Formula and production process of collagen solid beverage

Abstract

The invention relates to the technical field of food processing, and discloses a collagen solid beverage formula and a production technology, and the solid beverage comprises the following components: cod collagen peptide; inulin; blood orange powder; acerola cherry powder; gamma-aminobutyric acid; skipjack elastin peptide; blueberry powder; sodium hyaluronate; the production process comprises the following steps: sieving the raw materials for later use; the preparation method comprises the following steps: firstly, mixing part of cod collagen peptide with total amount of gamma-aminobutyric acid, skipjack elastin peptide, blueberry powder, sodium hyaluronate and food essence to obtain a first-grade mixture, then uniformly mixing the first-grade mixture with the remaining cod collagen peptide, total amount of inulin, blood orange powder and acerola cherry powder, and finally, performing metal detection and nitrogen-filled packaging to obtain a finished product. Through a mixing process, the moisture absorption agglomeration risk of the high-hygroscopicity raw material is reduced, the problem of uneven mixing of trace active ingredients is solved, and the obtained product is quick to dissolve, good in dispersity and uniform in nutritional ingredient.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, specifically to a collagen solid beverage formula and production process. Background Technology

[0002] Collagen peptides are widely used in oral beauty and nutritional supplement solid beverages due to their excellent bioavailability. To improve absorption efficiency, current technologies often employ enzymatic hydrolysis to break down collagen into smaller peptide molecules. However, as the molecular weight decreases, the number of exposed hydrophilic groups such as amino and carboxyl groups in the peptide chain increases, leading to a significant increase in the hygroscopicity of the raw material. During production, processing, storage, and transportation, highly hygroscopic collagen peptides readily absorb moisture from the environment and deliquesce, causing adhesion and clumping between powder particles. This not only worsens the product's flowability and hinders automatic packaging machine feeding but also severely impacts the sensory quality of the finished product during its shelf life and its dissolution rate during reconstitution.

[0003] Furthermore, to achieve multi-dimensional nutritional supplementation, collagen solid beverage formulations often require the addition of multiple trace active ingredients such as elastin peptides, sodium hyaluronate, and γ-aminobutyric acid (GABA). Because these trace ingredients are added in extremely low proportions, and their physical properties, such as bulk density and particle size, differ significantly from the collagen peptides used as the main ingredient, segregation is highly likely to occur in conventional mixing processes. Especially for highly hygroscopic main ingredients, trace ingredients are prone to adhering to the inner walls of mixing equipment or dead corners of the stirring paddle due to electrostatic adsorption or moisture absorption, resulting in poor mixing uniformity and making it difficult to ensure the consistency of nutrient content in individual small packages. Existing solutions employ wet granulation or increase the amount of anti-caking agents to improve powder properties, but this introduces a high-temperature drying process that can damage heat-sensitive active ingredients or significantly reduce the purity of effective collagen in the product. Therefore, developing a solid beverage formulation and preparation process that can effectively overcome the problem of moisture absorption and clumping of small molecule peptides while ensuring high mixing uniformity of trace components is a pressing technical challenge in this field. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a collagen solid beverage formula and production process, which solves the problems of easy moisture absorption and clumping of highly hygroscopic peptide raw materials, low uniformity of mixing of trace active ingredients, and poor product solubility caused by macromolecular raw materials in existing collagen solid beverages.

[0005] To achieve the above objectives, the present invention provides the following technical solution: In a first aspect, the present invention provides a collagen solid beverage formulation, which adopts the following technical solution: A collagen solid beverage comprises the following components in parts by weight: 60-90 parts cod collagen peptide, 3-10 parts inulin, 2-8 parts blood orange powder, 2-7 parts acerola cherry powder, 1.5-6 parts γ-aminobutyric acid, 1-5 parts bonito elastin peptide, 1-4 parts blueberry powder, 0.2-3 parts sodium hyaluronate, and 0.1-2 parts food flavoring.

[0006] By employing the above technical solution, inulin is used as a dispersing carrier and compounded with high-content cod collagen peptides. The physical structure of inulin acts as a spatial barrier between powder particles, reducing the frequency of direct contact between highly hygroscopic peptide particles, thereby lowering the probability of powder agglomeration due to moisture absorption. Simultaneously, γ-aminobutyric acid, bonito elastin peptides, and various fruit powders are added synergistically to the formula. While ensuring the main efficacy of collagen peptides, elastin and non-protein active ingredients are supplemented, achieving a dual supplementation of collagen and elastin. Under specific proportions, the components can maintain the looseness of the powder in its natural stacking state, ensuring the product's reconstitution and dispersibility.

[0007] Preferably, the raw materials are in the following proportions by weight: 75-80 parts cod collagen peptide, 6-8 parts inulin, 4.5-6 parts blood orange powder, 4-5 parts acerola cherry powder, 3.75-5 parts γ-aminobutyric acid, 2.5-3.5 parts bonito elastin peptide, 2-3 parts blueberry powder, 1.5-2.5 parts sodium hyaluronate, and 0.88-1.5 parts food flavoring.

[0008] Preferably, the weight-average molecular weight (Mw) of the cod collagen peptides is distributed between 500 Da and 3000 Da, wherein the proportion of components with a molecular weight less than 1000 Da is ≥88.5%. The cod collagen peptides are prepared by the following method: frozen deep-sea cod skin is selected, and after soaking in 0.2 mol / L sodium hydroxide solution to remove fat and non-collagenous proteins, it is subjected to double-enzyme hydrolysis. The double-enzyme hydrolysis is carried out by first adding pepsin at pH 2.5 and 38°C for 1.5 hours, adjusting the pH to 8.5, and then adding alkaline protease for 4 hours at 55°C. The hydrolysate is subjected to enzyme inactivation, decolorization, ultrafiltration with a molecular weight cutoff of 3000 Da, and concentration filtration with a molecular weight cutoff of 300 Da to 500 Da, and finally spray drying to obtain the final product.

[0009] By employing the above technical solution, a stepwise enzymatic hydrolysis strategy using pepsin and alkaline protease is adopted. Pepsin, under acidic conditions, opens the triple helix structure of collagen and performs initial cleavage, exposing internal sites; alkaline protease, under high temperature and high pH conditions, performs deep enzymatic hydrolysis, further breaking down polypeptide chains into shorter peptides, thus improving the degree of hydrolysis of the raw material. Specifically, a dual membrane separation technology of ultrafiltration and nanofiltration is introduced: a 3000 Da ultrafiltration membrane effectively retains incompletely hydrolyzed large molecular fragments, ensuring product clarity and dissolution rate; a 300 Da to 500 Da nanofiltration membrane removes inorganic salts and highly hygroscopic free amino acids, enriching active peptides within the target molecular weight range while desalting and purifying, thereby reducing hygroscopicity while maintaining high bioactivity.

[0010] Preferably, the total content of desmokine and isodesmokine in the skipjack tuna elastin peptide is ≥1.3 mg / g; the skipjack tuna elastin peptide is prepared by the following method: take skipjack tuna heart aortic bulb tissue, defatt it, add 0.1 mol / L sodium hydroxide solution and heat it at 90℃ to 95℃ for 30 to 60 minutes, collect the precipitate and wash it with water until neutral; adjust the pH of the precipitate to 9.0, add alkaline protease and enzymatically hydrolyze it at 55℃ for 8 to 10 hours; the enzymatic hydrolysate is subjected to enzyme inactivation, centrifugation, microfiltration through a 0.2 μm ceramic membrane and ultrafiltration through a molecular weight cutoff of 5000 Da, collect the permeate and freeze-dry it to obtain the peptide.

[0011] By employing the above-mentioned technical solution, leveraging the alkali-resistant and heat-resistant physicochemical properties of elastin, a high-temperature alkali treatment step is introduced before enzymatic hydrolysis. This step uses a hot alkali solution to hydrolyze and dissolve collagen and other proteins in the raw material, which are then removed by centrifugation. Only the insoluble, high-purity elastin precipitate is retained as the enzymatic hydrolysis substrate, effectively removing impurities and significantly improving the purity of characteristic amino acids (desiketin and isodesiketin) in the final product. Subsequently, ceramic membrane microfiltration and 5000Da ultrafiltration membrane retention are combined to remove enzymatic hydrolysis residues and suspended solids while screening for active peptides with a molecular weight less than 5000Da, ensuring high solubility and bioavailability of skipjack tuna elastin peptides.

[0012] Preferably, the sodium hyaluronate is enzymatically cleaved low molecular weight sodium hyaluronate with a weight-average molecular weight (Mw) of 3000 Da-10000 Da. The sodium hyaluronate is prepared by the following method: high molecular weight sodium hyaluronate is prepared into an aqueous solution, hyaluronidase is added, and the enzymatic cleavage reaction is carried out at pH 6.0 and 37°C, while the solution viscosity is monitored in real time; when the weight-average molecular weight drops to the target range, the enzyme is inactivated by heating, followed by decolorization with activated carbon, and the filtrate is pumped into a membrane separation device with a molecular weight cutoff of 1000 Da to 2000 Da for tangential flow filtration. After constant volume water addition dialyzing and concentration, it is spray-dried to obtain the final product.

[0013] By employing the above technical solution and utilizing real-time viscosity monitoring technology to precisely control the enzymatic hydrolysis endpoint, the molecular weight of the product is ensured to be concentrated within the target range, avoiding over- or under-hydrolysis caused by reaction time deviations. Specifically, tangential flow filtration technology is introduced to replace the traditional ethanol precipitation method for purification. A filter membrane with a molecular weight cutoff of 1000-2000 Da effectively retains the target low molecular weight sodium hyaluronate, while dialysis removes inorganic salt ions and non-biologically active monosaccharide and disaccharide impurities from the system. This improves the purity of the raw materials, reduces ash content, eliminates the additional moisture absorption risk from free monosaccharides, and results in a powder that maintains high solubility while exhibiting better storage stability.

[0014] Secondly, the present invention provides a production process for a collagen solid beverage formulation, comprising the following steps: S1. In a clean environment with controlled temperature and humidity, remove the raw materials from their packaging and sieve them. S2. Using a graded feeding method, a portion of cod collagen peptides is mixed with the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate, and food flavoring to obtain a primary mixture. S3. Mix the remaining cod collagen peptides, the total amount of inulin, blood orange powder, and acerola cherry powder with the primary mixture until homogeneous. S4. After the uniformly mixed materials are tested for metals, they are packaged and heat-sealed under nitrogen protection.

[0015] By adopting the above technical solution, a two-step mixing process was used to solve the problem of uneven mixing of multi-component raw materials with large differences in density and particle size. The first-stage mixing pre-disperses trace active ingredients with part of the matrix to prepare a high-concentration intermediate mixture, allowing the trace components to initially adhere to the surface of the matrix particles. The second-stage mixing then dilutes and disperses the intermediate mixture into the remaining bulk raw materials. This step-by-step dispersion strategy effectively prevents the segregation and aggregation of trace components in the final product, reduces the coefficient of variation of component content, and ensures the consistency of nutritional composition in each bag of product.

[0016] Preferably, in step S1, the temperature of the clean environment is controlled at 18-25℃, and the relative humidity (RH) is controlled at 30%-40%; the raw material is sieved using a 10-20 mesh stainless steel sieve.

[0017] By adopting the above technical solution, the relative humidity of the production environment is strictly controlled to be below 40%. Because collagen peptides have extremely strong hygroscopic properties, the surface energy of the powder increases in a high-humidity environment, and liquid bridges easily form between particles through water adsorption, leading to agglomeration and reduced flowability. A low-humidity environment blocks the contact path between moisture and the powder, maintaining the dry and loose state of the raw materials and providing an environmental guarantee for subsequent uniform mixing.

[0018] Preferably, in step S2, the graded feeding method is as follows: first, 15-20 parts by weight of cod collagen peptides are added as the base material, followed by the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring, and finally, 15-20 parts by weight of cod collagen peptides are added on top; in step S2, the mixing is carried out using a pneumatic mixer with a compressed air pressure of 0.40-0.55 MPa, a pulse frequency of 0.3s / 0.3s to 0.5s / 0.5s, and a mixing time of 4-6 minutes.

[0019] By adopting the above technical solution and employing a layered feeding strategy, trace active ingredients are placed between the bottom and top layers of the matrix, avoiding direct contact between trace powders and the inner wall of the mixer or the dead corners of the mixing, and preventing material loss due to electrostatic adsorption or wall adhesion. The pneumatic mixer uses high-pressure pulsed airflow to fluidize the powder, overcoming the van der Waals forces between the powders. Under the action of the airflow, the active ingredients in the middle layer rapidly diffuse and penetrate to the upper and lower layers of the matrix. Each component undergoes forced convection and diffusion in three-dimensional space, achieving uniform distribution of trace components in the matrix.

[0020] Preferably, in step S3, the mixing equipment is a double-helix conical mixer or a paddle mixer, and the mixing time is 120-300 seconds. In step S4, the nitrogen purity is ≥99.5%, and the heat sealing conditions are: longitudinal sealing temperature 120℃-180℃, and transverse sealing temperature 140℃-190℃.

[0021] By employing the above technical solution, the secondary mixing utilizes the convection and shearing forces generated by a double helix or paddle to uniformly disperse the primary mixture into the bulk materials containing inulin and fruit powder. During this process, inulin further fills the spaces between collagen peptide particles, achieving a physical separation effect. The packaging step uses high-purity nitrogen replacement, reducing the oxygen content and moisture partial pressure inside the packaging bag, preventing oxidation, deterioration, and moisture absorption / caking of the product during its shelf life. Combined with a specific heat-sealing temperature, this ensures the packaging's airtightness.

[0022] This invention provides a collagen solid beverage formula and production process. It has the following beneficial effects: 1. This invention introduces a specific proportion of inulin as a dispersing carrier into the formula, utilizing its physical barrier effect to block highly hygroscopic cod collagen peptide particles, reducing direct contact points between particles, effectively lowering the risk of moisture absorption and agglomeration of the powder during storage, and significantly improving the product's flowability (angle of repose less than 35°) and anti-caking properties. At the same time, by compounding skipjack tuna elastin peptide, γ-aminobutyric acid and sodium hyaluronate, a multi-layered nutritional supplement system is constructed. While maintaining good reconstitution properties of the solid beverage, the efficacy of the product is enhanced through the synergistic effect of the various components.

[0023] 2. This invention strictly limits the molecular weight distribution of each core raw material through dual-enzyme hydrolysis and membrane separation technology. In particular, it increases the proportion of components with less than 1000 Da in cod collagen peptides to more than 88.5%, and combines it with enzymatic hydrolysis of low molecular weight sodium hyaluronate. This fundamentally eliminates the surface gel barrier layer that is easily formed by large molecular proteins and polysaccharides in the early stage of dissolution. This allows the powder to be quickly wetted and sank after being put into water, shortening the dissolution time to less than 30 seconds. Moreover, the reconstituted solution is clear and transparent, without any undissolved particles or flocculent precipitates visible to the naked eye, thus improving the sensory quality of the product.

[0024] 3. The environmental humidity control and two-step graded mixing process adopted in this invention solve the problem of the difficulty in uniformly dispersing trace active ingredients in a large amount of matrix. In particular, the feeding strategy of bottom pre-laying, middle sandwiching and top covering adopted in the primary mixing stage, combined with pneumatic pulse dispersion, avoids the loss of trace components due to wall adhesion and electrostatic aggregation. The test results show that the coefficient of variation of key components in the finished product is controlled below 1.5%, ensuring the uniformity and stability of the nutrient content in a single bag of product. Attached Figure Description

[0025] Figure 1 This is a graph showing the moisture content data in the physicochemical property testing of the finished product of this invention; Figure 2 This is a graph showing the protein content data from the physicochemical property testing of the finished product of this invention. Figure 3 This is a graph showing the dissolution time data in the physicochemical property testing of the finished product of this invention; Figure 4 This is a graph showing pH value data from the physicochemical property testing of the finished product of this invention. Figure 5 This is a graph showing the average content data in the mixing uniformity test of the present invention; Figure 6 This is a graph showing the coefficient of variation data in the mixing uniformity test of this invention; Figure 7 This is a graph showing the transmittance data from the powder flowability and hygroscopic stability test of the present invention. Detailed Implementation

[0026] The technical solutions in 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0027] The main raw materials and reagents used in the following examples and comparative examples have the following sources and specifications. Reagents not specifically mentioned are all commercially available analytical grade or higher grade products.

[0028] Cod collagen peptides (CAS No.: 9007-34-5), food grade, with a weight-average molecular weight (Mw) ranging from 500 Da to 3000 Da; Skipjack tuna elastin peptide (CAS No.: 9007-58-3), food grade, with a total content of desmokinin and isodesmokinin greater than 1 mg / g; Sodium hyaluronate (CAS No.: 9067-32-7), food grade, with a weight-average molecular weight (Mw) of 3000 Da to 10000 Da; γ-Aminobutyric acid (CAS No.: 56-12-2), food grade, purity ≥99%; Inulin (CAS No.: 9005-80-5), food grade, degree of polymerization (DP) range 10 to 60; Blood orange powder, food grade, spray-dried powder, passed through an 80-mesh sieve; Acerola cherry powder, food grade, with natural vitamin C content ≥17%; Blueberry powder, food grade, spray-dried powder, passed through an 80-mesh sieve; Food-grade flavorings.

[0029] Preparation Example 1: This preparation example provides a method for preparing cod collagen peptides, including the following steps: Select frozen deep-sea cod skin, thaw it, wash it to remove impurities, and chop it into pieces of 0.5cm to 1cm. Soak the fish skin pieces in a 0.2mol / L sodium hydroxide solution at a liquid-to-material ratio of 10:1 (mL / g) at 25℃ for 2 hours to remove non-collagenous protein and fat. After soaking, rinse with water until neutral. The pretreated fish skin pieces were mixed with water and pulped, the solid-liquid ratio was adjusted to 1:10 (g / mL), the pH was adjusted to 2.5, and 1% of the fish skin weight of pepsin (enzyme activity 3000U / g) was added. The mixture was enzymatically hydrolyzed at 38℃ for 1.5 hours for initial degradation. Then the pH was adjusted to 8.5, and 2% of the fish skin weight of alkaline protease (or complex protease, enzyme activity 100000U / g) was added. The mixture was then enzymatically hydrolyzed at 55℃ for 4 hours. After enzymatic hydrolysis, the temperature is rapidly raised to 95°C and maintained for 10 minutes to inactivate the enzyme. After cooling, the solution is decolorized with activated carbon and the precipitate is removed by a tubular centrifuge. The supernatant is first filtered through an ultrafiltration membrane with a molecular weight cutoff of 3000 Da to remove incompletely hydrolyzed macromolecular fragments. The permeate is then concentrated and filtered through a nanofiltration membrane with a molecular weight cutoff of 300 Da to 500 Da to remove inorganic salts and free amino acids, and the retentate is collected. The retentate was centrifuged and spray-dried at an inlet air temperature of 180°C and an outlet air temperature of 85°C. The powder was collected to obtain cod collagen peptides.

[0030] The weight-average molecular weight (Mw) of cod collagen peptides ranges from 500 Da to 3000 Da, with components having a molecular weight of less than 1000 Da accounting for 88.5%.

[0031] Preparation Example 2: This preparation example provides a method for preparing skipjack tuna elastin peptides, including the following steps: Take the heart aortic bulb tissue of skipjack tuna, remove the reddish-brown part caused by blood residue, clean it and mince it; defatt it with acetone, and then air dry it; add the air-dried powder to 0.1 mol / L sodium hydroxide solution, with a liquid-to-solid ratio of 10:1 (mL / g), heat it at 90℃ to 95℃ for 30 to 60 minutes, centrifuge and discard the supernatant containing collagen and other proteins, collect the precipitate and wash it repeatedly with water until neutral; The purified elastin precipitate was mixed with water and slurried at a liquid-to-solid ratio of 15:1 (mL / g). The pH was adjusted to 9, and 3% of the dry weight of the precipitate was added with alkaline protease (enzyme activity 200000U / g). The mixture was then enzymatically hydrolyzed in a 55℃ constant temperature water bath for 8 to 10 hours to ensure the release of peptides rich in desmokinin. After enzymatic hydrolysis, the enzyme was inactivated by boiling for 15 minutes. After cooling, the mixture was centrifuged at 4000 r / min for 20 minutes, and the supernatant was collected. The supernatant was clarified by microfiltration through a ceramic membrane with a pore size of 0.2 μm to remove trace suspended solids. The filtrate was then filtered through an ultrafiltration membrane with a molecular weight cutoff of 5000 Da, and the permeate was collected. The permeate was placed in a vacuum freeze dryer and dried for 24 hours at a cold trap temperature of -40°C and a vacuum degree of 10Pa to obtain the bonito elastin peptide.

[0032] The total content of desmokinin and isodesmokinin in skipjack tuna elastin peptides is 1.3 mg / g.

[0033] Preparation Example 3: This preparation example provides a method for preparing sodium hyaluronate, including the following steps: Commercially available sodium hyaluronate prepared by fermentation was dissolved in pure water to prepare a 1% aqueous solution to ensure that the system viscosity was appropriate and the enzymatic hydrolysis was uniform. Hyaluronidase was added to the solution at a dosage of 1000 U per gram of substrate. The pH of the solution was adjusted to 6.0, and the solution was placed in a constant temperature reaction vessel at 37°C for enzymatic hydrolysis. The viscosity of the solution was monitored in real time using a rotational viscometer, and the reaction endpoint was determined by combining the pre-established viscosity-molecular weight standard curve. When the monitoring data indicates that the molecular weight drops to around the target value of 5500 Da (approximately 2.5 hours of reaction), the feed solution is rapidly heated to above 95°C using a plate heat exchanger and maintained for 10 minutes to instantly inactivate enzyme activity and prevent excessive degradation. After the lysis solution is cooled to room temperature, 0.5% activated carbon is added for decolorization and adsorption, and the activated carbon and impurities are removed by filtration. The filtrate is pumped into a nanofiltration or ultrafiltration membrane device with a molecular weight cutoff of 1000 Da to 2000 Da for tangential flow filtration. In constant volume mode, inorganic salts and monosaccharides and disaccharides produced by enzymatic hydrolysis are removed by water dialysis. Then, the solution is concentrated and collected. The concentrate is centrifuged and spray-dried (inlet air temperature 160-180℃, outlet air temperature 80-90℃), and the powder is collected.

[0034] The weight-average molecular weight (Mw) of sodium hyaluronate is 5500 Da.

[0035] Example 1: This embodiment provides a collagen solid beverage formulation, comprising the following components in parts by weight: Cod collagen peptides: 90 portions; Inulin: 10 parts; Blood orange powder: 8 portions; Acerola cherry powder: 7 servings; γ-Aminobutyric acid: 6 parts; Skipjack tuna elastin peptides: 5 parts; Blueberry powder: 4 servings; Sodium hyaluronate: 3 parts; Food flavoring: 2 parts.

[0036] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 25℃ and a relative humidity of 40%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transmission window. Pass the raw materials through a 20-mesh stainless steel sieve to remove false lumps. S2. Take 20 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 20 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.55 MPa, a pulse frequency of 0.3s / 0.3s, and a mixing time of 4 minutes to obtain a primary mixture. S3. Add the remaining 50 parts of cod collagen peptide, the total amount of inulin, blood orange powder, and acerola cherry powder to the double helix conical mixer in sequence, and finally add the primary mixture; turn on the spindle speed to 60 rpm and mix for 300 seconds; S4. The uniformly mixed material is transported through pipelines and passed through a metal detector (sensitivity Fe 0.8mm) into the hopper of the automatic packaging machine; it is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 180℃ and a transverse sealing temperature of 190℃ to obtain a finished product with a net content of 4g per bag.

[0037] Example 2: This embodiment provides a collagen solid beverage formulation, comprising the following components in parts by weight: Cod collagen peptides: 75 parts; Inulin: 6 parts; Blood orange powder: 4.5 parts; Acerola cherry powder: 4 servings; γ-Aminobutyric acid: 3.75 parts; Skipjack tuna elastin peptides: 2.5 parts; Blueberry powder: 2 servings; Sodium hyaluronate: 1.5 parts; Food flavoring: 0.88 parts.

[0038] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 22℃ and a relative humidity of 35%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transfer window. Pass the raw materials through a 20-mesh stainless steel sieve. S2. Take 20 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 20 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.45 MPa, a pulse frequency of 0.4 s / 0.4 s, and a mixing time of 5 minutes to obtain a primary mixture. S3. Add the remaining 35 parts of cod collagen peptide, the total amount of inulin, blood orange powder and acerola cherry powder to the paddle mixer in sequence, and finally add the primary mixture; turn on the mixing frequency of 50Hz and mix for 180 seconds. S4. The uniformly mixed material is transported through pipelines and passes through a metal detector before being fed into the hopper of an automatic packaging machine. It is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 150℃ and a transverse sealing temperature of 165℃ to obtain a finished product with a net content of 4g per bag.

[0039] Example 3: This embodiment provides a collagen solid beverage formulation, comprising the following components in parts by weight: Cod collagen peptides: 60 servings; Inulin: 3 parts; Blood orange powder: 2 parts; Acerola cherry powder: 2 servings; γ-Aminobutyric acid: 1.5 parts; Skipjack tuna elastin peptides: 1 serving; Blueberry powder: 1 serving; Sodium hyaluronate: 0.2 parts; Food flavoring: 0.1 parts.

[0040] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 18℃ and a relative humidity of 30%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transfer window. Pass the raw materials through a 10-mesh stainless steel sieve. S2. Take 15 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 15 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.40 MPa, a pulse frequency of 0.5s / 0.5s, and a mixing time of 6 minutes to obtain a primary mixture. S3. Add the remaining 30 parts of cod collagen peptide, the total amount of inulin, blood orange powder and acerola cherry powder to the paddle mixer in sequence, and finally add the primary mixture; turn on the mixing frequency of 40Hz and mix for 150 seconds. S4. The uniformly mixed material is transported through pipelines and passes through a metal detector before being fed into the hopper of an automatic packaging machine. It is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 120℃ and a transverse sealing temperature of 140℃ to obtain a finished product with a net content of 4g per bag.

[0041] Example 4: This embodiment provides a collagen solid beverage formulation, comprising the following components in parts by weight: Cod collagen peptides: 75 parts; Inulin: 6 parts; Blood orange powder: 4.5 parts; Acerola cherry powder: 4 servings; γ-Aminobutyric acid: 3.75 parts; Skipjack tuna elastin peptides: 2.5 parts; Blueberry powder: 2 servings; Sodium hyaluronate: 1.5 parts; Food flavoring: 0.88 parts.

[0042] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 22℃ and a relative humidity of 35%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transfer window. Pass the raw materials through a 20-mesh stainless steel sieve. S2. Take 20 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 20 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.45 MPa, a pulse frequency of 0.4 s / 0.4 s, and a mixing time of 5 minutes to obtain a primary mixture. S3. Add the remaining 35 parts of cod collagen peptide, the total amount of inulin, blood orange powder and acerola cherry powder to the paddle mixer in sequence, and finally add the primary mixture; turn on the mixing frequency of 50Hz and mix for 120 seconds. S4. The uniformly mixed material is transported through pipelines and passes through a metal detector before being fed into the hopper of an automatic packaging machine. It is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 130℃ and a transverse sealing temperature of 150℃ to obtain a finished product with a net content of 4g per bag.

[0043] Example 5: This embodiment provides a collagen solid beverage formulation, comprising the following components in parts by weight: Cod collagen peptides: 75 parts; Inulin: 6 parts; Blood orange powder: 4.5 parts; Acerola cherry powder: 4 servings; γ-Aminobutyric acid: 3.75 parts; Skipjack tuna elastin peptides: 2.5 parts; Blueberry powder: 2 servings; Sodium hyaluronate: 1.5 parts; Food flavoring: 0.88 parts.

[0044] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 22℃ and a relative humidity of 35%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transfer window. Pass the raw materials through a 20-mesh stainless steel sieve. S2. Take 20 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 20 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.45 MPa, a pulse frequency of 0.4 s / 0.4 s, and a mixing time of 8 minutes to obtain a primary mixture. S3. Add the remaining 35 parts of cod collagen peptide, the total amount of inulin, blood orange powder and acerola cherry powder to the paddle mixer in sequence, and finally add the primary mixture; turn on the mixing frequency of 45Hz and mix for 180 seconds. S4. The uniformly mixed material is transported through pipelines and passes through a metal detector before being fed into the hopper of an automatic packaging machine. It is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 150℃ and a transverse sealing temperature of 165℃ to obtain a finished product with a net content of 4g per bag.

[0045] Example 6: This embodiment provides a collagen solid beverage, comprising the following components in parts by weight: Cod collagen peptides: 80 servings; Inulin: 8 parts; Blood orange powder: 6 parts; Acerola cherry powder: 5 servings; γ-Aminobutyric acid: 5 parts; Skipjack tuna elastin peptides: 3.5 parts; Blueberry powder: 3 servings; Sodium hyaluronate: 2.5 parts; Food flavoring: 1.5 parts.

[0046] This embodiment also provides a production process for a collagen solid beverage formulation, including the following steps: S1. In a clean environment with a temperature of 22℃ and a relative humidity of 35%, remove the outer packaging of all powdered raw materials. After the inner packaging surface is disinfected with 75% ethanol, it is transferred through a UV transfer window. Pass the raw materials through a 20-mesh stainless steel sieve. S2. Take 20 parts of cod collagen peptides and put them into a pneumatic mixer as the base material. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover with 20 parts of cod collagen peptides. Start the mixer with a compressed air pressure of 0.45 MPa, a pulse frequency of 0.4 s / 0.4 s, and a mixing time of 5 minutes to obtain a primary mixture. S3. Add the remaining 40 parts of cod collagen peptide, the total amount of inulin, blood orange powder and acerola cherry powder to the paddle mixer in sequence, and finally add the primary mixture; turn on the mixing frequency of 50Hz and mix for 180 seconds. S4. The uniformly mixed material is transported through pipelines and passes through a metal detector before being fed into the hopper of an automatic packaging machine. It is then filled with nitrogen gas of 99.5% purity and heat-sealed at a longitudinal sealing temperature of 150℃ and a transverse sealing temperature of 165℃ to obtain a finished product with a net content of 4g per bag.

[0047] Comparative Example 1: Compared with Example 2, the difference is that bonito elastin peptides are not added, and their weight parts are made up by cod collagen peptides (i.e., the amount of cod collagen peptides is adjusted to 77.5 parts), while the other components and preparation steps are the same.

[0048] Comparative Example 2: Compared with Example 2, the difference is that inulin is replaced with an equal part by weight of maltodextrin, while the other components and preparation steps are the same.

[0049] Comparative Example 3: Compared with Example 2, the difference is that sodium hyaluronate (Mw3000Da-10000Da) is replaced with an equal part by weight of ordinary macromolecular sodium hyaluronate (Mw>1,000,000Da), while the other components and preparation steps are the same.

[0050] Comparative Example 4: Compared with Example 2, the difference is that the production process does not involve graded mixing. Specifically, the first-stage mixing in step S2 is cancelled, and all raw materials (cod collagen peptide, inulin, blood orange powder, acerola cherry powder, γ-aminobutyric acid, bonito elastin peptide, blueberry powder, sodium hyaluronate, and food flavoring) are added to the double helix conical mixer at one time, and the mixing time is extended to 480 seconds. All other steps and parameters are the same.

[0051] Comparative Example 5: Compared with Example 2, the difference is that in production process step S1, the relative humidity of the environment is set to 60%, while the other steps and parameters are the same.

[0052] Test Example 1: Experimental steps: Samples from each embodiment were randomly selected and placed in a white porcelain dish. Their color and texture were observed under natural light. 4.0 g of sample was dissolved in 150 mL of warm water (45°C), and its odor and taste were evaluated. The evaluation criteria used a pass / fail judgment, focusing on the presence of lumps, off-odors, or uneven color.

[0053] According to GB5009.3 "National Food Safety Standard - Determination of Moisture in Food", the direct drying method was adopted. 2.00 g (accurate to 0.0001 g) of sample was placed in a pre-weighed weighing bottle and dried in a drying oven at 101℃-105℃ until constant weight. The mass loss ratio was calculated.

[0054] According to GB5009.5 "National Food Safety Standard - Determination of Protein in Food", the total nitrogen content was determined by the Kjeldahl method and multiplied by the protein conversion factor (6.25).

[0055] Simulate a consumer mixing scenario. Add 150mL of distilled water at 45℃±1℃ to a 250mL beaker, turn on the magnetic stirrer, and set the speed to 150rpm (simulating gentle stirring with a spoon). Pour 4.0g of sample into the water quickly in one go, and start a stopwatch to record the time required from when the powder comes into contact with the water surface until no floating powder clumps or sediment are visible to the naked eye.

[0056] Weigh 1.0g of sample and dissolve it in 10mL of boiled and cooled distilled water. After complete dissolution, use a calibrated pH meter to measure the pH value of the solution.

[0057] Experimental results The test data records for the samples in each embodiment are shown in Table 5.

[0058] Table 1 Summary of Physicochemical Properties Test Data of Finished Products from Examples 1-6 Table 1 shows that the moisture content of all products in the examples was controlled below 4.0%, significantly better than the national standard requirement (≤7.0%). Comparing Example 1 (ambient RH 40%, moisture 3.92%), Example 2 (ambient RH 35%, moisture 3.41%), and Example 3 (ambient RH 30%, moisture 3.15%), it can be seen that the product moisture content increases with increasing ambient humidity. The low-humidity environment (RH 30%-40%) defined in this technical solution effectively blocks the moisture absorption path of hygroscopic raw materials (such as collagen peptides and fruit and vegetable powders) during the production process, ensuring the dryness of the finished product from the source. This low moisture content state slows down the formation of liquid bridges between powder particles, which is a key factor in ensuring that the product is loose and free of lumps.

[0059] Test data show that the dissolution time of each product in the embodiments is less than 30 seconds, demonstrating excellent rapid dissolution characteristics.

[0060] The cod collagen peptides and bonito elastin peptides selected in this scheme are both enzymatically hydrolyzed small molecule fragments. Compared with large molecule proteins, their hydrophilic groups are fully exposed, their hydration energy is lower, and they dissolve instantly in water.

[0061] Furthermore, Example 3 exhibited the shortest dissolution time (21.4 s), while Example 1 showed a relatively longer time (27.5 s). This is related to the aggregation effect of the high concentration of peptides in the formulation, but even under the high loading (90 parts) conditions of Example 1, the dissolution time remained within the ideal range. The introduction of inulin as a dispersion carrier in the preparation process, along with the graded mixing process that imparts a uniform particle size distribution to the powder, prevents the formation of high-viscosity localized agglomerates, allowing water molecules to rapidly penetrate into the particles.

[0062] After adjusting parameters such as mixing time and packaging temperature, Examples 4 and 5 showed no significant abrupt changes in their physicochemical indicators (moisture, protein, pH) compared to Example 2, with data fluctuations within a reasonable error range. This indicates that the process parameter window determined in this invention (e.g., mixing time 180s-300s, heat-sealing temperature range) has good process stability. In particular, the measured protein content highly matches the theoretical value of the formula, verifying the effectiveness of the mixing process in solving the stratification problem of raw materials with large density differences (e.g., heavy mineral salts and light spray-dried fruit powder), ensuring the uniformity and stability of the nutritional components in each bag of product.

[0063] Test Example 2: Experimental steps: Experiment A: Ten independent sample bags were randomly selected from the left, right, center, top, bottom, and dead corner positions of the automatic packaging machine's hopper in each group. The content of γ-aminobutyric acid (GABA) in each sample was determined using high-performance liquid chromatography (HPLC). The mean, standard deviation, and coefficient of variation were calculated. The coefficient of variation reflects the dispersion of the component distribution; a smaller value indicates a more uniform mixture.

[0064] Experiment B: The method for determining dissolution time is the same as in Test Example 1. Solution clarity determination: Weigh 1.0 g of sample and dissolve it in 100 mL of distilled water. After ultrasonic degassing, measure the transmittance at a wavelength of 600 nm using a UV spectrophotometer.

[0065] Experiment C: The angle of repose of the sample was determined using a powder property tester. Hygroscopic stability test: 5.00 g of sample was accurately weighed and placed in a weighing bottle, then left uncovered in a constant temperature and humidity chamber (25℃, 75% relative humidity) for 12 hours. After removal, the sample was weighed, the moisture gain rate was calculated, and the appearance of the powder was observed.

[0066] Experimental results: The test data for each experimental group are recorded in Tables 2 to 4 below.

[0067] Table 2 Summary of Mixing Uniformity Test Data Table 3. Solubility and Clarity Test Data Table 4. Test data on powder flowability and hygroscopic stability Table 2 shows that Experiment A data indicates that the CV values ​​of GABA content in Examples 1 to 6 were all controlled below 1.5%, demonstrating extremely high mixing uniformity. Comparative Example 4 (without staged mixing) had a CV value as high as 8.54%, and Comparative Example 5 (high humidity environment) had a CV value of 4.59%. This demonstrates that a multi-stage dispersion strategy and a low humidity environment are key to the uniform distribution of trace components. In Comparative Example 5, the powder absorbed moisture, generating agglomeration forces that hindered the free movement of particles within the mixer, leading to a decrease in uniformity.

[0068] As shown in Table 3, Experiment B results indicate that the dissolution time for all examples was within 30 seconds, and the solutions were clear. Comparative Example 3 (high molecular weight sodium hyaluronate) showed a significantly prolonged dissolution time of 68.5 seconds and low light transmittance, confirming the influence of raw material molecular weight screening on product solubility. Comparative Example 5 had a dissolution time of approximately 39 seconds, likely due to the formation of small, damp clumps within the powder, which slowed the rate of moisture penetration.

[0069] As shown in Table 4, in Experiment C, the angle of repose of the example groups was less than 35°, and the moisture absorption weight gain was less than 4.6%, demonstrating excellent flowability and moisture resistance. Comparative Example 2 (maltodextrin replacing inulin) showed a moisture absorption weight gain as high as 8.92% and exhibited severe caking, proving that inulin has a superior physical barrier and moisture-proof function compared to maltodextrin in the formulation. Comparative Example 5 had an initial angle of repose of 46.8°, indicating that uncontrolled environmental humidity directly damaged the physical structure of the finished product, causing it to lose its flowability.

[0070] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A collagen solid beverage formula, characterized in that, The solid beverage comprises components in the following parts by weight: 60-90 parts cod collagen peptides; 3-10 parts inulin; 2-8 parts blood orange powder; Acerola cherry powder 2-7 parts; 1.5-6 parts of γ-aminobutyric acid; Skipjack tuna elastin peptides 1-5 parts; 1-4 parts blueberry powder; Sodium hyaluronate 0.2-3 parts; Food flavoring 0.1-2 parts.

2. The collagen solid beverage formula according to claim 1, characterized in that, The solid beverage comprises components in the following parts by weight: 75-80 parts cod collagen peptides; 6-8 parts inulin; Blood orange powder 4.5-6 parts; 4-5 parts acerola cherry powder; γ-Aminobutyric acid 3.75-5 parts; Skipjack tuna elastin peptides 2.5-3.5 parts; 2-3 parts blueberry powder; Sodium hyaluronate 1.5-2.5 parts; Food flavoring: 0.88-1.5 parts.

3. The collagen solid beverage formula according to claim 1, characterized in that, The weight-average molecular weight (Mw) of the cod collagen peptides is distributed between 500 Da and 3000 Da, with the proportion of components with a molecular weight less than 1000 Da being ≥88.5%. The cod collagen peptides are prepared by the following method: frozen deep-sea cod skin is selected, and after soaking in 0.2 mol / L sodium hydroxide solution to remove fat and non-collagenous proteins, it is subjected to double-enzyme hydrolysis. The double-enzyme hydrolysis is carried out by first adding pepsin at pH 2.5 and 38°C for 1.5 hours, adjusting the pH to 8.5, and then adding alkaline protease for 4 hours at 55°C. The hydrolysate is subjected to enzyme inactivation, decolorization, ultrafiltration with a molecular weight cutoff of 3000 Da, and concentration filtration with a molecular weight cutoff of 300 Da to 500 Da, and finally spray drying to obtain the final product.

4. The collagen solid beverage formula according to claim 1, characterized in that, The total content of desmokinin and isodesmokinin in the skipjack tuna elastin peptide is ≥1.3 mg / g; The skipjack tuna elastin peptide was prepared by the following method: skipjack tuna heart bulb tissue was taken, defatted, and then heated in 0.1 mol / L sodium hydroxide solution at 90°C to 95°C for 30 to 60 minutes. The precipitate was collected and washed with water until neutral. The pH of the precipitate was adjusted to 9.0, and alkaline protease was added and enzymatically hydrolyzed at 55°C for 8 to 10 hours. The hydrolysate was subjected to enzyme inactivation, centrifugation, microfiltration through a 0.2 μm ceramic membrane, and ultrafiltration through a 5000 Da molecular weight cutoff membrane. The permeate was collected and freeze-dried to obtain the final product.

5. The collagen solid beverage formulation according to claim 1, characterized in that, The weight-average molecular weight (Mw) of the sodium hyaluronate is 3000 Da-10000 Da; The sodium hyaluronate is prepared by the following method: a high molecular weight sodium hyaluronate is prepared into an aqueous solution, hyaluronidase is added, and an enzymatic reaction is carried out at pH 6.0 and 37°C, while the solution viscosity is monitored in real time; when the weight-average molecular weight drops to the target range, the enzyme is inactivated by heating, followed by decolorization with activated carbon, and the filtrate is pumped into a membrane separation device with a molecular weight cutoff of 1000 Da to 2000 Da for tangential flow filtration. After constant volume water addition dialyzing and concentration, it is spray dried to obtain the final product.

6. A production process for a collagen solid beverage formula, characterized in that, The preparation of a collagen solid beverage formulation according to any one of claims 1-5 includes the following steps: S1. Sieve all raw materials and set aside for later use; S2. Take a portion of cod collagen peptides as the base material and put it into the mixer. Then, add the full amount of γ-aminobutyric acid, bonito elastin peptides, blueberry powder, sodium hyaluronate and food flavoring in sequence. Finally, cover the remaining cod collagen peptides and mix to obtain the first-stage mixture. S3. Add the remaining amount of cod collagen peptide, the full amount of inulin, blood orange powder and acerola cherry powder to the mixer in sequence, and finally add the primary mixture and mix. S4. After the uniformly mixed materials are tested for metals, they are then packaged with nitrogen to obtain the finished product.

7. The production process of a collagen solid beverage formulation according to claim 6, characterized in that, In step S1, the ambient temperature is controlled at 18℃-25℃ and the relative humidity is controlled at 30%-40%; the raw material is passed through a 10-20 mesh sieve.

8. The production process of a collagen solid beverage formulation according to claim 6, characterized in that, In step S2, the mixer is a pneumatic mixer, and the amount of cod collagen peptide used as the base material is 15-20 parts, and the amount of cod collagen peptide used for covering is 15-20 parts. The mixing parameters are: compressed air pressure 0.40MPa-0.55MPa, pulse frequency 0.3s / 0.3s-0.5s / 0.5s, and mixing time 4-8 minutes.

9. The production process of a collagen solid beverage formulation according to claim 6, characterized in that, In step S3, the mixer is a double-helix conical mixer or a paddle mixer; the mixing time is 120 seconds to 300 seconds.

10. The production process of a collagen solid beverage formulation according to claim 6, characterized in that, In step S4, nitrogen gas with a purity of ≥99.5% is used for replacement filling; the heat sealing conditions are: longitudinal sealing temperature 120℃-180℃, and transverse sealing temperature 140℃-190℃.

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