A method for improving the stability of a product containing calcium beta-hydroxy-beta-methylbutyrate and protein

Abstract

The application discloses a method for improving the stability of a product containing calcium beta-hydroxy-beta-methylbutyrate and protein, and relates to the technical field of functional food. The preparation method comprises the following steps: mixing the protein with water to obtain a first emulsion; mixing a first buffer solution with a calcium beta-hydroxy-beta-methylbutyrate composition to obtain an HMB-Ca solution; mixing the HMB-Ca solution and the first emulsion, and adding a second buffer solution after complete dispersion, so as to adjust the pH of the system to 6.0-6.3; and the calcium beta-hydroxy-beta-methylbutyrate composition comprises calcium beta-hydroxy-beta-methylbutyrate and calcium caseinate. The application can optimize the particle size and surface charge state, reduce the precipitation of the protein product when the protein product is subjected to brewing or heating at a temperature of more than 90 DEG C, and improve the high-temperature stability of the product.

Description

Technical Field

[0001] This invention relates to the field of functional food technology, and more specifically to a method for improving the stability of products containing calcium β-hydroxy-β-methylbutyrate and protein. Background Technology

[0002] The core function of calcium β-hydroxy-β-methylbutyrate is to promote muscle synthesis, accelerate exercise recovery, reduce muscle damage, and inhibit muscle breakdown. Clinically, it is often used to treat sarcopenia in the elderly and in postoperative recovery patients. It is usually taken in conjunction with high-protein products such as protein powder and milk powder.

[0003] However, when calcium β-hydroxy-β-methylbutyrate is combined with protein-based raw materials, especially when users frequently use high-temperature water (above 90°C) for brewing, it will cause precipitation in the system, which will greatly affect the application of calcium β-hydroxy-β-methylbutyrate in terms of product stability and taste.

[0004] Chinese patent CN114568515A discloses a method for preparing a protein solution containing calcium β-hydroxy-β-methylbutyrate, comprising the following steps: Step 1: Add milk powder to 50℃ warm water to prepare milk powder solution. The milk powder is selected from one or more of whole milk powder, skim milk powder, whey protein powder, and whey powder, with or without added nutritional fortifiers or food additives. Step 2: Add the calcium β-hydroxy-β-methylbutyrate raw material to room temperature water to prepare an aqueous solution of calcium β-hydroxy-β-methylbutyrate; Step 3: Add an organic acid to the aqueous solution of calcium β-hydroxy-β-methylbutyrate prepared in Step 2 to adjust the pH value of the aqueous solution of calcium β-hydroxy-β-methylbutyrate to 6.7-6.9. The organic acid is selected from one or more of citric acid, malic acid, lactic acid, tartaric acid, and ascorbic acid. Step 4: Add the aqueous solution of calcium β-hydroxy-β-methylbutyrate prepared in Step 3 to the milk powder solution prepared in Step 1.

[0005] However, when prepared according to the method of this patent, a large amount of precipitate is generated at 95°C, and the high-temperature stability is poor.

[0006] Chinese patent CN116098292A discloses a method for improving the storage stability of emulsions containing calcium β-hydroxy-β-methylbutyrate, comprising the following steps: (1) Prepare a whey protein solution by weight ratio of whey protein to water of 2:100-6:100; (2) Prepare a maltodextrin solution with a weight ratio of maltodextrin to water of 10:100-20:100; (3) Prepare a composite solution of casein phosphopeptide and calcium β-hydroxy-β-methylbutyrate at a weight ratio of 1:5 to 1:45, wherein the concentration of calcium β-hydroxy-β-methylbutyrate in the composite solution is 1 mol / L. (4) Mix whey protein solution, maltodextrin solution, casein phosphopeptide and calcium β-hydroxy-β-methylbutyrate in a volume ratio of 10:10:1 as the aqueous phase, add oil phase, disperse at high speed, and then sterilize under high pressure to obtain calcium-fortified emulsion.

[0007] This patent improves the storage stability of emulsions containing calcium β-hydroxy-β-methylbutyrate by adding casein phosphopeptide. However, adding casein phosphopeptide does not improve its high-temperature stability. A large amount of precipitation occurs at 95°C, indicating poor high-temperature stability.

[0008] Therefore, there is an urgent need in this field for a protein product containing calcium β-hydroxy-β-methylbutyrate that can withstand high temperatures. Summary of the Invention

[0009] In view of this, the purpose of the present invention is to provide a method for improving the stability of products containing calcium β-hydroxy-β-methylbutyrate and protein. By using a specific mass ratio of calcium β-hydroxy-β-methylbutyrate and calcium caseinate, and adjusting the pH to 6-6.3, the particle size and surface charge state can be optimized, reducing precipitation of protein products when brewed or heated at temperatures above 90°C, and improving the high-temperature stability of the product.

[0010] To achieve the above-mentioned objectives, the technical solution of the present invention is as follows: In a first aspect, the present invention provides: a method for improving the stability of a product containing calcium β-hydroxy-β-methylbutyrate and protein, comprising the following steps: The protein is mixed with water to obtain a first emulsion; The first buffer solution was mixed with the calcium β-hydroxy-β-methylbutyrate composition to obtain the HMB-Ca solution; The HMB-Ca solution and the first emulsion were mixed and completely dispersed. Then, a second buffer solution was added to adjust the pH of the system to 6.0-6.3. The calcium β-hydroxy-β-methylbutyrate composition comprises calcium β-hydroxy-β-methylbutyrate and calcium caseinate.

[0011] In some embodiments, the first emulsion is a 20-30 wt% protein solution.

[0012] Preferably, the first emulsion is a protein solution of 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, 25wt%, 26wt%, 27wt%, 28wt%, 29wt%, or 30wt%, or any combination thereof.

[0013] In some embodiments, the protein is mixed with water at a temperature of 30-41°C.

[0014] Preferably, the temperature at which the protein is mixed with water is 30°C, 31°C, 32°C, 33°C, 34°C, 35°C, 36°C, 37°C, 38°C, 39°C, 40°C, 41°C, or any combination thereof.

[0015] In some implementations, the pH of the first buffer solution is 6.0-6.3.

[0016] In some embodiments, the first buffer solution is a citric acid-citrate solution.

[0017] Preferably, the pH of the first buffer solution is 6.0, 6.1, 6.2, 6.3, or any combination thereof; In some embodiments, the concentration of the calcium β-hydroxy-β-methylbutyrate composition in the HMB-Ca solution is 45-55 wt%.

[0018] Preferably, the concentration of the calcium β-hydroxy-β-methylbutyrate composition in the HMB-Ca solution is 45wt%, 46wt%, 47wt%, 48wt%, 49wt%, 50wt%, 51wt%, 52wt%, 53wt%, 54wt%, 55wt%, or any combination thereof.

[0019] In some embodiments, the mass ratio of the calcium β-hydroxy-β-methylbutyrate to the calcium caseinate is (3-7):(0.5-1).

[0020] Preferably, the mass ratio of calcium β-hydroxy-β-methylbutyrate to calcium caseinate is 3:0.5, 3:1, 4:0.5, 4:1, 5:0.5, 5:1, 6:0.5, 6:1, 7:0.5, 7:1, 10:1, or any combination thereof.

[0021] In some embodiments, the pH of the second buffer solution is 14-15.

[0022] In some embodiments, the second buffer solution is a 40 wt% aqueous solution of potassium hydroxide or a 40 wt% aqueous solution of sodium hydroxide.

[0023] Preferably, the pH of the second buffer solution is 14, 14.1, 14.2, 14.3, 14.4, 14.5, 14.6, 14.7, 14.8, 14.9, 15, or any combination thereof.

[0024] In some embodiments, the pH of the adjustment system is 6.0, 6.1, 6.2, 6.3, or a range of any two thereof.

[0025] In some embodiments, the mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to the protein is (3.5-8):(75-130).

[0026] Preferably, the mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to the protein is 3.5:75, 3.5:130, 4:75, 4:130, 5:75, 5:130, 6:75, 6:100, 6:130, 7:75, 7:130, 8:75, 8:130, or any combination thereof.

[0027] In some embodiments, the product includes powders and emulsions.

[0028] Preferably, when the product is a powder, the method further includes: shear emulsification, homogenization, and drying.

[0029] More preferably, the drying is spray drying.

[0030] More preferably, the inlet air temperature of the spray dryer is 143-148°C, and the temperature inside the tower is 93-97°C.

[0031] Preferably, when the product is an emulsion, the preparation method further includes: shear emulsification and homogenization.

[0032] In some embodiments, the product includes: protein and excipients.

[0033] In some embodiments, the protein includes at least one of plant protein, animal protein, and microbial protein.

[0034] Preferably, the protein includes at least one of soy protein isolate, yeast protein, whey protein concentrate, whey protein isolate, and α-lactalbumin.

[0035] In some embodiments, the product further includes at least one of a nutrient fortifier, carbohydrates, fillers, thickeners, stabilizers, sweeteners, and flavoring agents.

[0036] Preferably, the stabilizer includes at least one of xanthan gum, polydextrose, maltodextrin, sodium carboxymethyl cellulose, guar gum, konjac flour, and psyllium husk powder.

[0037] Secondly, the present invention provides the application of calcium β-hydroxy-β-methylbutyrate and calcium caseinate in combination to improve the stability of protein products; The method for preparing the protein product includes the following steps: The protein is mixed with water to obtain a first emulsion; The first buffer solution was mixed with the calcium β-hydroxy-β-methylbutyrate composition to obtain the HMB-Ca solution; The HMB-Ca solution and the first emulsion were mixed and completely dispersed. Then, a second buffer solution was added to adjust the pH of the system to 6.0-6.3. The calcium β-hydroxy-β-methylbutyrate composition comprises calcium β-hydroxy-β-methylbutyrate and calcium caseinate.

[0038] Beneficial effects: This invention uses a specific mass ratio of calcium β-hydroxy-β-methylbutyrate and calcium caseinate, and adjusts the pH to 6-6.3 to solve the technical problem of protein precipitation caused by calcium β-hydroxy-β-methylbutyrate. Furthermore, it can reduce precipitation and improve the high-temperature stability of the product when brewed or heated at temperatures above 95°C. Detailed Implementation

[0039] To make the technical means, creative features, and achieved objectives and effects of this invention easier to understand, the invention is further illustrated below with specific embodiments. However, the following embodiments are only preferred embodiments of this invention and not all embodiments. Other embodiments obtained by those skilled in the art based on the embodiments described herein without creative effort are all within the protection scope of this invention. In the following embodiments, unless otherwise specified, the operating methods used are conventional operating methods, the equipment used is conventional equipment, and the equipment and materials used in each embodiment are the same.

[0040] The CaHMB described in this invention is: calcium β-hydroxy-β-methylbutyrate.

[0041] In the following embodiments, some of the raw materials are sourced from the sources shown in Table 1.

[0042] Table 1

[0043] Example 1 (1) Prepare a citric acid-potassium citrate aqueous solution with pH 6.3 using production water to obtain the first buffer solution, and prepare a 40wt% potassium hydroxide aqueous solution to obtain the second buffer solution (pH=15).

[0044] (2) Prepare a 25wt% solution of soy protein isolate powder with water at 36℃ and stir thoroughly (600rpm, 10min) to obtain a first emulsion that is free of particles, insoluble matter and wall adhesion.

[0045] (3) Prepare a 50wt% solution of calcium β-hydroxy-β-methylbutyrate composition using the first buffer solution to obtain HMB-Ca solution; the calcium β-hydroxy-β-methylbutyrate composition is calcium β-hydroxy-β-methylbutyrate and calcium caseinate in a mass ratio of 10:1; the mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to soybean protein isolate powder is 6:100.

[0046] (4) Add HMB-Ca solution to the first emulsion and stir (500 rpm). After complete dispersion, adjust the pH of the system to 6.3 using the second buffer solution.

[0047] (5) Add 2.5wt% xanthan gum and polydextrose (mass ratio 1:2) of non-aqueous raw materials, and then continue stirring (600rpm, 10min) until there are no particles, no insoluble matter, and no sticking to the wall. Then emulsify at high speed for 5min and homogenize (pressure 20MPa, 33±5℃).

[0048] (6) Spray drying in the upper tower (inlet air temperature 145℃, tower temperature 95℃) to obtain the finished product (powder).

[0049] Example 2 (1) Prepare a citric acid-potassium citrate aqueous solution with pH 6 using production water to obtain the first buffer solution, and prepare a 40wt% potassium hydroxide aqueous solution to obtain the second buffer solution (pH=15).

[0050] (2) Prepare a 20wt% solution of protein (concentrated whey protein powder) with production water at 30℃ and stir thoroughly (600rpm, 10min) to obtain a first emulsion without particles, insoluble matter, or wall adhesion.

[0051] (3) Prepare a 45wt% solution of calcium β-hydroxy-β-methylbutyrate composition using the first buffer solution to obtain HMB-Ca solution; the calcium β-hydroxy-β-methylbutyrate composition is calcium β-hydroxy-β-methylbutyrate and calcium caseinate in a mass ratio of 3:1; the mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to the protein is 3.5:130.

[0052] (4) Add HMB-Ca solution to the first emulsion and stir (500 rpm). After complete dispersion, adjust the pH of the system to 6 using the second buffer solution.

[0053] (5) Add 1 wt% xanthan gum and polydextrose (mass ratio 1:4) of non-aqueous raw materials, and then continue stirring (600 rpm, 10 min) until there are no particles, no insoluble matter, and no sticking to the wall. Then emulsify at high speed for 5 min and homogenize (pressure 20 MPa, 33 ± 5 ℃).

[0054] (6) Spray drying in the upper tower (inlet air temperature 143℃, tower temperature 97℃) to obtain the finished product (powder).

[0055] Example 3 (1) Prepare a citric acid-potassium citrate aqueous solution with pH 6 using production water to obtain the first buffer solution, and prepare a 40wt% potassium hydroxide aqueous solution to obtain the second buffer solution (pH=15).

[0056] (2) Prepare a 30wt% solution of yeast protein powder with production water at 41℃ and stir thoroughly (600rpm, 10min) to obtain a first emulsion without particles, insoluble matter, or wall adhesion.

[0057] (3) Prepare a 55wt% solution of calcium β-hydroxy-β-methylbutyrate composition using the first buffer solution to obtain HMB-Ca solution; the calcium β-hydroxy-β-methylbutyrate composition is calcium β-hydroxy-β-methylbutyrate and calcium caseinate in a mass ratio of 7:0.5; the mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to the protein is 8:75.

[0058] (4) Add HMB-Ca solution to the first emulsion and stir (500 rpm). After complete dispersion, adjust the pH of the system to 6 using the second buffer solution.

[0059] (5) Add 5 wt% xanthan gum and polydextrose (mass ratio 1:1) of non-aqueous raw materials, and then continue stirring (600 rpm, 10 min) until there are no particles, no insoluble matter, and no sticking to the wall. Then emulsify at high speed for 5 min and homogenize (pressure 20 MPa, 33±5℃) to obtain (emulsion).

[0060] Comparative Example 1 The difference from Example 1 is that the pH of the citric acid-potassium citrate aqueous solution is 6.6, and step (4) adjusts the pH of the system to 6.6 by using a second buffer solution.

[0061] Comparative Example 2 The difference from Example 1 is that the mass ratio of calcium β-hydroxy-β-methylbutyrate to calcium caseinate is 2.5:1.2.

[0062] Comparative Example 3 The difference from Example 1 is that calcium caseinate is replaced with an equal mass of casein phosphopeptide.

[0063] Comparative Example 4 The preparation was carried out according to the preparation method of Example 1 of Chinese Patent CN114568515A.

[0064] Test Example 1: Stability Test Sample group: Examples 1-3 and Comparative Examples 1-4 were prepared into solutions with a protein concentration of 10 wt%.

[0065] Blank group 1: A solution with a soy protein isolate concentration of 10 wt%.

[0066] Blank group 2: A solution of concentrated whey protein with a concentration of 10 wt%.

[0067] Blank group 3: A solution with a yeast protein concentration of 10 wt%.

[0068] Experimental method: Both the blank group and the sample group were heated at 95℃ for 30 minutes, centrifuged and the precipitate was collected. The difference in precipitate after drying was the mass of protein precipitation caused by CaHMB (3 parallel experiments for each group).

[0069] The difference in precipitation after drying is the precipitation mass of Examples 1-3 and Comparative Examples 1-4 minus the precipitation mass of the corresponding protein blank group.

[0070] The experimental results are shown in Table 2.

[0071] Table 2

[0072] The precipitation difference can reflect the degree of protein precipitation at 95℃. As shown in Table 2, under the conditions of pH 6.0-6.3 and a specific ratio of calcium β-hydroxy-β-methylbutyrate to calcium caseinate, the precipitation difference in Examples 1-3 is low, which is significantly better than that in Comparative Example 1 where the pH deviates from the target range, Comparative Example 2 where the composition ratio is inappropriate, Comparative Example 3 where casein phosphopeptide is replaced, and Comparative Example 4 of the prior art. This shows that controlling both pH and composition ratio can significantly improve the system's high-temperature anti-precipitation ability.

[0073] Example 2: Particle size and potential determination The particle size of the samples was determined using a Malvern high-sensitivity nanoparticle potentiometer, specifically a Zetasizer Nano S90 (Malvern Panaco, UK, Shanghai).

[0074] Solutions of Examples 1-3 and Comparative Examples 1-4 were prepared with a solid content concentration of 0.1 mg / mL, heated at 95°C for half an hour, filtered through a 0.45 μm filter membrane, and after the filtrate cooled to room temperature, the particle size and potential of the filtrate were measured. The test environment was room temperature (25°C) throughout the test.

[0075] The experimental results are shown in Table 3.

[0076] Table 3

[0077] As can be seen from the particle size and potential data in Table 3, the particle size distribution of Examples 1-3 is between 289.6 nm and 349.3 nm, and the Zeta potential distribution is between -33.13 and -22.66 mV, indicating that the protein products prepared by the present invention also have moderate particle size and surface charge after high-temperature heating.

[0078] After being heated at 95°C for half an hour, compared to Comparative Example 1 3. In Example 1, the particle size was smaller and the absolute value of the negative Zeta potential was higher, indicating that the particle dispersion of the system was better and the electrostatic repulsion was stronger, which could inhibit particle aggregation and precipitation.

[0079] The protein species in Comparative Example 4 are different from those in Example 1 and Comparative Examples 1-3, but are closer to those in Example 2. Compared with Example 2, Comparative Example 4 has a larger particle size, a lower absolute value of the negative Zeta potential, and decreased stability.

[0080] This invention optimizes particle size and surface charge state by precisely controlling the pH of the system at 6.0-6.3 and synergizing calcium β-hydroxy-β-methylbutyrate and calcium caseinate in a specific mass ratio, thereby significantly improving the stability of protein products under brewing or heating conditions above 90°C.

[0081] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for improving the stability of products containing calcium β-hydroxy-β-methylbutyrate and protein, characterized in that, Includes the following steps: The protein is mixed with water to obtain a first emulsion; The first buffer solution was mixed with the calcium β-hydroxy-β-methylbutyrate composition to obtain the HMB-Ca solution; The HMB-Ca solution and the first emulsion were mixed and completely dispersed. Then, a second buffer solution was added to adjust the pH of the system to 6.0-6.

3. The calcium β-hydroxy-β-methylbutyrate composition comprises calcium β-hydroxy-β-methylbutyrate and calcium caseinate.

2. The method according to claim 1, characterized in that, The first emulsion is a 20-30 wt% protein solution; The pH of the first buffer solution is 6.0-6.3; The pH of the second buffer solution is 14-15; The first buffer solution is an aqueous solution of citric acid and potassium citrate; The second buffer solution is a 40 wt% potassium hydroxide aqueous solution or a 40 wt% sodium hydroxide aqueous solution.

3. The method according to claim 1, characterized in that, The protein is mixed with water at a temperature of 30-41°C.

4. The method according to claim 1, characterized in that, The concentration of the calcium β-hydroxy-β-methylbutyrate composition in the HMB-Ca solution is 45-55 wt%.

5. The method according to claim 1, characterized in that, The mass ratio of the calcium β-hydroxy-β-methylbutyrate to the calcium caseinate is (3-7):(0.5-1). The mass ratio of the calcium β-hydroxy-β-methylbutyrate composition to the protein is (3.5-8):(75-130).

6. The method according to claim 1, characterized in that, The product is in the form of powder or emulsion.

7. The method according to claim 1, characterized in that, The protein includes at least one of plant protein, animal protein, and microbial protein.

8. The method according to claim 1, characterized in that, The protein includes at least one of soy protein isolate, yeast protein, whey protein concentrate, whey protein isolate, and α-lactalbumin.

9. The method according to claim 1, characterized in that, The product also includes at least one of the following: nutritional fortifiers, carbohydrates, fillers, thickeners, stabilizers, sweeteners, and flavorings.

10. The application of calcium β-hydroxy-β-methylbutyrate and calcium caseinate in combination for improving the stability of protein products, characterized in that, The method for preparing the protein product includes the following steps: The protein is mixed with water to obtain a first emulsion; The first buffer solution was mixed with the calcium β-hydroxy-β-methylbutyrate composition to obtain the HMB-Ca solution; The HMB-Ca solution and the first emulsion were mixed and completely dispersed. Then, a second buffer solution was added to adjust the pH of the system to 6.0-6.

3. The calcium β-hydroxy-β-methylbutyrate composition comprises calcium β-hydroxy-β-methylbutyrate and calcium caseinate.

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