Instant giant salamander collagen freeze-dried ball and preparation method thereof

Abstract

The invention discloses an instant giant salamander collagen freeze-dried ball and a preparation method thereof. The freeze-dried ball comprises 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol and 30-50 parts of sodium polyglutamate. The freeze-dried ball can be combined with the giant salamander hydrolyzed collagen through electrostatic interaction or hydrogen-bond interaction by utilizing the compounding effect of the sodium polyglutamate and the mannitol, so that the giant salamander hydrolyzed collagen is prevented from being gathered, the giant salamander hydrolyzed collagen can be helped to be better dispersed in water, and meanwhile, the sodium polyglutamate has good moisture retention, water absorption and biocompatibility, so that the freeze-dried ball can be used for preparing the giant salamander hydrolyzed collagen. The mannitol can form a stable supporting structure in the freeze-drying process, so that the giant salamander hydrolyzed collagen is prevented from shrinking or deforming in the freezing and drying processes, the activity of the giant salamander hydrolyzed collagen is protected, and the mannitol can be matched with the sodium polyglutamate in the dissolving process, so that the giant salamander hydrolyzed collagen can be dissolved in the freeze-drying process; the giant salamander hydrolyzed collagen is quickly released, and the dissolving speed is increased.

Description

Technical Field

[0001] The present invention relates to the technical field of collagen freeze-dried pellets, in particular to instant-dissolving giant salamander collagen freeze-dried pellets and a preparation method thereof. Background Art

[0002] Freeze-dried collagen pellets are powdered products obtained by low-temperature drying and vacuuming collagen extracts (i.e., freeze-drying technology). Collagen components have a certain degree of hydrophilicity. Using freeze-dried collagen pellets can replenish a certain amount of collagen for the skin, which has a moisturizing effect, can maintain the skin's hydration, and has a hydrating and moisturizing effect. Collagen components can also participate in the growth and metabolism of skin cells, to a certain extent, whitening, brightening the skin tone, and improving dull skin.

[0003] Giant salamander hydrolyzed collagen is a type of enzymatically hydrolyzed collagen with a lower molecular weight, generally having better solubility and bioavailability. However, due to the wide molecular weight distribution of giant salamander hydrolyzed collagen, it may contain fragments with larger molecular weights. These large molecular fragments have poor solubility, especially the secondary structure of giant salamander hydrolyzed collagen (such as α-helix and β-fold), which affects its solubility, resulting in poor overall fast-dissolving performance.

[0004] In the prior art, a fast-soluble collagen freeze-dried ball is disclosed, which uses collagen, trehalose, pullulan, mannitol and water, wherein the collagen is acylated collagen to improve the fast solubility of collagen. However, not all collagen can be improved in water solubility through acylation. If the giant salamander hydrolyzed collagen is treated with acylation technology, its secondary structure (such as α-helix and β-fold) will be destroyed, which will eventually affect its original hydrating and moisturizing effects. Summary of the Invention

[0005] In order to overcome the deficiencies of the prior art, one of the objectives of the present invention is to provide a fast-dissolving giant salamander collagen freeze-dried pellet to solve the above-mentioned traditional technical problems.

[0006] The second object of the present invention is to provide a method for preparing the instant-soluble giant salamander collagen freeze-dried pellets, which has a simple preparation process and is easy to promote.

[0007] One of the objectives of the present invention is achieved by the following technical solution:

[0008] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0009] 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, and 30-50 parts of sodium polyglutamate.

[0010] In the present invention, the inventors discovered that by utilizing the compound effect of sodium polyglutamate and mannitol, it can be combined with giant salamander hydrolyzed collagen through electrostatic action or hydrogen bonding, preventing the aggregation of giant salamander hydrolyzed collagen and helping the giant salamander hydrolyzed collagen to be better dispersed in water. At the same time, sodium polyglutamate has good moisturizing properties, water absorption and biocompatibility, and can improve the moisturizing, skin repair and other effects of giant salamander hydrolyzed collagen. Mannitol can form a stable support structure during the freeze-drying process, preventing the giant salamander hydrolyzed collagen from shrinking or deforming during the freezing and drying process, protecting the activity of the giant salamander hydrolyzed collagen, and can cooperate with the effect of sodium polyglutamate during dissolution to quickly release the giant salamander hydrolyzed collagen and increase its dissolution rate.

[0011] Furthermore, the mass ratio of giant salamander hydrolyzed collagen, mannitol, and sodium polyglutamate is 1:(1-1.2):(2.5-3), such as the weight ratio of 10 parts:12 parts:30 parts, 12 parts:14 parts:36 parts, 15 parts:15 parts:45 parts, etc. Preferably, the mass ratio of giant salamander hydrolyzed collagen and sodium polyglutamate is 1:3.

[0012] Furthermore, the molecular weight of the giant salamander hydrolyzed collagen is 200Da-800Da, and the molecular weight of the sodium polyglutamate is 600kDa-800kDa. Appropriate molecular weights result in better solubility.

[0013] One of the purposes of the present invention is also achieved by the following technical solution:

[0014] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0015] 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, 30-50 parts of sodium polyglutamate, and 1-5 parts of black tea powder.

[0016] In the present invention, the inventors discovered that by adding a small amount of black tea powder, since the black tea powder contains acidic substances such as tea polyphenols and tannic acid, after dissolving at low temperature, the solution becomes weakly acidic, which increases the dissolution rate of giant salamander hydrolyzed collagen at low temperature and makes the system have a better instant dissolution effect. At the same time, black tea powder is rich in antioxidant ingredients, which can neutralize free radicals, reduce the damage of free radicals to skin cells, help the skin maintain elasticity, and thus improve the moisturizing effect of the system.

[0017] Furthermore, the mass ratio of giant salamander hydrolyzed collagen and black tea powder is 1:(0.1-0.2), such as 1:0.1, 1:0.12, 1:0.5, 1:0.8, 1:0.2, etc.

[0018] Furthermore, the particle size of the black tea powder is 60 μm-120 μm.

[0019] One of the purposes of the present invention is also achieved by the following technical solution:

[0020] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0021] 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, 30-50 parts of sodium polyglutamate, 1-5 parts of black tea powder, and 1-5 parts of white fungus powder.

[0022] In the present invention, the inventors found that by adding a small amount of tremella powder in combination with mannitol, sodium polyglutamate and black tea powder, the instant dissolution effect of giant salamander hydrolyzed collagen at low temperature is improved. Among them, since tremella powder can dissolve rapidly in cold water, it can better cooperate with the effects of mannitol and sodium polyglutamate, further preventing the aggregation of giant salamander hydrolyzed collagen, and can help the giant salamander hydrolyzed collagen to be better dispersed in water. The acidic substances decomposed by the black tea powder are then used to make the giant salamander hydrolyzed collagen achieve a better instant dissolution effect and increase its dissolution rate at low temperatures.

[0023] Furthermore, the mass ratio of giant salamander hydrolyzed collagen and tremella powder is 1:(0.1-0.2), such as 1:0.1, 1:0.12, 1:0.5, 1:0.8, 1:0.2, etc.

[0024] Furthermore, the molecular weight of the Tremella powder is 1000kDa-5000kDa.

[0025] The second object of the present invention is achieved by the following technical solution:

[0026] A method for preparing instant giant salamander collagen freeze-dried pellets comprises the following steps:

[0027] Add an appropriate amount of deionized water to the stirring device, then add mannitol and sodium polyglutamate respectively, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, then perform homogenization, and finally fill into a forming mold, and prepare freeze-dried balls through freeze-drying technology.

[0028] The second object of the present invention is also achieved by the following technical solution:

[0029] A method for preparing instant giant salamander collagen freeze-dried pellets comprises the following steps:

[0030] Add an appropriate amount of deionized water to the mixing equipment, then add mannitol, sodium polyglutamate and black tea powder respectively, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, then perform homogenization, and finally fill into a molding mold, and prepare freeze-dried balls through freeze-drying technology.

[0031] The second object of the present invention is also achieved by the following technical solution:

[0032] A method for preparing instant giant salamander collagen freeze-dried pellets comprises the following steps:

[0033] Add an appropriate amount of deionized water to the stirring device, then add mannitol, sodium polyglutamate, tremella powder and black tea powder respectively, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, then perform homogenization, and finally fill into a forming mold, and prepare freeze-dried balls through freeze-drying technology.

[0034] In the above preparation method, the amount of deionized water added is 2-6 times the amount of giant salamander hydrolyzed collagen, and the average particle size of the freeze-dried pellets is 100-250nm. The freeze-drying technology is as follows: the raw materials are placed in a pre-freezing device and pre-frozen at a temperature of -40°C to -60°C until the raw materials are completely frozen. The pre-frozen raw materials are placed in a freeze-drying device and heated under vacuum to sublime the ice crystals to complete the freeze-drying process. The sublimation temperature during the freeze-drying process is 20°C to 40°C, and the sublimation time is 8h to 24h.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] 1. The instant giant salamander collagen freeze-dried pellets of the present invention utilize the combined effect of sodium polyglutamate and mannitol, which can be combined with giant salamander hydrolyzed collagen through electrostatic interaction or hydrogen bonding, thereby preventing the giant salamander hydrolyzed collagen from aggregating and helping the giant salamander hydrolyzed collagen to be better dispersed in water. At the same time, sodium polyglutamate has good moisture retention, water absorption and biocompatibility, and can improve the moisture retention, skin repair and other effects of giant salamander hydrolyzed collagen. Mannitol can form a stable support structure during the freeze-drying process, preventing the giant salamander hydrolyzed collagen from shrinking or deforming during the freezing and drying process, protecting the activity of the giant salamander hydrolyzed collagen, and can cooperate with the effect of sodium polyglutamate during dissolution to quickly release the giant salamander hydrolyzed collagen and increase its dissolution rate.

[0037] 2. In the invention, the inventors were able to increase the solubility of giant salamander hydrolyzed collagen while also improving its moisturizing effect by adding black tea powder, or black tea powder and white fungus powder. DETAILED DESCRIPTION

[0038] Below, the present invention is further described in conjunction with specific embodiments. It should be noted that, under the premise of no conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments. In the following examples, giant salamander hydrolyzed collagen was purchased from Zhangjiajie (China) Niu Zhenbang Biotechnology Co., Ltd., with a molecular weight of 200Da-800Da; mannitol was purchased from Shanghai Zhongfeng Biotechnology Co., Ltd.; sodium polyglutamate was purchased from Shanxi Zhongnuo Biotechnology Co., Ltd., with a molecular weight of 600kDa-800kDa; black tea powder was purchased from Shanyang Lianfeng Biotechnology Co., Ltd., with an average particle size of 60μm-120μm; white fungus powder was purchased from Xi'an Ruierli Bioengineering Co., Ltd., with a molecular weight of 1000kDa-5000kDa.

[0039] Example 1

[0040] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0041] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, and 30 parts of sodium polyglutamate.

[0042] The preparation method thereof comprises the following preparation steps:

[0043] Add an appropriate amount of deionized water to a mixing device, then add mannitol and sodium polyglutamate respectively, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, then homogenize, and finally fill into a forming mold. Use freeze-drying technology to produce freeze-dried balls with an average particle size of 100-250 nm (crushed and sieved). The amount of deionized water added is 3 times the amount of giant salamander hydrolyzed collagen.

[0044] Example 2

[0045] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0046] 15 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, and 30 parts of sodium polyglutamate.

[0047] The preparation method is the same as that in Example 1.

[0048] Example 3

[0049] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0050] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 30 parts of sodium polyglutamate, and 2 parts of black tea powder.

[0051] The preparation method thereof comprises the following preparation steps:

[0052] Add an appropriate amount of deionized water to a mixing device, then add mannitol, sodium polyglutamate, and black tea powder, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, homogenize, and finally fill into a forming mold. Use freeze-drying technology to produce freeze-dried balls with an average particle size of 100-250 nm (crushed and sieved). The amount of deionized water added is 3 times the amount of giant salamander hydrolyzed collagen.

[0053] Example 4

[0054] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0055] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 30 parts of sodium polyglutamate, and 5 parts of black tea powder.

[0056] The preparation method is the same as that of Example 3.

[0057] Example 5

[0058] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0059] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 30 parts of sodium polyglutamate, 2 parts of black tea powder, and 2 parts of white fungus powder.

[0060] The preparation method thereof comprises the following preparation steps:

[0061] An appropriate amount of deionized water is added to a mixing device, followed by the addition of mannitol, sodium polyglutamate, tremella powder, and black tea powder, and the mixture is stirred evenly. The mixture is then added with the giant salamander hydrolyzed collagen while stirring, and the mixture is thoroughly stirred. The mixture is then homogenized and filled into a mold. The mixture is freeze-dried (crushed and sieved) to produce freeze-dried pellets having an average particle size of 100-250 nm. The amount of deionized water added is three times the amount of the giant salamander hydrolyzed collagen.

[0062] Example 6

[0063] A quick-dissolving giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0064] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 30 parts of sodium polyglutamate, 2 parts of black tea powder, and 5 parts of white fungus powder.

[0065] The preparation method is the same as that of Example 5.

[0066] Comparative Document 1

[0067] A giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0068] 10 parts of giant salamander hydrolyzed collagen, 42 parts of mannitol.

[0069] The preparation method is similar to that of Example 1.

[0070] Comparative Document 2

[0071] A giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0072] 10 parts of giant salamander hydrolyzed collagen, 42 parts of sodium polyglutamate.

[0073] The preparation method is similar to that of Example 1.

[0074] Comparative Example 3

[0075] A giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0076] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 2 parts of black tea powder.

[0077] The preparation method is similar to that of Example 3.

[0078] Comparative Example 4

[0079] A giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0080] 10 parts of giant salamander hydrolyzed collagen, 12 parts of mannitol, 2 parts of black tea powder, and 2 parts of white fungus powder.

[0081] The preparation method is similar to that of Example 5.

[0082] Comparative Example 5

[0083] A giant salamander collagen freeze-dried pellet comprising the following components in parts by weight:

[0084] 10 parts of giant salamander hydrolyzed collagen, 30 parts of sodium polyglutamate, 2 parts of black tea powder, and 2 parts of white fungus powder.

[0085] The preparation method is similar to that of Example 5.

[0086] Performance Testing

[0087] 1. Test objects: Examples 1-6, Comparative Examples 1-5.

[0088] 2. Solubility test

[0089] (1) Room temperature test: Add 10 mg of sample to 100 mL of water at room temperature and let it stand until it dissolves. During this process, record the time required for complete dissolution.

[0090] (2) Medium temperature test: 10 mg of sample was added to 100 mL of water at 40 °C and allowed to stand until it dissolved. During this process, the time required for complete dissolution was recorded.

[0091] The test results are shown in Table 1.

[0092] Table 1

[0093] project Normal temperature test Medium temperature test Example 1 15s 9s Example 2 19s 12s Example 3 12s 7s Example 4 13s 8s Example 5 10s 5s Example 6 11s 6s Comparative Example 1 56s 47s Comparative Example 2 52s 40s Comparative Example 3 48s 37s Comparative Example 4 42s 33s Comparative Example 5 31s 24s

[0094] As can be seen from the above table, the instant dissolution time of the freeze-dried balls of Examples 1-6 of the present invention does not exceed 20 seconds, and the fastest dissolution speed is 5 seconds.

[0095] 3. Moisturizing effect test

[0096] The moisturizing properties of the samples were tested with reference to the "Guidelines for the Evaluation of Moisturizing Efficacy of Cosmetics". 55 volunteers aged 18-30 were selected as test subjects. The test subjects were divided into 11 groups, with 5 subjects in each group. The subjects washed their faces with facial cleanser and let them dry naturally. A 4cm*4cm application area was marked symmetrically on the left and right sides of the face. The test sample was applied at a concentration of 2mg / cm 2 The dosage was applied once with a latex fingertip and tested with Corneometer CM825. The test was conducted once before use and once 15 minutes, 1 hour, 2 hours, and 4 hours after use. Each area was measured in parallel 3 times each time, and the average value was taken to calculate the water retention difference = water retention value at each time point after use of the product - water retention value before use of the product (for convenience of calculation and comparison, the water retention value before the test was taken as 0). The test results are shown in Table 2.

[0097] Table 2

[0098] project Before the test 15min 1h 2h 4h Example 1 0 30.2 29.6 21.3 19.2 Example 2 0 30.1 28.8 20.4 18.9 Example 3 0 30.8 30.1 25.5 22.1 Example 4 0 30.5 29.8 24.3 21.5 Example 5 0 31.3 30.8 26.6 23.2 Example 6 0 31.0 30.1 26.1 22.9 Comparative Example 1 0 20.6 16.5 10.3 5.9 Comparative Example 2 0 23.5 18.7 15.4 12.5 Comparative Example 3 0 22.3 17.2 13.5 10.5 Comparative Example 4 0 22.5 17.8 14.2 10.9 Comparative Example 5 0 24.0 20.1 16.5 13.4

[0099] As can be seen from the above table, compared with the comparative example, the freeze-dried balls of Examples 1-6 of the present invention have better moisturizing effects.

[0100] The above embodiments are only preferred embodiments of the present invention and cannot be used to limit the scope of protection of the present invention. Any non-substantial changes and replacements made by technicians in this field on the basis of the present invention fall within the scope of protection required by the present invention.

Claims

1. A fast-dissolving giant salamander collagen freeze-dried pellet, characterized in that: The composition comprises the following components in parts by weight: 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, and 30-50 parts of sodium polyglutamate.

2. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 1, characterized in that: The mass ratio of the giant salamander hydrolyzed collagen, mannitol and sodium polyglutamate is 1:(1-1.2):(2.5-3).

3. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 2, characterized in that: The mass ratio of the giant salamander hydrolyzed collagen to sodium polyglutamate is 1:

3.

4. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 1, characterized in that: The molecular weight of the giant salamander hydrolyzed collagen is 200Da-800Da, and the molecular weight of the sodium polyglutamate is 600kDa-800kDa.

5. A fast-dissolving giant salamander collagen freeze-dried pellet, characterized in that: The composition comprises the following components in parts by weight: 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, 30-50 parts of sodium polyglutamate, and 1-5 parts of black tea powder.

6. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 5, characterized in that: The mass ratio of the giant salamander hydrolyzed collagen to the black tea powder is 1:(0.1-0.2).

7. A fast-dissolving giant salamander collagen freeze-dried pellet, characterized in that: The composition comprises the following components in parts by weight: 10-20 parts of giant salamander hydrolyzed collagen, 10-15 parts of mannitol, 30-50 parts of sodium polyglutamate, 1-5 parts of black tea powder, and 1-5 parts of white fungus powder.

8. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 7, characterized in that: The mass ratio of the giant salamander hydrolyzed collagen to the tremella powder is 1:(0.1-0.2).

9. The instant-dissolving giant salamander collagen freeze-dried pellet according to claim 7, characterized in that: The molecular weight of the tremella powder is 1000kDa-5000kDa.

10. A method for preparing the instant-soluble giant salamander collagen freeze-dried pellets according to any one of claims 1 to 4, characterized in that: The method comprises the following preparation steps: Add an appropriate amount of deionized water to the stirring device, then add mannitol and sodium polyglutamate respectively, stir evenly, then add giant salamander hydrolyzed collagen while stirring, stir thoroughly, then perform homogenization, and finally fill into a forming mold, and prepare freeze-dried balls through freeze-drying technology.