvious clumping 12 hours after being pulverized, discoloration and off-taste after 3 months, and severe hardening after 6 months of storage, rendering it unusable. The Polygonatum polysaccharide content retention rate was only 64.8%.

[0137] Comparative Example 2: Pure Polygonatum Powder (no excipients, process route two)

[0138] The only difference between this comparative example and Example 11 is that no functional excipients are added in step (2).

[0139] The pure Polygonatum powder prepared in this comparative example has a large specific surface area and strong hygroscopicity after ultrafine grinding. After one month of sealed storage at room temperature, the particles agglomerate and harden, and after three months, severe caking occurs, indicating a short storage period.

[0140] The present invention provides a Polygonatum sibiricum powder that is resistant to clumping and easy to store. The specific effects are verified as follows:

[0141] (1) Anti-caking effect test: The flowability of the powder was tested by the angle of repose method. The smaller the angle of repose, the better the flowability and the stronger the anti-caking ability. At the same time, the agglomeration situation at different storage times was observed. The results showed that the angle of repose of the Polygonatum powder prepared in Examples 1-14 of this invention was ≤33°, the flowability was good, and there was no obvious agglomeration phenomenon after 18-24 months of storage; while the angle of repose of the Polygonatum powder in Comparative Examples 1-2 was >45°, the flowability was poor, and serious agglomeration occurred after short-term storage.

[0142] (2) Detection of effective component retention rate: The content of Polygonatum polysaccharide was detected by phenol-sulfuric acid method. The results showed that the Polygonatum powder prepared in the embodiments of the present invention had a Polygonatum polysaccharide retention rate of ≥86.5% and a Polygonatum saponin retention rate of ≥88%, and the effective components were well retained; while the Polygonatum powder in the comparative example had an effective component retention rate of only 60%-70% due to oxidation and degradation.

[0143] (3) Microbial index detection: The total number of colonies, molds and yeasts, coliforms and other microbial indicators were detected according to the GB4789 series standards. The results showed that the microbial indicators of the Polygonatum powder prepared in the embodiments of the present invention all met the relevant requirements of GB 2760-2024 and the 2025 edition of the Chinese Pharmacopoeia, and no microbial exceedances were observed after 24 months of storage.

[0144] It should be noted that, in this invention, although the specification describes the embodiments, not every embodiment contains only one independent technical solution. This way of describing the specification is only for clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A type of Polygonatum sibiricum powder that is resistant to clumping and easy to store, characterized in that, The moisture content of the Polygonatum powder is ≤5%, and it contains anti-caking components; The Polygonatum powder is packaged in nitrogen-filled packaging, and the packaging material is a composite packaging material that is oxygen-barrier, moisture-proof, and light-proof.

2. The Polygonatum sibiricum powder with anti-caking and easy storage according to claim 1, characterized in that, The anti-caking component is a food-grade anti-caking agent, and the amount added is 0.2%-0.5% of the mass of the pulverized Polygonatum powder; Alternatively, the anti-caking component may be a functional excipient (Poria cocos / maltodextrin), and the amount added is 10%-20% of the mass of the Polygonatum odoratum raw material before maturation.

3. The anti-caking and easily stored Polygonatum powder according to claim 1, characterized in that, The content retention rate of Polygonatum polysaccharides in the Polygonatum powder is ≥86%, and the content retention rate of Polygonatum saponins is ≥88%.

4. A preparation process for anti-caking and easily stored Polygonatum sibiricum powder, comprising the steps of raw material pretreatment, ripening and drying, pulverization, sterilization, and packaging, characterized in that, It also includes an anti-caking treatment step; Among them, the moisture content of the material after aging and drying is ≤5%; The pulverization is a low-temperature pulverization, which is carried out in an environment where the material tank temperature of the low-temperature pulverizer is -15 to -10℃; The sterilization process employs cobalt-60 irradiation. The packaging is nitrogen-filled, using composite packaging materials that are oxygen-barrier, moisture-proof, and light-proof, with a nitrogen replacement rate of ≥99%.

5. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, The anti-caking treatment involves adding Poria cocos or a food-grade anti-caking agent to the premixed Polygonatum granules before low-temperature pulverization and mixing them evenly. The food-grade anti-caking agent is selected from one or more of silicon dioxide, tricalcium phosphate, sodium aluminosilicate, microcrystalline cellulose, and maltodextrin.

6. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, The anti-caking treatment involves mixing the Polygonatum sibiricum raw material with functional excipients evenly before vacuum freeze-drying, before aging and drying. The functional excipients are Poria cocos powder or maltodextrin.

7. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, The aging and drying process includes a steaming step, followed by low-temperature freeze-drying until the moisture content is ≤5%. The low-temperature drying method is selected from one of the following: heat pump drying, vacuum freeze drying, and microwave drying.

8. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, The low-temperature pulverization uses a low-temperature ultrafine pulverizer with a built-in cooling system. The material tank temperature is -15 to -10℃, the pulverizer speed is 15000-20000r / min, and the feeding speed is 5-10kg / h.

9. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, The irradiation dose for cobalt-60 irradiation sterilization is 5-10 kGy.

10. The preparation process of the anti-caking and easily stored Polygonatum sibiricum powder according to claim 4, characterized in that, It also includes the repair steps for caking Polygonatum sibiricum powder: after mechanically breaking up and sieving the caking Polygonatum sibiricum powder, it is dried at a low temperature of 50-55℃, and then anti-caking components are added, mixed evenly, and repackaged with nitrogen.

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