Two-stage granulation solid direct drinking composition and preparation method thereof

Abstract

The invention discloses a two-stage granulation solid direct drinking composition and a preparation method thereof, and belongs to the technical field of functional food and nutritional health products. The composition is prepared from the following raw materials in parts by weight: 50 to 250 parts of chitosan oligosaccharide, 20 to 100 parts of sodium hyaluronate, 20 to 100 parts of non-denatured II type collagen, 5 to 50 parts of sugarcane polyphenol, 5 to 50 parts of folium cortex eucommiae extract, 5 to 50 parts of curcumin, 10 to 100 parts of galactooligosaccharide, 100 to 500 parts of inulin, 10 to 50 parts of citric acid and 800 to 1500 parts of erythritol. The preparation method comprises the following steps: (1) weighing raw materials; (2) pretreatment and premixing; (3) dry granulation; (4) wet granulation and drying; and (5) total mixing and filling. According to the invention, an innovative'dry process + wet process' two-stage granulation process is adopted, and a specific functional component formula is combined, so that a solid ready-to-drink joint maintenance product which is instantly dissolved in the mouth, is efficiently absorbed and is convenient to take is realized, and the solid ready-to-drink joint maintenance product is particularly suitable for middle-aged and elderly people, sports people and other groups with high requirements on joint health.

Description

Technical Field

[0001] This invention relates to the field of functional foods and nutritional health products, and more specifically to a two-stage granulation solid direct drinking composition and its preparation method. Background Technology

[0002] Osteoarthritis is a general term for diseases characterized by joint pain and limited mobility. It encompasses degenerative, inflammatory, and metabolic disorders, including osteoarthritis, rheumatoid arthritis, gouty arthritis, and ankylosing spondylitis. In recent years, osteoarthritis has become a major public health issue affecting the health of the entire population, especially against the backdrop of an aging population, where the number of osteoarthritis patients continues to rise.

[0003] Currently, mainstream bone and joint health products on the market mainly contain glucosamine, chondroitin sulfate, and calcium, and are primarily available in tablet and hard capsule forms. However, most of them suffer from the following prominent problems:

[0004] 1. Inconvenience of taking: Middle-aged and elderly people generally have difficulty swallowing, and tablets / capsules are prone to causing choking or discomfort; 2. Low absorption efficiency: Industrial heat processing can easily destroy active ingredients (such as collagen and plant extracts), and they need to be digested in the gastrointestinal tract before they can be absorbed; 3. Slow onset of action: Traditional dosage forms disintegrate slowly, resulting in low local nutrient concentrations, making it difficult to achieve rapid relief of inflammation and joint lubrication. 4. Severe homogenization of ingredients: Approximately 80% of products use the basic formula of "glucosamine + chondroitin + calcium", lacking differentiation and high-end innovation; 5. Lack of ready-to-eat design: Most products require water to take, which cannot meet the needs of modern life scenarios where "replenishment is needed anytime and anywhere".

[0005] Although some emerging ingredients, such as non-denatured type II collagen (UC-II, also known as "cartilage powder containing type II collagen"), MSM, and plant anti-inflammatory extracts, have been proven to have better joint protection effects, they have not yet been widely used in mainstream products due to their poor stability, unpleasant taste, or difficulty in processing.

[0006] In summary, existing bone and joint health products have significant shortcomings in dosage form design, processing technology, absorption pathway, and user experience, making it difficult to meet consumers' comprehensive demands for "high efficiency, safety, convenience, and comfort".

[0007] Therefore, developing a novel solid-state direct drinking product that requires no water delivery, dissolves instantly in the mouth, retains high activity, and has high bioavailability for the maintenance and improvement of bone and joint health is a problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0008] In view of this, the purpose of the present invention is to provide a two-stage granulation solid direct drinking composition and its preparation method, so as to overcome the shortcomings of the prior art.

[0009] To achieve the above objectives, the present invention adopts the following technical solution: A two-stage granulation solid direct drinking composition comprises the following raw materials in parts by weight: 50-250 parts chitosan oligosaccharide, 20-100 parts sodium hyaluronate, 20-100 parts undenatured type II collagen, 5-50 parts sugarcane polyphenols, 5-50 parts Eucommia ulmoides leaf extract, 5-50 parts curcumin, 10-100 parts galactooligosaccharides, 100-500 parts inulin, 10-50 parts citric acid, and 800-1500 parts erythritol.

[0010] The preferred composition is: 125 parts chitosan oligosaccharide, 50 parts sodium hyaluronate, 40 parts non-denatured type II collagen, 10 parts sugarcane polyphenols, 10 parts Eucommia ulmoides leaf extract, 10 parts curcumin, 30 parts galactooligosaccharide, 300 parts inulin, 40 parts citric acid, and 1385 parts erythritol.

[0011] In this invention: Chitosan oligosaccharide has anti-inflammatory properties and supplements glucosamine.

[0012] Sodium hyaluronate replenishes synovial fluid in joints.

[0013] Non-denatured type II collagen, anti-inflammatory.

[0014] Sugarcane polyphenols have anti-inflammatory and antioxidant properties.

[0015] Eucommia ulmoides leaf extract, which nourishes the kidneys and strengthens bones.

[0016] Curcumin, anti-inflammatory.

[0017] Galacto-oligosaccharides regulate gut microbiota and induce anti-inflammatory receptors.

[0018] Inulin regulates gut microbiota and induces anti-inflammatory receptors.

[0019] Citric acid helps to adjust the sour taste.

[0020] Erythritol regulates sweetness and mouth-crushing speed.

[0021] A method for preparing a two-stage granulated solid direct drinking composition specifically includes the following steps: (1) Weigh the raw materials Weigh each raw material according to the above two-stage granulation solid direct drinking composition by weight; (2) Pretreatment and premixing Crush citric acid and erythritol separately and sieve them. Chitosan oligosaccharide, undenatured type II collagen, galactooligosaccharide and curcumin were mixed to obtain premix component 1; Sugarcane polyphenols, Eucommia ulmoides leaf extract and citric acid were mixed to obtain premix component 2; (3) Dry granulation Premixed component 1 is dry granulated and sized to obtain pre-granulated component 3; (4) Wet granulation and drying Erythritol, premixed component 2, sodium hyaluronate and inulin were wet granulated and dried to obtain pre-granulated component 4. (5) Total mixing and filling Feed the materials in the following order: “1 / 2 pre-granulated granule component 3 → 1 / 2 pre-granulated granule component 4 → 1 / 2 pre-granulated granule component 3 → 1 / 2 pre-granulated granule component 4”, mix, and fill to obtain a two-stage granulated solid direct drinking water composition.

[0022] Furthermore, in step (2) above, the sieve mesh size is 40 mesh.

[0023] Furthermore, in step (2) above, the mixing speed of premixed component 1 is 10 rpm and the time is 20 min.

[0024] Furthermore, in step (2) above, the premixed component 2 is mixed manually for 5-10 minutes.

[0025] Furthermore, in step (3) above, the equipment for dry granulation is a dry granulator, and the equipment parameters are set as follows: stirring speed: 40 rpm, conveying speed: 30 rpm, pressure roller spacing: 1.2 mm, hydraulic pressure: 5.0 MPa, pressure roller speed: 5 rpm, granulation speed: 120 rpm, and screen mesh: 16-22 mesh.

[0026] Furthermore, in step (4) above, the equipment for wet granulation is a high-level wet mixing granulator, and the equipment parameters are set as follows: dry mixing: stirring 80 r / min, shearing 700-900 r / min, time 2-4 min; wet mixing: adding binder, stirring 100 r / min, cutting 1400-1600 r / min, time 3-7 min; binder pressure: 0.45-0.55 MPa; wet granulation: 8×8 mm sieve.

[0027] Furthermore, in step (4) above, the drying equipment is a fluidized bed, and the equipment parameters are set as follows: air inlet temperature: 75-85℃, material final temperature: 65-75℃, moisture control: ≤1%; cooled to below 45℃, and granulated through a 1.2mm sieve.

[0028] Furthermore, in step (5) above, the mixing speed is 10 rpm and the time is 20 min.

[0029] The advantages of this invention are as follows: I. The present invention has the following core advantages: 1. Achieves instant oral dissolution and immediate consumption, improving ease of use and patient compliance; 2. Through a two-stage granulation process, "active carrier particles" and "instant-dissolving inducing particles" are constructed respectively, achieving efficient release and dual absorption of functional ingredients; 3. The combined process of "low-temperature dry method + fluidized bed wet method" is adopted to maximize the protection of heat-sensitive active ingredients; 4. The formula incorporates a multi-target synergistic mechanism, covering functions such as anti-inflammation, repair, lubrication, and immune regulation; 5. Suitable for people of all ages, especially for middle-aged and elderly people, athletes, and high-risk groups such as those who sit or stand for long periods of time.

[0030] II. Core Technical Features: InstaSol™ Solid-State Direct Drinking Technology This invention innovatively proposes a "two-stage granulation, dual-phase synergy" technical approach, named InstaSol™ solid-state direct drinking technology, the principle of which is as follows: 1. Dry granulation for preparation of active carrier microparticles A Dry extrusion granulation is used to process functional heat-sensitive ingredients such as chitosan oligosaccharide, undenatured type II collagen, and curcumin into firm microparticles with low water activity and high activity retention. Process parameter control: pressure roller pressure 5.0MPa, rotation speed 5rpm, granulation screen 16-22 mesh; Advantages: Avoids high temperature and humidity environments, effectively protects the structural integrity of non-denatured type II collagen, and prevents collagen denaturation.

[0031] 2. Preparation of rapidly soluble inducing microparticles B by fluidized bed wet granulation Using soluble carriers such as erythritol, inulin, and citric acid, loose, rounded, and high specific surface area fast-dissolving particles are formed by fluidized bed spray granulation. Drying endpoint control: moisture content ≤1%, material endpoint temperature 65-75℃; Function: Upon entering the oral cavity, it rapidly absorbs water and disintegrates, inducing saliva secretion and initiating a "pre-dissolution" mechanism.

[0032] 3. Mixing and Filling Active carrier microparticles A and fast-dissolving inducing microparticles B are mixed in a certain proportion to ensure uniform distribution; A vacuum feeding system is used to connect to the strip bag filling machine to achieve dust-free, high-precision filling (filling volume 2000mg±3%).

[0033] III. Oral Absorption Mechanisms and Dual Absorption Pathways This invention breaks through the traditional "swallowing → intestinal absorption" model and proposes a dual pathway of "oral local absorption + intestinal synergistic absorption": 1. Oral instant dissolution stage Microparticle B dissolves rapidly and stimulates saliva production; Small molecule active substances (such as chitosan oligosaccharide and curcumin) can be directly absorbed into the bloodstream through the capillaries of the oral mucosa, achieving rapid onset of action; 2. Post-swallowing intestinal absorption stage Large molecular components (such as UC-II and sodium hyaluronate) flow into the gastrointestinal tract with food, and are promoted for intestinal adsorption and utilization by prebiotics such as inulin and galactooligosaccharides; Erythritol and citric acid regulate intestinal pH and enhance nutrient stability.

[0034] IV. Innovation Points and Patentability Analysis 1. It pioneered the "two-stage granulation + solid direct drinking" technology architecture, solving the problems of slow dissolution and poor absorption of traditional solid dosage forms; 2. A dual-mechanism synergistic model of "oral rapid dissolution induction + active carrier protection" is proposed to achieve efficient delivery of functional components; 3. For the first time, the formula combines UC-II, chitosan oligosaccharide, sodium hyaluronate, plant anti-inflammatory components, and a prebiotic system to form a multi-target synergistic network; 4. The entire process is controlled at low temperatures to avoid the deactivation of heat-sensitive components, which is significantly superior to traditional wet granulation or high-temperature drying processes; 5. It is suitable for automated continuous production and has good prospects for industrialization.

[0035] V. Application Prospects and Market Value This invention can be widely applied to: 1. Products for bone and joint health management for middle-aged and elderly people; 2. Sports nutrition supplements (for runners and fitness enthusiasts). 3. Joint protection for office workers who sit for long periods; 4. Joint support to reduce the burden on overweight individuals; 5. Nutritional support products for hospital rehabilitation departments.

[0036] The product comes in individual small packaging packets, making it easy to carry and consume. It aligns with the consumer trends of "precision nutrition" and "instant health" and has the potential to become a benchmark product for high-end joint care.

[0037] VI. Other Instructions 1. This invention has completed functional verification, pilot production, pilot scale-up, and mass production; 2. All raw materials used are food-grade or new food raw materials, which comply with relevant national regulations.

[0038] As can be seen from the above technical solution, compared with the prior art, the beneficial effects of the present invention are as follows: 1. Faster onset of action The local absorption pathway in the oral cavity shortens the time for active ingredients to reach peak concentration, and can relieve joint discomfort within 30 minutes; 2. Higher absorption rate The dual absorption mechanism enhances overall bioavailability, increasing it by more than 40% compared to traditional tablets; 3. More convenient to take Ready to eat right out of the bag, no water needed, suitable for various scenarios such as travel, office, and exercise; 4. Good safety It contains no added sucrose and uses erythritol as a sweetener, making it suitable for people with diabetes. 5. Stable and controllable process The two-stage granulation parameters are clearly defined, making it suitable for industrial-scale production. 6. Excellent taste By synergistically regulating the sweet and sour taste with erythritol, a pleasant experience with no unpleasant odor is achieved.

[0039] In summary, this invention employs an innovative two-stage granulation process combining dry and wet methods, along with a specific functional ingredient formula, to create a solid, ready-to-drink joint care product that is instantly soluble, highly absorbable, and convenient to consume. It is particularly suitable for middle-aged and elderly individuals, as well as athletes and other groups with high demands for joint health. Detailed Implementation

[0040] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0041] Example 1 The two-stage granulation solid direct drinking composition comprises the following raw materials by weight (2000mg per bag): chitosan oligosaccharide 125mg, sodium hyaluronate 50mg, non-denatured type II collagen 40mg, sugarcane polyphenols 10mg, eucommia leaf extract 10mg, curcumin 10mg, galactooligosaccharide 30mg, inulin 300mg, citric acid 40mg, and erythritol 1385mg; The preparation method of the above-mentioned two-stage granulation solid direct drinking composition specifically includes the following steps: (1) Weigh the raw materials Weigh each raw material according to the weight of the above two-stage granulation solid direct drinking composition; (2) Pretreatment and premixing Citrate and erythritol were separately pulverized and passed through a 40-mesh sieve; Take a 500L stainless steel mixing hopper, add chitosan oligosaccharide, undenatured type II collagen, galactooligosaccharide and curcumin, set the mixing speed to 10 rpm, mix for 20 min, and obtain premixed component 1; Add sugarcane polyphenols, Eucommia ulmoides leaf extract and citric acid to a transparent mixing bag and mix manually for 5-10 minutes to obtain premix component 2. (3) Dry granulation Premixed component 1 was fed into a dry granulator. The equipment parameters were set as follows: stirring speed: 40 rpm, conveying speed: 30 rpm, pressure roller spacing: 1.2 mm, hydraulic pressure: 5.0 MPa, pressure roller speed: 5 rpm, granulation speed: 120 rpm, and screen mesh: 16 mesh. Granulation was started after the machine was running stably. Premixed granules component 3 was obtained after granulation. (4) Wet granulation and drying Erythritol, premixed component 2, sodium hyaluronate, and inulin were fed into a high-level wet mixing granulator. The equipment parameters were set as follows: dry mixing: stirring 80 r / min, shearing 800 r / min, time 3 min; wet mixing: adding binder, stirring 100 r / min, cutting 1500 r / min, time 5 min; binder pressure: 0.45 MPa; wet granulation: 8×8 mm sieve; fluidized bed drying: inlet air temperature: 80℃, material final temperature: 65℃, moisture control: ≤1%; cooled to below 45℃, and granulated through a 1.2 mm sieve to obtain pre-formed granule component 4. (5) Total mixing and filling Take a 1000L mixing hopper and feed the materials in the following order: “1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4 → 1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4”. Mix at 10 rpm for 20 minutes. Vacuum feed the material to a 10-row strip bag filling machine with a set filling amount of 2000mg ± 3%. Take samples every 30 minutes to test the filling amount and airtightness (negative pressure 60-80KPa, 120s) to obtain the two-stage granulated solid direct drinking water composition.

[0042] Example 2 The two-stage granulation solid direct drinking composition comprises the following raw materials by weight (2000mg per bag): chitosan oligosaccharide 125mg, sodium hyaluronate 50mg, non-denatured type II collagen 40mg, sugarcane polyphenols 10mg, eucommia leaf extract 10mg, curcumin 10mg, galactooligosaccharide 30mg, inulin 300mg, citric acid 40mg, and erythritol 1385mg; The preparation method of the above-mentioned two-stage granulation solid direct drinking composition specifically includes the following steps: (1) Weigh the raw materials Weigh each raw material according to the weight of the above two-stage granulation solid direct drinking composition; (2) Pretreatment and premixing Citrate and erythritol were separately pulverized and passed through a 40-mesh sieve; Take a 500L stainless steel mixing hopper, add chitosan oligosaccharide, undenatured type II collagen, galactooligosaccharide and curcumin, set the mixing speed to 10 rpm, mix for 20 min, and obtain premixed component 1; Add sugarcane polyphenols, Eucommia ulmoides leaf extract and citric acid to a transparent mixing bag and mix manually for 5-10 minutes to obtain premix component 2. (3) Dry granulation Premixed component 1 was fed into a dry granulator. The equipment parameters were set as follows: stirring speed: 40 rpm, conveying speed: 30 rpm, pressure roller spacing: 1.2 mm, hydraulic pressure: 5.0 MPa, pressure roller speed: 5 rpm, granulation speed: 120 rpm, and screen mesh: 20 mesh. Granulation was started after the machine was running stably. Premixed granules component 3 was obtained after granulation. (4) Wet granulation and drying Erythritol, premixed component 2, sodium hyaluronate, and inulin were fed into a high-level wet mixing granulator. The equipment parameters were set as follows: dry mixing: stirring 80 r / min, shearing 900 r / min, time 2 min; wet mixing: adding binder, stirring 100 r / min, cutting 1600 r / min, time 3 min; binder pressure: 0.55 MPa; wet granulation: 8×8 mm sieve; fluidized bed drying: inlet air temperature: 75℃, material final temperature: 70℃, moisture control: ≤1%; cooled to below 45℃, and granulated through a 1.2 mm sieve to obtain pre-formed granule component 4. (5) Total mixing and filling Take a 1000L mixing hopper and feed the materials in the following order: “1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4 → 1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4”. Mix at 10 rpm for 20 minutes. Vacuum feed the material to a 10-row strip bag filling machine with a set filling amount of 2000mg ± 3%. Take samples every 30 minutes to test the filling amount and airtightness (negative pressure 60-80KPa, 120s) to obtain the two-stage granulated solid direct drinking water composition.

[0043] Example 3 The two-stage granulation solid direct drinking composition comprises the following raw materials by weight (2000mg per bag): chitosan oligosaccharide 125mg, sodium hyaluronate 50mg, non-denatured type II collagen 40mg, sugarcane polyphenols 10mg, eucommia leaf extract 10mg, curcumin 10mg, galactooligosaccharide 30mg, inulin 300mg, citric acid 40mg, and erythritol 1385mg; The preparation method of the above-mentioned two-stage granulation solid direct drinking composition specifically includes the following steps: (1) Weigh the raw materials Weigh each raw material according to the weight of the above two-stage granulation solid direct drinking composition; (2) Pretreatment and premixing Citrate and erythritol were separately pulverized and passed through a 40-mesh sieve; Take a 500L stainless steel mixing hopper, add chitosan oligosaccharide, undenatured type II collagen, galactooligosaccharide and curcumin, set the mixing speed to 10 rpm, mix for 20 min, and obtain premixed component 1; Add sugarcane polyphenols, Eucommia ulmoides leaf extract and citric acid to a transparent mixing bag and mix manually for 5-10 minutes to obtain premix component 2. (3) Dry granulation Premixed component 1 was fed into a dry granulator. The equipment parameters were set as follows: stirring speed: 40 rpm, conveying speed: 30 rpm, pressure roller spacing: 1.2 mm, hydraulic pressure: 5.0 MPa, pressure roller speed: 5 rpm, granulation speed: 120 rpm, and screen mesh: 22 mesh. Granulation was started after the machine was running stably. Premixed granules component 3 was obtained after granulation. (4) Wet granulation and drying Erythritol, premixed component 2, sodium hyaluronate, and inulin were fed into a high-level wet mixing granulator. The equipment parameters were set as follows: dry mixing: stirring 80 r / min, shearing 700 r / min, time 4 min; wet mixing: adding binder, stirring 100 r / min, cutting 1400 r / min, time 7 min; binder pressure: 0.5 MPa; wet granulation: 8×8 mm sieve; fluidized bed drying: inlet air temperature: 85℃, material final temperature: 75℃, moisture control: ≤1%; cooled to below 45℃, and granulated through a 1.2 mm sieve to obtain pre-formed granule component 4. (5) Total mixing and filling Take a 1000L mixing hopper and feed the materials in the following order: “1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4 → 1 / 2 pre-granulated component 3 → 1 / 2 pre-granulated component 4”. Mix at 10 rpm for 20 minutes. Vacuum feed the material to a 10-row strip bag filling machine with a set filling amount of 2000mg ± 3%. Take samples every 30 minutes to test the filling amount and airtightness (negative pressure 60-80KPa, 120s) to obtain the two-stage granulated solid direct drinking water composition.

[0044] Performance testing The two-stage granulated solid direct drinking composition prepared in Example 1 was used to test its dissolution time, moisture content, microbial limit, activity retention rate (UC-II), and taste score. Among these: 1. Dissolving time The testing method involves an oral simulated fluid test, and the specific steps are as follows: (1) Procedure: Pour the measured 37℃ simulated liquid into a transparent beaker; (2) Feeding: Sprinkle the weighed powder evenly on the liquid surface at once (simulating saliva contact after being sprinkled into the mouth). (3) Timing: Start the stopwatch at t=0; (4) Observation: Without any stirring, relying solely on the natural penetration and diffusion of the liquid; (5) Endpoint determination: The powder is observed to be completely wetted by the naked eye, with no floating dry powder, no bottom clumps, and completely dissolved / dispersed in the liquid; (6) Record: Record the total time (in seconds) from feeding to complete dissolution.

[0045] 2. Moisture content The test method is the Karl Fischer method, and the specific steps are as follows: (1) Standardization of Karl Fischer solution (determination of titer F) 1. Before testing a sample, the “water equivalent” of the Karl Fischer solution (i.e., how many milligrams of water are equivalent to each milliliter of the solution) must be determined.

[0046] 2. Add solvent: Add about 10-20 ml of anhydrous methanol to the titration cup.

[0047] 3. Pre-titration: Turn on the stirrer and titrate the solvent with Karl Fischer solution until the solution turns slightly brown (or the instrument indicates the endpoint) to consume any trace amounts of water remaining in the solvent.

[0048] 4. Add standard water sample: Using a microsyringe or by weighing, accurately add 10-30 mg of purified water (known weight, e.g., W_{water}).

[0049] 5. Titration: Continue titrating with Karl Fischer solution until the solution color changes from pale yellow to reddish brown (visual method) or the instrument ammeter pointer changes abruptly (perpetual stop titration method).

[0050] 6. Record volume: Record the volume of Karl Fischer solution consumed (A_{label}).

[0051] 7. Calculate the titer F: F = W_{water}}{A_{standard} - B}; where, F: titer (mg water / ml test solution), W_{water}: weight of pure water added (mg), A_{standard}: volume of test solution consumed in titrating water (ml), B: volume of test solution consumed in blank test (ml, usually very small and negligible, but a blank test is required for accurate determination).

[0052] (2) Sample determination (instant powder) 1. Solvent preparation: Add an appropriate amount of anhydrous methanol (or other solvent) to the titration vessel and start stirring.

[0053] 2. Pre-titration: As above, titrate to the endpoint with Karl Fischer solution to remove background moisture from the solvent.

[0054] 3. Weighing: Based on the estimated moisture content, weigh an appropriate amount of sample (usually between 1-10 mg of moisture, for example, about 0.1g-1g, accurate to 0.0001g).

[0055] 4. Note: Instant powders are usually hygroscopic, so they should be handled quickly.

[0056] 5. Sample injection: Quickly add the weighed sample into the solvent in the titration cup.

[0057] 6. Titration: After the sample dissolves, water is released. Continue titrating with Karl Fischer solution until the same endpoint (color or current change) is reproduced.

[0058] 7. Record volume: Record the total volume (A) of Karl Fischer solution consumed in the titration of the sample.

[0059] 3. Microbial limits The test method is based on the Chinese Pharmacopoeia, and the specific steps are as follows: (1) Preparation of test solution Solid / semi-solid samples: Take the specified amount of test sample, add 90 ml of diluent, and use a homogenizer or shake to disperse it evenly.

[0060] (2) Inspection of test samples (formal testing) A. Microbial count (total aerobic bacteria & total mold and yeast count) PourPlateMethod 1. Take 1 ml of the test solution of appropriate dilution and add it to a sterile Petri dish.

[0061] 2. Inject 15-20 ml of culture medium at a temperature of about 45℃ (use tryptic soy agar TSA for aerobic bacteria, and Sabouraud dextrose agar SDA for molds / yeasts).

[0062] 3. Mix well, let it solidify, and then invert it for incubation.

[0063] B. Control bacteria test (using Escherichia coli as an example) 1. Enrichment culture: Take the test solution equivalent to 1g / ml and inoculate it into tryptic soy peptone liquid medium (TSB), and incubate at 30-35℃ for 18-24h.

[0064] 2. Selective enrichment: Take 1 ml of the above culture and inoculate it into MacConkey liquid medium, and incubate at 42-44℃ for 24-48 h.

[0065] 3. Isolation and culture: Streak inoculate onto MacConkey agar plates and incubate at 30-35℃ for 18-72 hours.

[0066] 4. Result interpretation: Observe whether there are typical colonies (e.g., Escherichia coli is usually a pink colony on MacConkey agar plates) and perform biochemical identification for confirmation.

[0067] (3) Cultivation and Counting 1. Cultivation conditions: Total aerobic bacteria count: TSA medium, 30-35℃, incubate for 3-5 days.

[0068] Total mold and yeast count: SDA medium, 20-25℃, incubate for 5-7 days.

[0069] 2. Colony count: Select plates with colony counts between 30 and 300 for counting (plate method).

[0070] Units of measurement (e.g., cfu / g or cfu / ml).

[0071] 4. Activity retention rate (UC-II) The test method was HPLC-GPC to detect changes in the molecular weight of the triple helix structure. The specific steps are as follows:

[0072] (1) Establishing a standard curve (the basis for determining the molecular weight of an unknown sample) 1. Determination of standard products: Prepare a series of known standard solutions with different molecular weights (e.g., 1000 Da, 3000 Da, 5000 Da, etc.).

[0073] 2. Sample injection analysis: Each standard solution was injected into the HPLC system for separation.

[0074] 3. Record data: Record the elution volume (Ve) or retention time for each standard.

[0075] 4. Plot the curve: Plot the standard curve with the logarithm of the molecular weight of the standard (logMW) on the ordinate and the elution volume (Ve) on the abscissa (or perform linear regression to obtain the standard equation).

[0076] (2) Sample determination 1. Sample preparation: Dissolve the collagen peptide sample in the mobile phase or a suitable solvent to prepare a solution of a certain concentration (e.g., 1-5 mg / mL).

[0077] 2. Filtration: Use a 0.22µm or 0.45µm filter membrane to filter the sample solution to remove particulate impurities and avoid clogging the chromatographic column.

[0078] 3. Injection: Take an appropriate amount (e.g., 10-20 µL) of filtrate and inject it into the HPLC system.

[0079] 4. Chromatographic separation: Elution and separation are performed under the same chromatographic conditions as the standard.

[0080] (3) Data calculation 1. Obtain the elution volume: Read the elution volume (Ve) of the main peak of the sample from the chromatogram.

[0081] 2. Calculate molecular weight: Substitute the elution volume of the sample into the standard curve (or standard equation) established in the first step to calculate the number-average molecular weight (Mn) and weight-average molecular weight (Mw) of the sample.

[0082] 3. Analysis of distribution: Based on the width and shape of the chromatographic peaks, the molecular weight distribution of the sample can be analyzed (i.e., polydispersity index PDI = Mw / Mn).

[0083] 5. Taste rating The testing method was a sensory evaluation panel (n=30), and the specific steps were as follows: (1) Evaluation personnel selection and grouping (n=30) These 30 evaluators are typically divided into two categories: top-tier evaluators (who have received professional training) or consumer preference evaluators (who have not received professional training but represent the target audience). "Taste rating" usually refers to the latter.

[0084] 1. Recruitment Requirements: Non-smoker, no oral diseases, and has not taken antibiotics or hormone medications recently.

[0085] No special dietary preferences (unless testing a specific population) and no bias against the tested product.

[0086] Screening tests: Conduct basic taste recognition tests (identify sour, sweet, bitter, and salty) and odor recognition tests to eliminate those with dulled taste buds.

[0087] 2. Quantity Confirmation: A total of 30 evaluators were confirmed to participate in the test to ensure the reliability of the data (statistically, n=30 is the starting point for a large sample).

[0088] (2) Sample preparation and coding 1. Mixing ratio: Strictly follow the product's recommended mixing ratio (e.g., 1:100 or 1:200) to dissolve the powder in purified water to prepare the test solution.

[0089] 2. Temperature control: Adjust the sample to a suitable tasting temperature (usually room temperature 20-25℃, or the product's optimal drinking temperature).

[0090] 3. Random Coding: Use a 3-digit random number to code the samples (e.g., 345, 789, 102). Each evaluator should receive a different sample code to avoid order effects.

[0091] 4. Placement: Put about 10-20ml of sample into a disposable transparent tasting cup and cover it (to prevent the aroma from evaporating too early).

[0092] (3) Preparation before evaluation 1. No eating or smoking: Evaluators are required to refrain from smoking, drinking alcohol, chewing gum, or consuming spicy foods for 1-2 hours before the test.

[0093] 2. Rinse your mouth: Before the test, rinse your mouth thoroughly with warm water to remove any bad breath.

[0094] 3. Distribute questionnaires: Distribute a standardized sensory evaluation questionnaire (paper or electronic version) to each evaluator.

[0095] (4) Sensory evaluation process (specific scoring steps) The evaluators assessed the "taste" and related attributes in the following order: 1. Observation (visual): Observe the color, transparency, and presence of any precipitate or suspended matter in the solution.

[0096] Rating criteria: Appearance acceptability (e.g., presence or absence of cloudiness or layering).

[0097] 2. Smelling (sense of smell): Lift the lid, gently shake, and then smell the aroma.

[0098] Scoring criteria: Aroma characteristics, aroma intensity, presence or absence of off-odors.

[0099] 3. Tasting (Taste and Sensation - Core Step): Sipping: Use a clean spoon to take a small sample (about 5-10ml) and put it in your mouth.

[0100] Oral distribution: Spread the sample throughout the oral cavity, touching the tip, root, and sides of the tongue, and leave it for 5-10 seconds.

[0101] Swallow / Spit out: Swallow (eat it all) or spit out (swallow after rinsing your mouth) as required by the test.

[0102] Evaluation indicators: Flavor profile: sweet and sour, bitterness, umami, and aftertaste.

[0103] Texture / taste: smoothness, graininess (whether it feels gritty), viscosity, and refreshing feel.

[0104] Aftertaste: The lingering taste in the mouth after swallowing and its duration.

[0105] 4. Clean the oral cavity: After evaluating one sample, rinse your mouth with warm water or tasteless biscuits / apple slices, rest for 1-2 minutes, and then evaluate the next sample.

[0106] (5) Data collection and analysis 1. Scoring scale: The Hedonic Scale, a 5-point preference scale, is used. 2. Data Processing: We collected 30 questionnaires and removed those that were obviously filled out randomly.

[0107] Calculate the mean and standard deviation of each indicator.

[0108] Key criteria: If the average score is ≥3.5 (assuming 5 is the maximum score), the product's taste is generally considered acceptable; if it is ≥4.0, the taste is excellent.

[0109] The results are shown in Table 1.

[0110] Table 1 Performance test results of the two-stage granulated solid direct drinking composition in Example 1

[0111] As shown in Table 1, the process technology of this invention can maintain the activity of nutrients with low moisture and high activity, and can achieve rapid oral disintegration and a wide range of palatable taste preferences.

[0112] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A two-stage granulation solid-state direct drinking composition, characterized in that, The ingredients include the following parts by weight: 50-250 parts chitosan oligosaccharide, 20-100 parts sodium hyaluronate, 20-100 parts undenatured type II collagen, 5-50 parts sugarcane polyphenols, 5-50 parts Eucommia ulmoides leaf extract, 5-50 parts curcumin, 10-100 parts galactooligosaccharides, 100-500 parts inulin, 10-50 parts citric acid, and 800-1500 parts erythritol.

2. The two-stage granulation solid direct drinking composition according to claim 1, characterized in that, The ingredients include the following parts by weight: 125 parts chitosan oligosaccharide, 50 parts sodium hyaluronate, 40 parts non-denatured type II collagen, 10 parts sugarcane polyphenols, 10 parts Eucommia ulmoides leaf extract, 10 parts curcumin, 30 parts galactooligosaccharide, 300 parts inulin, 40 parts citric acid, and 1385 parts erythritol.

3. A method for preparing a two-stage granulation solid direct drinking composition, characterized in that, Specifically, the following steps are included: (1) Weigh the raw materials Weigh each raw material according to the weight proportions of the two-stage granulated solid direct drinking composition as described in claim 1 or 2; (2) Pretreatment and premixing Crush citric acid and erythritol separately and sieve them. Chitosan oligosaccharide, UC-II, galactooligosaccharide and curcumin were mixed to obtain premix component 1; Sugarcane polyphenols, Eucommia ulmoides leaf extract and citric acid were mixed to obtain premix component 2; (3) Dry granulation Premixed component 1 is dry granulated and sized to obtain pre-granulated component 3; (4) Wet granulation and drying Erythritol, premixed component 2, sodium hyaluronate and inulin were wet granulated and dried to obtain pre-granulated component 4. (5) Total mixing and filling The materials are added in the following order: "1 / 2 pre-granulated granule component 3 → 1 / 2 pre-granulated granule component 4 → 1 / 2 pre-granulated granule component 3 → 1 / 2 pre-granulated granule component 4", mixed, and filled to obtain the two-stage granulated solid direct drinking composition.

4. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (2), the sieve mesh number is 40.

5. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (2), the mixing speed of the premixed component 1 is 10 rpm and the mixing time is 20 min.

6. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (2), the premixed component 2 is mixed manually for 5-10 minutes.

7. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (3), the dry granulation equipment is a dry granulator with the following parameters: stirring speed: 40 rpm, conveying speed: 30 rpm, pressure roller spacing: 1.2 mm, hydraulic pressure: 5.0 MPa, pressure roller speed: 5 rpm, granulation speed: 120 rpm, and screen mesh: 16-22 mesh.

8. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (4), the wet granulation equipment is a high-level wet mixing granulator, and the equipment parameters are set as follows: dry mixing: stirring 80 r / min, shearing 700-900 r / min, time 2-4 min; wet mixing: adding binder, stirring 100 r / min, cutting 1400-1600 r / min, time 3-7 min; binder pressure: 0.45-0.55 MPa; wet granulation: 8×8 mm sieve.

9. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (4), the drying equipment is a fluidized bed, and the equipment parameters are set as follows: air inlet temperature: 75-85℃, material end temperature: 65-75℃, moisture control: ≤1%; cooled to below 45℃, and granulated through a 1.2mm sieve.

10. The method for preparing a two-stage granulation solid direct drinking composition according to claim 3, characterized in that, In step (5), the mixing speed is 10 rpm and the time is 20 min.

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