Product capable of providing muscle nutrition support and preparation method thereof
Through supercritical CO2 pulse atomization granulation and low-temperature step drying technology, combined with microcapsule protection and precise sweeteners, the problems of slow dissolution, poor taste, easy inactivation of immune components and short replenishment window of sports nutrition protein powder have been solved, and rapid dissolution, continuous ammonia supply and efficient immune support have been achieved.
Patent Information
- Application Number
- CN202511204346.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-27
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2045-08-27
AI Technical Summary
Existing sports nutrition protein powders have technical pain points in terms of preparation speed, bitterness control, immune activity protection, continuous ammonia supply and powder fluidity, especially the loss of active ingredients and difficulty in particle dispersion caused by high-temperature spraying.
Supercritical CO2 pulse atomization granulation technology combined with low-temperature step-down pressure drying is used to prepare protein particles with an open pore structure. Bovine colostrum IgG is protected by α-lactalbumin/hydrolyzed whey copolymer shell microcapsules, and combined with a precise sweetener system to achieve 15s instant dissolution and sustained amino acid release.
The protein powder achieves instant dissolution in 15 seconds, high IgG activity, low sugar and no bitterness, and continuous ammonia supply, significantly improving the dissolution speed, taste and immune support effect of sports nutrition powder, overcoming the long-standing pain points of existing technologies.
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Figure CN120753310A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of sports nutrition food, and in particular to a product that can provide muscle nutrition support and a preparation method thereof. Background Art
[0002] In recent years, the market for sports protein powders targeting strength training, functional rehabilitation, and weight management has maintained rapid growth. Whey protein is considered the "gold standard" for sports nutritional supplements due to its high content of branched-chain amino acids, rapid digestion, and high nitrogen utilization rate. For the past two decades, commercially available muscle-building or rehabilitation protein powders have mostly been dry-blended with a single whey protein concentrate (WPC) or whey protein isolate (WPI), supplemented with carbohydrates such as maltodextrin. While these powders provide a quick boost of amino acids and energy after training, they have been plagued by issues such as difficulty in dissolving, a bland taste, a short absorption window, and a lack of immune support, which have plagued both consumers and R&D professionals.
[0003] To expand nutritional coverage, researchers have begun combining different protein sources in a "matrix" format. The Chinese invention patent CN117796531B, filed by the applicant, employs the general concept of a "triple whey protein matrix, bovine colostrum powder, α-lactalbumin, and zinc and magnesium" formula to increase muscle mass, with the muscle-building effect validated through animal and human studies. While this approach is significantly more complex than single whey powder, its core process remains "direct mixing of all powders at room temperature." It fails to consider the heat-acid inactivation of bovine colostrum IgG and does not address any technical measures for the product's solubility, staged release, or bitterness control.
[0004] Furthermore, traditional whey powder tends to float and clump, requiring consumers to shake vigorously for 30-60 seconds in a shaker cup for substantial dissolution. Shanghai Bright Dairy's Chinese invention patent CN102599402B improves wettability and dispersibility by introducing 0.5%-1.0% sodium carboxymethylcellulose (Na-CMC) and 0.2%-0.6% soy lecithin into the WPC / WPI system to create a hydrophilic-lipophilic bilayer. However, official testing still requires "continuous shaking for more than 30 seconds" for complete dissolution, significantly increasing viscosity and resulting in a thicker mouthfeel. While further spray instantaneous granulation or fluidized bed granulation can improve sinking speed, they often rely on high-temperature drying or large amounts of water-soluble colloidal binders, which can damage heat-sensitive active ingredients (such as colostrum IgG) and may introduce excessive sodium salts, resulting in a "greasy" mouthfeel.
[0005] To enhance post-exercise immune support, the industry has experimented with incorporating bovine colostrum powder or its immunoglobulin (IgG) directly into protein powder (e.g., CN117796531B). However, IgG is extremely sensitive to heat, acid, and shear, and conventional high-temperature spraying can result in over 50% loss of activity. Earlier Chinese invention patents CN1284602C and CN101219152B from Jilin Agricultural University proposed using spray drying or suspension granulation with wall materials such as gelatin, gum arabic, and lactose to enhance IgG's gastric acid resistance. However, these microcapsules generally have a particle size greater than 20μm, making them prone to floating and creating a sandy texture, making them difficult to disperse with 100-300μm transient whey particles. Furthermore, the wall materials, primarily composed of polysaccharides or gelatin, are not designed for the rapid and sustained, segmented protein absorption required by athletes.
[0006] Currently, instantaneous protein powder production primarily utilizes high-temperature spray cooling to create pores or high-shear wet granulation followed by hot air drying. Publicly available literature reports on the application of supercritical CO2 pulse foaming and low-temperature pore formation to food powders. Existing CO2 foaming research focuses on thermoplastic materials like starch and polylactic acid (e.g., CN110684230A). The associated process temperatures range from 60°C to 120°C, well above the denaturation point of IgG and unsuitable for fluidized sedimentation of natural protein powders. Summary of the Invention
[0007] In order to solve the above-mentioned technical problems, the purpose of the present invention is to provide a method for preparing a product that can provide muscle nutritional support. The product prepared by this method can be dissolved in 15 seconds, thereby comprehensively solving the long-term technical pain points of existing protein powder in terms of preparation speed, bitterness control, immune activity protection, continuous ammonia supply and powder fluidity.
[0008] A method for preparing a product that can provide muscle nutritional support, the method comprising the following consecutive steps:
[0009] 1) Dry powder premix: Mix the product raw materials, whey protein concentrate powder, whey protein isolate powder, hydrolyzed whey protein powder, bovine colostrum powder, α-lactalbumin powder, calcium silicate, and compound sweetening system components in a drum mixer at low speed for 3–5 minutes at ≤25°C to obtain a uniform premix powder;
[0010] 2) Supercritical CO2 pulse atomization granulation: The premixed powder is fed into a multi-zone fluidized bed, maintained at a bed temperature of 35–40°C and a bed pressure of 0.3–0.5 MPa. An aqueous binder is intermittently sprayed into the bed, while supercritical CO2 at 6–8 MPa and 35–40°C is simultaneously introduced as an atomization and instantaneous foaming medium. This causes the CO2 to rapidly expand within the particles, forming an open-pore structure. This results in wet particles with a true porosity ≥60% and a water content ≤8%.
[0011] 3) Step-down drying: Continuously reduce the bed pressure to normal pressure, maintain hot air at 40-45°C, and promote the simultaneous removal of residual CO2 and moisture until the moisture content of the particles is ≤4%;
[0012] 4) Vibration classification recovery: The particles are subjected to two-stage vibration screening to retain the main material with a particle size of 180-300μm; particles >300μm are recovered and crushed; and fine powder <180μm is returned to step 1) for reuse.
[0013] Preferably, the bovine colostrum powder is added in the form of bovine colostrum powder microcapsules. The preparation method of the bovine colostrum powder microcapsules is as follows:
[0014] a) Wall material solution preparation: Dissolve α-lactalbumin powder and hydrolyzed whey protein powder in deionized water at a ratio of 2–4:1, resulting in a total solids content of 15–25% (w / w). Adjust the pH to 6.7–6.8. The wall material should comprise 50–80% of the weight of the bovine colostrum powder.
[0015] b) Enzymatic covalent crosslinking: Cool the solution from step 1) to 30-40°C, add 4-10 U of microbial transglutaminase per gram of wall material protein, and react with gentle stirring for 20-40 minutes before terminating the enzyme activity.
[0016] c) Homogenizing and dispersing the core material: Add freeze-dried bovine colostrum powder with an IgG content of not less than 20% to the solution in step 2) and subject the mixture to high-speed shearing at 5,000-70,000 rpm for 4-8 minutes. Subsequently, subject the mixture to high-pressure homogenization at 80-120 bar and 20-35 bar, respectively. The outlet temperature is controlled to be no higher than 30°C.
[0017] d) Nitrogen protection spray drying: Adjust the system viscosity to 45±5 mPa·s; spray dry the emulsion from step c) in a closed-circuit nitrogen spray drying tower until the resulting powder has a moisture content of no more than 4% and an IgG retention rate of no less than 85%;
[0018] e) Airflow classification: Use an inert airflow classifier to obtain bovine colostrum powder microcapsules.
[0019] Preferably, the adhesive liquid used in step 2) is composed of 5wt% to 10wt% sodium carboxymethyl cellulose and 0.3wt% to 0.5wt% lecithin, with a mass ratio of 10:1 to 25:1, and the viscosity of the solution is maintained at 60mPa·s to 100mPa·s at 25°C; the instantaneous spray volume of the adhesive liquid is controlled at 0.2kg to 0.6kg / kg premixed powder.
[0020] Preferably, in step 2), supercritical CO2 is injected in a pulse mode of 2s to 4s injection and 6s to 8s intermittently, with a total gas consumption of 0.3kg to 0.6kg / kg premixed powder, so that the average pore size of the final particles is controlled at 20μm to 50μm and the true porosity is not less than 65%.
[0021] Preferably, the final particles after vibration classification in step 4) have a bulk density of 0.38 g / cm³ to 0.45 g / cm³, a Hausner ratio of 1.08 to 1.15, and an agglomeration index of less than 10% after accelerated storage at 40°C and 75% relative humidity for 7 days, and can still be completely dissolved within 15 seconds to reach a solubility of more than 90%.
[0022] Preferably, the raw materials of the product in step 1) include the following components by dry weight: concentrated whey protein powder 35-55wt%; isolated whey protein powder 15-35wt%; hydrolyzed whey protein powder 5-15wt%; bovine colostrum powder 1-5wt%; α-lactalbumin powder 2-10wt%; calcium silicate 0.1-0.3wt%; and a composite sweetening system 0.1-1.0wt%; the bovine colostrum powder is in the form of α-lactalbumin / hydrolyzed whey copolymer shell microcapsules with a particle size of 2-6 μm.
[0023] Preferably, the raw materials of the product further include 0.3-0.5 wt% of lecithin, 2-6 wt% of cocoa powder and 0.5-1.0 wt% of edible salt.
[0024] Preferably, the composite sweetness system comprises mogroside and stevioside with a sweetness equivalent ratio of 1:0.5-1, and optionally further comprises acesulfame potassium and sucralose, with the total amount of acesulfame potassium and sucralose not exceeding 0.008 wt%.
[0025] Preferably, the calcium silicate has an average particle size of 5-15 μm and a BET specific surface area of 70-120 m² / g.
[0026] Furthermore, the present invention also provides a product that can provide muscle nutritional support. The product is prepared using the method described above, and the product has a true porosity of ≥60%; the product has an average bulk density of 0.38–0.45 g / cm³, and a viscosity after redispersion of 20–40 mPa·s; the product reaches a solubility greater than 90% when stirred in 230 mL of water at 15–40°C for ≤15 seconds.
[0027] Preferably, the protein amino acid release of this product has a "fast segment, slow segment" bimodal curve, with a cumulative release of ≥40% at 30 minutes and a cumulative release of ≥90% at 4 hours.
[0028] The present invention has the following technical effects due to the adoption of the above technical solution:
[0029] 1. Instant settlement - instant dissolution dual improvement
[0030] By "supercritical CO2 pulse atomization - stepwise decompression drying" process, ≥60% (preferably ≥65%) true porosity is instantaneously generated inside the particles at a full-link temperature control below 45℃, and the volume average particle size is maintained at 200-280µm. On the one hand, this structure significantly reduces the surface tension, and the powder can be completely wetted and settled after 3 times of light shaking after adding water; on the other hand, a large number of open channels form capillary suction passages, so that the solubility can reach ≥90% within 15s.
[0031] 2. High-preservation bovine colostrum IgG, small intestine targeted delivery
[0032] For the first time, α-lactalbumin / hydrolyzed whey copolymer shell is used for bovine colostrum microcapsules with a particle size of 2-6µm, and a tough protein network is obtained by TGase cross-linking; the outlet temperature is controlled at ≤90℃ in nitrogen protection spraying, and the IgG retention rate reaches more than 85%. The artificial gastric juice-small intestine juice transfer test shows that the integrity is ≥95% at pH<3 for 30min, and the disintegration is ≥80% at pH 6.8 within 30min, ensuring that IgG and slow-release amino acids reach the small intestine absorption site at the same time, realizing the synergistic effect of exercise and immunity.
[0033] 3. "Fast segment - slow segment" amino acid double peak release
[0034] The formula takes 5-15wt% hydrolyzed whey protein as the fast-release component, 35-55wt% WPC and 15-35wt% WPI to form a slow-release skeleton, and at the same time, a controllable amount of sodium carboxymethyl cellulose and microporous structure are dispersed in the particles, so that free diffusion and matrix erosion are carried out cooperatively. The in vitro drug release curve shows that the cumulative release is ≥40% at 30min and ≥90% at 4h, forming a clear "double peak" kinetics that can cover the anabolic window within 0-4h after training; compared with existing single whey protein products (usually reaching a peak at 60-90min and rapidly falling after 2h), the sustainable amino acid supply time is extended by 1.5-2 times.
[0035] 4. Bitterness masking and low sugar flavor balance
[0036] The mogroside: stevioside sweetness equivalent ratio is precisely locked at 1:0.5-1, which can effectively reduce the bitterness after stevia; combined with a total amount of acesulfame K + sucralose ≤0.008wt%, it not only maintains the "zero sucrose" label, but also eliminates the metal-bitterness brought by hydrolyzed whey, so that the sensory score is improved by >1.2 points (9-point system) compared with the unoptimized formula. Compared with the traditional scheme of using only flavor or a single sweetener, the sweetness peak is about 3s earlier, and the after-bitterness residue is reduced by more than 40%.
[0037] In summary, the present invention achieves significant improvements in four major dimensions: instant dissolution in 15 seconds, continuous ammonia supply for 4 hours, high IgG activity, low sugar and no bitterness. It overcomes the long-term technical pain points of existing sports protein powders, such as slow dissolution, poor taste, easy inactivation of immune components and short replenishment window. The technical effect is significant and can be promoted industrially. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] Figure 1 These are the protein release curves of Examples 1 to 3 and Ref-CN. DETAILED DESCRIPTION
[0039] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts are within the scope of protection of the present invention.
[0040] Example (E-1)
[0041]
[0042] (A) Preparation of bovine colostrum microcapsules
[0043] 1) Wall material solution: Dissolve 1.5 kg of α-LA and 0.6 kg of WPH in 9.6 kg of deionized water (18% solids, pH 6.75);
[0044] 2) TGase copolymerization: add 5 U / g protein of transglutaminase at 40°C, gently stir for 30 minutes, and then incubate at 80°C for 2 minutes to stop the enzyme;
[0045] 3) Homogenization and dispersion: Add 2.0 kg of bovine colostrum powder to the wall material liquid cooled to 25°C, shear at 6000 rpm for 5 minutes, and then homogenize at two levels of high pressure at 100 bar and 25 bar, with the outlet temperature controlled at no more than 30°C.
[0046] 4) Nitrogen spray: Adjust the system viscosity to 45±5mPa·s; in a closed-cycle nitrogen spray drying tower, with air inlet 165℃ / air outlet 85℃, nozzle φ0.7mm, the moisture content is 3.5%, D 50 =3.8µm powder; IgG retention rate 87%;
[0047] 5) Airflow classification: removes particles >8µm and <1µm, resulting in 2.3kg of microcapsules.
[0048] (B) Product Preparation
[0049] 1) Premixing: Place WPC, WPI, remaining α-LA, WPH, calcium silicate, sweetener, and microcapsules into a drum mixer at 22°C, 12 rpm, for 3 minutes;
[0050] 2) CO2 pulse granulation: The premixed powder is fed into a multi-zone fluidized bed, maintained at a bed temperature of 37°C and a bed pressure of 0.4 MPa. A binder (8% CMC-Na, 0.4% lecithin, viscosity 80 mPa·s) is pulsed for 3 seconds and 7 seconds, with a total spray volume of 0.4 kg / kg. Simultaneously, supercritical CO2 at 7 MPa and 37°C is introduced as an atomization and instantaneous foaming medium, causing the CO2 to rapidly expand within the granules, forming an open-pore structure. This results in wet granules with a true porosity ≥60% and a water content ≤8%.
[0051] 3) Step-down pressure drying: linearly reduce pressure from 0.4 MPa to normal pressure for 15 minutes, and dry with hot air at 45°C until the moisture content is ≤4%; D 50 =230µm, true porosity 66%;
[0052] 4) Vibration classification: particles between 180 and 300 µm are retained; particles <180 µm are recycled, and particles >300 µm are crushed and reused.
[0053] Example 2 (E-2)
[0054] Formula differences: α-LA 8.0%; bovine colostrum powder 4.0%; WPC 40%; WPI 15%; WPH 12%; CMC-Na 0.15%; other proportions are the same as E1, and the total amount is adjusted to 100%.
[0055] The wall material protein extraction ratio remained the same as above; the total wall material volume was increased accordingly to 2.4 kg α-LA + 0.6 kg WPH. All other process parameters remained unchanged, with only the CO2 pressure adjusted to 6 MPa to maintain the same porosity.
[0056] Example 3 (E-3)
[0057] Key ingredients: WPC 35%; WPI 35%; WPH 6%; α-LA 2%; colostrum powder 1%; CMC-Na 0.05%; all other ingredients are the same as E1. Wall protein = α-LA 0.6kg + WPH 0.3kg. CO2 pressure 8MPa, spray 0.35kg / kg.
[0058] The effects of the present invention are described in detail below through specific test examples.
[0059] 1. Overall arrangement of the test (unified requirements)
[0060] Parallel number: n = 6 (powder science / instant dissolution / flowability / porosity), n = 4 (digestion release / IgG / sensory and electronic tongue), reported means ± SD.
[0061] Statistical methods: One-way or two-way ANOVA + Dunnett (compared with the baseline group), α = 0.05; η is given when necessary 2 Effect size.
[0062] 2. Instruments and methods
[0063] True porosity: He pycnometer density + bulk density → (1-ρ_bulk / ρ_true) × 100%.
[0064] Pore size distribution: Mercury intrusion porosimetry (MIP), reports median pore size and open pore volume fraction.
[0065] Solubility (15 s): 230 mL of 25°C water + 30.0 g of powder, shake horizontally back and forth 3 times (≈8 s), filter immediately after 15 seconds, and dry the residue → (1-residue / 30) × 100%.
[0066] Redispersion viscosity: 25℃, shear rate 50s -1 , 30 s for stable reading.
[0067] Hausner ratio: bulk / tapped density (ASTM D7481 idea).
[0068] Caking index: 40℃ / 75%RH, after 7d and 30d, mechanically broken up and passed through a 10-mesh sieve, with a pass rate of %.
[0069] IgG activity: ELISA (correct for dilution and recovery), take samples immediately after spraying and compare with the prepared solution.
[0070] In vitro digestion: modified INFOGEST-30 min gastric segment (pH 1.8, pepsin 1 mg mL -1 ) → transferred to the intestine (pH 6.8, bile salt 5 mM, pancreatic enzyme 2 mg mL -1 Sampling was performed at 5–240 min intervals, and soluble nitrogen was measured by Kjeldahl method, which was converted into cumulative release %.
[0071] Electronic tongue bitterness index: normalized to quinine equivalent; QDA sensory 9-point scale (trained assessors, ethical compliance).
[0072] Microcapsule particle size: dry particle size analyzer (spray powder), report D10 / D50 / D90.
[0073] Experimental Example 1: scCO2 pulse-process orthogonal optimization on the main effects of "porosity, rapid dissolution, and flow"
[0074] Design: L9(3 4 )Orthogonal experiment
[0075] Factors and levels:
[0076] A: scCO2 pressure (6 / 7 / 8MPa),
[0077] B: Pulse on (2 / 3 / 4s),
[0078] C: Pulse off time (6 / 7 / 8s),
[0079] D: Bed pressure (0.3 / 0.4 / 0.5MPa).
[0080] Fixation: bed temperature 37°C; adhesive liquid = 8% Na-CMC + 0.4% lecithin, 80 mPa·s; spray liquid 0.40 kg·kg -1 Outlet air 45°C; stepwise depressurization for 15 minutes to normal pressure. The formulation used is that of Example E-1.
[0081] Core responses: true porosity (%), 15s instant dissolution (%), Hausner ratio, and agglomeration index (7d, %).
[0082] The results (mean ± SD, n = 6) are shown in Table 1 (key lines are selected):
[0083] Table 1L9 orthogonal test data
[0084]
[0085] ANOVA (main effect contribution, η²)
[0086] For “true porosity”: A(pressure)=46.1%>D(bed pressure)=21.3%>B=18.0%>C=10.4% (all p<0.05).
[0087] For “15s instant dissolution”: A=42.5%>B=23.7%>D=19.2% (all p<0.05); C was marginally significant (p=0.06).
[0088] For “Hausner”: A=38.4%, B=22.1% (both p<0.05).
[0089] Optimal zone: A=8MPa, B=2–3s, C=6–8s, D=0.4MPa; under this combination, true porosity ≥66%, 15s instant dissolution ≥95%, Hausner≈1.08–1.09, and 7d agglomeration ≤8.5%.
[0090] Key points for judgment: The interaction term between scCO2 pressure and pulse onset is most sensitive to "pore opening and rapid dissolution"; a bed pressure of 0.4 MPa can stabilize fluidization and facilitate pore connectivity.
[0091] Test Example 2: Comparative test of step-down pressure reduction, one-time pressure relief, and no scCO2 (conventional thermorheology)
[0092] Grouping
[0093] B-1 (present invention): 8 MPa, 3 / 7s pulse; 37°C; 0.4 MPa; stepwise pressure reduction for 15 min; other parameters are the same as those in A.
[0094] B-2 (one-time pressure relief control): Same as B-1, but with rapid pressure relief to normal pressure within 10 seconds.
[0095] B-3 (comparative example without scCO2): atmospheric pressure air; 50℃ hot air wet granulation; no foaming; drying to ≤4% water.
[0096] The results (mean ± SD, n = 6) are shown in Table 2 .
[0097] Table 2 Comparative test data of step-by-step pressure reduction, one-time pressure relief, and no scCO2 (conventional hot rheumatic method)
[0098]
[0099] Statistical Conclusion: The present invention (B-1) showed significant differences in true porosity, open porosity, and 15-second dissolution rate compared to B-2 / B-3 (p<0.001), and significantly reduced redispersion viscosity (p<0.01). This demonstrates that "stepped pressure reduction" is essential for achieving both interconnected pore formation and instant dissolution / mouthfeel (moderate viscosity), and cannot be replaced by simply "presence or absence of scCO2."
[0100] Experimental Example 3: Effects of Microcapsule Wall Materials and Processes on IgG Activation and Intestinal Release
[0101] The formula of Example 1 remains unchanged, only the microcapsule system is changed (particle size target 2-6 μm):
[0102] C-1: α-lactalbumin / whey hydrolysate (2.5:1, w / w) + TGase cross-linking; closed N2 spray (air outlet ≤ 90℃).
[0103] C-2: Single WPI wall material; closed N2 spray.
[0104] C-3: Gelatin / gum arabic (8% / 4%), air spray (air outlet 95℃).
[0105] C-4: No encapsulation, direct dry mixing with colostrum powder.
[0106] The results (mean ± SD, n = 4) are shown in Table 3.
[0107] Table 3 Experimental data on the effects of capsule wall materials and processes on IgG activation and intestinal release
[0108]
[0109] Statistical conclusion: C-1 significantly outperformed C-2 / C-3 / C-4 (p<0.001) and was the only product to simultaneously meet the criteria of "gastric stability ≥95% + intestinal disintegration ≥80% within 30 minutes." This demonstrates that the copolymerized shell design of α-LA / WPH+TGase plays a decisive role in targeted intestinal release and, in conjunction with the low-temperature scCO2 backbone process, achieves high potency and rapid disintegration.
[0110] Experiment 4: Protein "double peak" ammonia supply kinetics experiment
[0111] Groups: E-1 (the present invention), C-1 (all dry-mixed commercial ideas), C-2 (no microcapsules).
[0112] Quantification: Cumulative release curves from 0–240 min (n=4) were fitted using a two-phase Weibull fit (fast phase F1, slow phase F2). F1(30 min), F2(240 min − 30 min), and overall R² were reported.
[0113] The results are shown in Table 4.
[0114] Table 4 Protein "double peak" ammonia supply kinetics test data
[0115]
[0116] Statistical Conclusion: E-1 exhibits a significantly higher fast-phase rate (vs. C-2, p=0.018; vs. C-1, p<0.001) and the highest slow-phase rate constant (vs. C-2, p=0.012), indicating that the diffusion-erosion synergy of the "open-pore structure + low-content CMC embedding" reaction is not solely determined by the WPH / WPC / WPI ratio. This data supports Quan 10's "double-peak" claim and reinforces its correlation with process structure (not limiting the results).
[0117] Test Example 5: Storage stability and redispersibility (40°C / 75%RH) test
[0118] Groups: E-1 (the present invention) and B-3 (conventional hot air, no scCO2).
[0119] Period: 0, 7, 30d.
[0120] The results are shown in Table 5.
[0121] Table 5 Storage stability and redispersibility (40°C / 75%RH) test data
[0122]
[0123] Statistical conclusion: E-1 still maintained low agglomeration, excellent flowability, high solubility, and high IgG activity after 30 days (the decrease relative to 0 day was significantly smaller than that of B-3; p < 0.001), proving that the open-pore structure + moderately loose stacking reduced the risk of irreversible agglomeration caused by moisture-heat adhesion.
[0124] Test Example 6: Sensory and electronic tongue (bitter / sweet taste chronology), verifying the sweetness system window
[0125] Groups: E-1 (mogroside:stevioside = 1:0.7, total amount of acesulfame potassium + sucralose 0.007%), S-1 (stevioside only), S-2 (mogroside only), S-3 (sucrose only, fine-tuned for sweetness). n = 20 assessors.
[0126] The results are shown in Table 6.
[0127] Table 6 Sensory and electronic tongue test data
[0128]
[0129] Test Example 7: Product Effect Test
[0130] 1. Subject recruitment and grouping
[0131] Thirty-six men (25 ± 2 years old) were recruited from a single fitness club using the methods of CN117796531B. Initial screening included chest circumference of 87–89 cm, upper arm circumference of 28–29 cm, and body mass index (BMI) of 22–24 kg / m². After excluding any history of smoking, chronic disease, or protein supplement use, participants were randomly assigned to six groups of six:
[0132] Blank: only training, hydration;
[0133] Placebo: Training + 60g maltodextrin;
[0134] Ref-CN: training + 60gCN117796531B product;
[0135] E-1, E-2, E-3: training + 60g protein powder of the corresponding embodiment of the present invention.
[0136] 2. Training and Supplementation Program
[0137] All participants, under the supervision of a professional trainer, performed strength training five days a week, following the content and intensity guidelines outlined in CN117796531B: 3 hours daily, 10 RM × 4 sets per muscle group. Within 30 minutes after training, the supplement group shook 60g of powder with 230mL of 25°C water for 8 seconds; the blank group drank the same volume of water alone. This continued for 60 days.
[0138] 3. Measurement and recording
[0139] On the mornings of Days 0 and 60, participants were fasting and had their chest and upper arm circumferences measured (average of the three measurements). On the same day, fat-free mass (FFM) was measured using the InBody S10. Throughout the trial, participants were provided a balanced diet containing 1.5g of protein per kg-1bw to ensure nutritional equivalence.
[0140] 4. Statistical analysis
[0141] The results are presented as mean ± SD. Paired t-test was used to compare the differences between groups before and after the experiment. One-way ANOVA+Dunnett test was used to compare the differences between groups. The significance was set at p < 0.05.
[0142] 5. The results of human muscle growth over 60 days are shown in Table 7
[0143] Table 7 Human muscle growth results data
[0144]
[0145] Compared with the Blank group, p < 0.05; †Compared with the Ref-CN group, p < 0.05.
[0146] 6. Interpretation of results
[0147] Ref-CN (CN117796531B) showed an average increase of 4.0 cm in chest circumference and 2.2 cm in upper arm circumference within 60 days, confirming its muscle-building potential. The present invention's E1 / E-20 / E-30 all significantly outperformed Ref-CN: chest circumference increased by 40–78%, upper arm circumference increased by 14–55%, and lean body mass increased by 36–50%. Among them, E-2 (high α-lactalbumin + high colostrum) showed the most significant effect, indicating that α-LA and IgG synergistically enhance anabolism and recovery.
[0148] The above is a description of the embodiments of the present invention. The above description of the disclosed embodiments will enable professionals in the field to implement or use the present invention. Various modifications to these embodiments will be apparent to professionals in the field. The general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but should conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A method for preparing a product that can provide muscle nutritional support, characterized in that: The method comprises the following consecutive steps: 1) Dry powder premix: Mix the product raw materials, whey protein concentrate powder, whey protein isolate powder, hydrolyzed whey protein powder, bovine colostrum powder, α-lactalbumin powder, calcium silicate, and compound sweetening system components in a drum mixer at low speed for 3–5 minutes at ≤25°C to obtain a uniform premix powder; 2) Supercritical CO2 pulse atomization granulation: The premixed powder is fed into a multi-zone fluidized bed, maintained at a bed temperature of 35–40°C and a bed pressure of 0.3–0.5 MPa. An aqueous binder is intermittently sprayed into the bed, while supercritical CO2 at 6–8 MPa and 35–40°C is simultaneously introduced as an atomization and instantaneous foaming medium. This causes the CO2 to rapidly expand within the particles, forming an open-pore structure. This results in wet particles with a true porosity ≥60% and a water content ≤8%. 3) Step-down drying: Continuously reduce the bed pressure to normal pressure, maintain hot air at 40-45°C, and promote the simultaneous removal of residual CO2 and moisture until the moisture content of the particles is ≤4%; 4) Vibration classification recovery: The particles are subjected to two-stage vibration screening to retain the main material with a particle size of 180-300μm; particles >300μm are recovered and crushed; and fine powder <180μm is returned to step 1) for reuse.
2. The method according to claim 1, characterized in that In step 1), bovine colostrum powder is added in the form of bovine colostrum powder microcapsules. The preparation method of bovine colostrum powder microcapsules is as follows: a) Wall material solution preparation: Dissolve α-lactalbumin powder and hydrolyzed whey protein powder in deionized water at a ratio of 2–4:1, resulting in a total solids content of 15–25% (w / w). Adjust the pH to 6.7–6.
8. The wall material should comprise 50–80% of the weight of the bovine colostrum powder. b) Enzymatic covalent crosslinking: Cool the solution from step 1) to 30-40°C, add 4-10 U of microbial transglutaminase per gram of wall material protein, and react with gentle stirring for 20-40 minutes before terminating the enzyme activity. c) Homogenizing and dispersing the core material: Add freeze-dried bovine colostrum powder with an IgG content of not less than 20% to the solution in step 2) and subject the mixture to high-speed shearing at 5,000-70,000 rpm for 4-8 minutes. Subsequently, subject the mixture to high-pressure homogenization at 80-120 bar and 20-35 bar, respectively. The outlet temperature is controlled to be no higher than 30°C. d) Nitrogen protection spray drying: Adjust the system viscosity to 45±5 mPa·s; spray dry the emulsion from step c) in a closed-circuit nitrogen spray drying tower until the resulting powder has a moisture content of no more than 4% and an IgG retention rate of no less than 85%; e) Airflow classification: Use an inert airflow classifier to obtain bovine colostrum powder microcapsules.
3. The method according to claim 1 or 2, characterized in that The adhesive liquid used in step 2) is composed of 5wt% to 10wt% sodium carboxymethyl cellulose and 0.3wt% to 0.5wt% lecithin, with a mass ratio of 10:1 to 25:1, and the solution viscosity is maintained at 60mPa·s to 100mPa·s at 25°C; the instantaneous spray volume of the adhesive liquid is controlled at 0.2kg to 0.6kg / kg premixed powder.
4. The method according to claim 1, wherein Step 2) Supercritical CO2 is injected in a pulse mode of 2s to 4s injection and 6s to 8s intermittently, with a total gas consumption of 0.3kg to 0.6kg per kg of premixed powder, so that the average pore size of the final particles is controlled at 20μm to 50μm and the true porosity is not less than 65%.
5. The method according to claim 1, wherein The final particles after vibration classification in step 4) have a bulk density of 0.38 g / cm³ to 0.45 g / cm³, a Hausner ratio of 1.08 to 1.15, and an agglomeration index of less than 10% after accelerated storage at 40°C and 75% relative humidity for 7 days, and can still be completely dissolved within 15 seconds to reach a solubility of more than 90%.
6. The method according to claim 2, characterized in that In step 1), the raw materials of the product include the following components on a dry weight basis: 35-55wt% concentrated whey protein powder; 15-35wt% isolated whey protein powder; 5-15wt% hydrolyzed whey protein powder; 1-5wt% bovine colostrum powder; 2-10wt% α-lactalbumin powder; 0.1-0.3wt% calcium silicate; and 0.1-1.0wt% of a composite sweetening system; the bovine colostrum powder is in the form of α-lactalbumin / hydrolyzed whey copolymer shell microcapsules with a particle size of 2-6 μm.
7. The method according to claim 6, characterized in that The raw materials of the product also include 0.3-0.5wt% lecithin, 2-6wt% cocoa powder and 0.5-1.0wt% edible salt.
8. The method according to claim 6, characterized in that The composite sweetness system comprises mogroside and stevioside with a sweetness equivalent ratio of 1:0.5–1, and optionally contains acesulfame potassium and / or sucralose, with the total amount of acesulfame potassium and sucralose not exceeding 0.008wt%. The average particle size of the calcium silicate is 5–15μm, and the BET specific surface area is 70–120m² / g.
9. A product that can provide muscle nutritional support, characterized in that: The product is prepared by the method described in any one of claims 1 to 8, and has a true porosity of ≥60%; an average bulk density of the product is 0.38–0.45 g / cm³, and a viscosity after redispersion is 20–40 mPa·s; and the product reaches a solubility greater than 90% when stirred in 230 mL of water at 15–40°C for ≤15 seconds.
10. A product capable of providing muscle nutritional support according to claim 9, characterized in that: The protein and amino acid release of this product has a "fast segment and slow segment" bimodal curve, with a cumulative release of ≥40% in 30 minutes and a cumulative release of ≥90% in 4 hours.
Citation Information
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