CN115104688A - Liquid preparation of non-denatured II type collagen and preparation method thereof - Google Patents
Liquid preparation of non-denatured II type collagen and preparation method thereof Download PDFInfo
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- CN115104688A CN115104688A CN202110284358.1A CN202110284358A CN115104688A CN 115104688 A CN115104688 A CN 115104688A CN 202110284358 A CN202110284358 A CN 202110284358A CN 115104688 A CN115104688 A CN 115104688A
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- 108010041390 Collagen Type II Proteins 0.000 claims abstract description 91
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Images
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/62—Clouding agents; Agents to improve the cloud-stability
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
- A23L33/18—Peptides; Protein hydrolysates
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Mycology (AREA)
- Molecular Biology (AREA)
- Non-Alcoholic Beverages (AREA)
Abstract
The invention discloses a liquid preparation of non-denatured type II collagen and a preparation method thereof, belonging to the technical field of food processing. The liquid preparation is a colloidal suspension or a suspension type solid beverage which can be prepared into the colloidal suspension by adopting water with the temperature of below 35 ℃; the colloidal suspension is uniform and transparent, the suspension stability is kept for at least 30 days, and the colloidal suspension can be kept stable under the condition of pH 3-7. The non-denatured type II collagen-containing suspension type solid beverage prepared by the invention can be prepared by cold water, avoids the denaturation of non-denatured type II collagen caused by high temperature, keeps the functional activity of the non-denatured type II collagen to the maximum extent, increases the application range of the non-denatured type II collagen in the field of foods, and fills the gap that tablets or capsules can be only produced aiming at non-denatured type II collagen products in the field of health foods without other types of products.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a liquid preparation of non-denatured type II collagen and a preparation method thereof.
Background
The non-denatured type II collagen has a secondary structure of triple helix composed of three peptide chains, amino acids in each chain are bonded together through peptide bonds, and the three peptide chains are maintained in the triple helix structure through hydrogen bonds, dipole-dipole bonds, ionic bonds and van der Waals force interaction. However, the triple-helix structure of the non-denatured type II collagen is very susceptible to internal or external factors, for example, the environmental temperature is higher than 35 ℃, which can lead to the continuous weakening of hydrogen bonds between three peptide chains of the non-denatured type II collagen, the reduction of the helicity of the peptide chains, the gradual straightening and unwinding of the helicity, the increase of the disorder of the whole protein structure, and the obvious reduction of the bioactivity of the denatured type II collagen.
Non-denatured type II collagen is an indispensable collagen component in articular cartilage, and plays an essential role in the development and maturation of chondrocytes. Meanwhile, clinical tests have been reported in pathological researches on rheumatoid arthritis and osteoarthritis and in the aspect of oral rheumatoid arthritis treatment, and the oral rheumatoid arthritis treatment has great development and application potential in prevention and treatment of rheumatoid arthritis and osteoarthritis.
Although the non-denatured type II collagen has high physiological activity, the specific dense fibrous structure of the non-denatured type II collagen results in insolubility in water and low denaturation temperature, which limits the application of the non-denatured type II collagen in the fields of food and health food.
In recent years, studies on non-denatured type II collagen have been increasing, but studies on extraction processes have been focused on, and studies on the application of non-denatured type II collagen that is hardly soluble in water have been small. In the prior art, chewing type or tablet type products containing type II collagen are not beneficial to old people to take, and cannot be applied to cold chain foods such as live bacteria type yoghourt, fruit juice, jelly and the like, so that the functionality of improving the health of knee joints by the foods is increased.
Therefore, it is highly desirable to provide a colloidal suspension of non-denatured type II collagen and a solid granular beverage that can be taken with low temperature water and maintains the activity of type II collagen, which fills the gap in the field of health food that only tablets or capsules can be produced for non-denatured type II collagen products without other types of products.
Disclosure of Invention
In order to solve the above problems, the present invention provides a liquid preparation of non-denatured type II collagen, which is a colloidal suspension or a suspension type solid beverage that can be reconstituted into a colloidal suspension with water at 35 ℃ or lower.
The colloidal suspension is uniform and transparent, the suspension stability can be maintained for at least 30 days, and the colloidal suspension can be kept stable under the condition of pH 3-7.
The colloidal suspension consists of the following raw materials: 2-10 parts of non-denatured II type collagen powder, 1-5 parts of hydrophilic colloid, 1-3 parts of oligosaccharide, 1-5 parts of hydrolyzed II type collagen, and the balance of water to 100 parts.
The suspension type solid beverage is prepared from the following raw materials: 25-70 parts of the colloidal suspension of claim 2, from which water has been removed; 10-20 parts of fish collagen peptide, 5-10 parts of sea buckthorn powder, 0-10 parts of citric acid, 0-5 parts of vitamin C, 0-3 parts of sodium citrate, 0.1-1 parts of turmeric and 0-1 part of essence.
The suspension type solid beverage is prepared from the following raw materials: 5-30 parts of hydrophilic colloid, 10-15 parts of non-denatured II type collagen powder, 0-15 parts of oligosaccharide, 10-20 parts of fish collagen peptide, 10-20 parts of hydrolyzed II type collagen, 5-10 parts of sea buckthorn powder, 0-10 parts of citric acid, 0-5 parts of vitamin C, 0-3 parts of sodium citrate, 0.1-1 part of turmeric and 0-1 part of essence.
The hydrophilic colloid is one or more of xanthan gum, carrageenan, gellan gum, konjac gum, pectin, sodium alginate or sodium carboxymethylcellulose;
the oligosaccharide is one or more of inulin, fructo-oligosaccharide, malto-oligosaccharide and xylo-oligosaccharide.
A method of preparing a colloidal suspension comprising the steps of:
a. preparing materials: adding non-denatured type II collagen powder, oligosaccharide and hydrolyzed type II collagen into sterile water according to the proportion, and shearing and dispersing for 10-60min under the condition of 3000 plus 5000rpm to obtain crude dispersion;
b. high-pressure homogenization: allowing the coarse dispersion solution to enter a high-pressure homogenizer, and circulating for 2-5 times under homogenizing pressure of 20-60 MPa to obtain dispersion solution, wherein the temperature is controlled at 18-28 deg.C;
c. sol: adding hydrophilic colloid into hot water with the temperature of more than 80 ℃ according to the material-liquid ratio of 1:50-1:100, shearing for 5-30min under the condition of 3000-;
d. mixing: uniformly mixing the dispersion liquid in the step b with the colloidal solution in the step c to obtain a mixed liquid;
e. high-pressure micro-jet homogenization: homogenizing the mixed solution in a high-pressure micro-jet homogenizer at 80-150MPa for 1-3 times, and controlling the temperature at 28-38 deg.C to obtain suspension;
f. cooling and standing: standing the suspension, and cooling to obtain gel;
g. shearing the gel: the gel was dispersed by shearing at 1000-5000rpm to obtain a colloidal suspension.
A preparation method of a suspension type solid beverage comprises the following steps:
1) freeze drying the colloidal suspension of claim 1 at a pre-freezing temperature of-80 ℃ to-20 ℃, for a drying time of 24-72h, for a crushing time of 5-15min, at an impact speed of 10-20 times s -1 The crushing temperature is controlled at 5-18 ℃, and a product with the average grain diameter smaller than 40 mu m and the water removed from the colloidal suspension is obtained, namely the non-denatured II type collagen colloidal suspension freeze-dried powder;
2) weighing the freeze-dried powder of the colloidal suspension and the raw materials in the step 1) according to the proportion, and gradually mixing the freeze-dried powder and the raw materials in a gradient manner from light weight to heavy weight, so that the mixing degree is more uniform; and (3) after fully and uniformly mixing, subpackaging by using a composite film under an aseptic environment to obtain the suspension type solid beverage.
A preparation method of a suspension type solid beverage comprises the following steps:
1) weighing raw materials of fish collagen peptide, sea buckthorn powder, citric acid, vitamin C, sodium citrate, turmeric and essence according to a ratio, fully and uniformly mixing, adding the mixture into the colloidal suspension of claim 1, and uniformly stirring to obtain a mixed solution;
2) freeze drying the mixed solution of step 1) at-60 deg.C for 24-72 hr, pulverizing for 5-15min at impact speed of 10-20 times s -1 And the crushing temperature is controlled to be 5-18 ℃, and the crushed solid beverage is subpackaged by a composite membrane in a sterile environment to obtain the suspension type solid beverage.
A preparation method of a suspension type solid beverage comprises the following steps:
1) mixing the non-denatured II type collagen powder and the hydrophilic colloid according to the mass ratio of 1:9-9:1, and crushing for 15-120min at the rotation speed of 100-500r/min and the crushing temperature of 5-18 ℃ to prepare non-denatured II type collagen/hydrophilic colloid composite powder with the average particle size of less than 40 mu m;
2) weighing the non-denatured type II collagen/hydrocolloid containing composite powder and the rest raw materials according to the proportion, mixing the raw materials in a gradient manner from light to heavy step by step, fully mixing the raw materials uniformly, and subpackaging the mixture by using a composite membrane in an aseptic environment to obtain the suspended solid beverage.
The invention has the beneficial effects that:
1. the colloid suspension containing the non-denatured type II collagen prepared by the invention is uniform and transparent, and has good suspension stability; the suspended solid beverage containing non-denatured type II collagen can be brewed with cold water below 35 ℃, avoids thermal denaturation of type II collagen caused by temperature above 35 ℃, has good instant property and suspension property, fresh taste and rich nutrition, has excellent health-care components, and is beneficial to bone and joint health.
2. The colloidal suspension containing the non-denatured type II collagen prepared by the invention can stably suspend, uniformly and transparently the water-insoluble non-denatured type II collagen, and improves the suspension property of the non-denatured type II collagen.
3. The non-denatured II type collagen-containing suspension type solid beverage prepared by the invention has good flavor, instant property and suspension stability, has certain health-care components, and is beneficial to bone joint health.
4. The suspension type solid beverage containing the non-denatured type II collagen prepared by the invention can be prepared by cold water, avoids the denaturation of the non-denatured type II collagen caused by high temperature, keeps the functional activity of the non-denatured type II collagen to the maximum extent, increases the application range of the non-denatured type II collagen in the field of food, fills the blank that the non-denatured type II collagen product in the field of health food can only be used for producing tablets or capsules without other types of products, and widens the application range of the non-denatured type II collagen.
Drawings
FIG. 1 is a brewing condition of a non-denatured type II collagen-containing suspension type solid beverage prepared in example 2;
FIG. 2 shows the reconstitution of a non-denatured type II collagen-containing suspension-type solid beverage prepared in example 3;
FIG. 3 is a reconstitution of a non-denatured type II collagen-containing suspension type solid beverage prepared in example 4;
FIGS. 4-a, 4-b, 4-c and 4-d are graphs showing the variation of the backscattered light intensity with time of the colloidal suspension containing non-denatured type II collagen measured by Turbiscan Lab in example 5 and a control group, respectively;
FIG. 5 is a graph of TSI values over time for the non-denatured type II collagen-containing colloidal suspension and control of example 5;
FIG. 6 is a graph showing the particle size distributions of the colloidal suspension containing non-denatured type II collagen of example 5 and a control group;
FIG. 7 shows the non-denatured type II collagen-containing colloidal suspension of example 5 before storage for 30 days
FIG. 8 shows the non-denatured type II collagen-containing colloidal suspension of example 5 stored for 30 days.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
Colloidal suspension of non-denatured type II collagen and preparation method thereof
Raw materials and proportion: 2-10 parts of non-denatured II type collagen powder, 1-5 parts of hydrophilic colloid, 1-3 parts of oligosaccharide, 1-5 parts of hydrolyzed II type collagen, and the balance of water to 100 parts.
The preparation of a colloidal suspension of non-denatured type II collagen was as follows:
a. preparing materials: 30g of non-denatured type II collagen-containing protein powder, 15g of inulin, and 16g of hydrolyzed type II collagen were added to 1000mL of sterile water, and the mixture was dispersed by shearing at 3000rpm for 15 minutes to obtain a crude dispersion.
b. High-pressure homogenization: allowing the coarse dispersion solution to enter a high-pressure homogenizer, and circulating for 2 times under the homogenization pressure of 35MPa to obtain dispersion solution, wherein the temperature is controlled at 28 ℃;
c. sol: to 1000mL of sterile water was added 10g of xanthan gum: gellan gum: mixing konjac glucomannan 4:3:3 colloid, adding 80 deg.C hot water under aseptic condition, shearing and dispersing at 5000rpm for 10min to fully swell, and cooling to 35 deg.C to obtain colloid solution;
d. mixing: uniformly mixing the dispersion liquid obtained in the step b and the colloidal solution obtained in the step c at 35 ℃ to obtain a mixed liquid;
e. high-pressure micro-jet homogenization: homogenizing the mixed solution for 2 times under 100MPa in a high-pressure micro-jet homogenizer, and controlling the temperature at 30 ℃ to obtain a suspension;
f. cooling and standing: standing the mixed dispersion liquid, and cooling to obtain hydrogel with certain gel strength;
g. shearing the gel: the gel was dispersed by shearing at 2000rpm to give a colloidal suspension.
Example 2
Suspension type solid beverage containing non-denatured type II collagen and preparation method thereof
Weighing 25 parts of colloid suspension freeze-dried powder containing non-denatured II type collagen, 15 parts of inulin, 15 parts of fish collagen peptide, 20 parts of hydrolyzed II type collagen, 10 parts of sea buckthorn powder, 5 parts of citric acid, 2 parts of vitamin C, 2 parts of sodium citrate, 1 part of turmeric and 5 parts of essence.
The preparation method comprises the steps of preparing freeze-dried powder of colloid suspension containing non-denatured type II collagen and blending solid beverage. The preparation method comprises the following steps:
1) preparation of colloid suspension freeze-dried powder containing non-denatured type II collagen
A colloidal suspension of non-denatured type II collagen was prepared in the same manner as in example 1, and the colloidal suspension was pre-frozen in a refrigerator at-80 ℃ for 3 hours, and dried by a freeze-drying apparatus for 48 hours.
2) Solid beverage blending
Weigh colloid suspension freeze-dried powder that contains non-degeneration type II collagen and other required raw materials according to the ratio, mix earlier according to the raw materials that weight ratio is close, begin to carry out gradient mixing step by step from the raw materials that weight is lighter, the mixing order is in proper order: turmeric, vitamin C, sodium citrate, citric acid, essence, sea buckthorn powder, inulin, fish collagen peptide, hydrolyzed type II collagen and colloid suspension freeze-dried powder containing non-denatured type II collagen; and (3) after fully and uniformly mixing, subpackaging by using a composite membrane under an aseptic condition to obtain the non-denatured II type collagen solid beverage with the specification of 5 g/bag.
The eating method comprises the following steps: the picture of the non-denatured type II collagen-containing suspension type solid beverage brewed with 100mL of 25 ℃ water at 0s, 10s, 20s and 30s is shown in figure 1, and the colloidal suspension can be obtained for drinking after fully stirring for 30 s.
Example 3
Suspension type solid beverage containing non-denatured type II collagen and preparation method thereof
Raw materials and proportion: 8 parts of non-denatured II type collagen, 12 parts of xanthan gum, 30 parts of inulin, 20 parts of fish collagen peptide, 20 parts of hydrolyzed II type collagen, 5 parts of sea buckthorn powder and 5 parts of curcumin.
The preparation method comprises the preparation of colloid suspension containing non-denatured type II collagen and the preparation of solid beverage. The preparation method comprises the following steps:
1) preparation of colloidal suspension containing non-denatured type II collagen
The same as in example 1.
2) Solid beverage blending
Weighing other required raw materials except non-denatured type II collagen powder according to a ratio, fully mixing uniformly, adding into colloidal suspension containing non-denatured type II collagen, stirring uniformly, freeze drying the mixed solution at-60 deg.C for 48 hr, pulverizing for 10min,The impact velocity was 20 times s -1 Crushing at 18 deg.c, sieving with 200 mesh sieve, and packing in sterile environment to obtain solid beverage containing non-denatured type II collagen.
The eating method comprises the following steps: the picture of the non-denatured type II collagen-containing suspension type solid beverage brewed with 100mL of 30 ℃ water at 0s, 10s, 20s and 30s is shown in FIG. 2, and the colloidal suspension can be obtained and drunk after fully stirring for 30 s.
Example 4
Suspended solid beverage containing non-denatured II type collagen and preparation method thereof
Raw materials and proportion: 8 parts of non-denatured II type collagen, 12 parts of xanthan gum, 30 parts of inulin, 20 parts of fish collagen peptide, 20 parts of hydrolyzed II type collagen, 5 parts of sea buckthorn powder and 5 parts of curcumin.
The preparation method comprises the preparation of non-denatured type II collagen/hydrocolloid colloid composite powder and the blending of solid beverage, and specifically comprises the following steps:
1) preparation method of non-denatured type II collagen/hydrocolloid colloid composite powder
Weighing the non-denatured type II collagen and the xanthan gum according to the proportion of 2:3, uniformly mixing, pouring into a high-energy nano impact mill for grinding for 6 hours, cooling to 2 ℃, grinding the medium zirconia ceramic balls at the machine power of 4kw and the rotating speed of 400r/min, and grinding to obtain the non-denatured type II collagen/hydrocolloid colloid composite powder.
2) Solid beverage blending
Weighing the required raw materials according to the proportion, carrying out gradient mixing step by step according to the sequence of the sea buckthorn powder, the curcumin, the fish collagen peptide, the hydrolyzed type II collagen, the inulin and the non-denatured type II collagen/hydrophilic colloid composite powder, fully mixing uniformly, and subpackaging by using a composite membrane under an aseptic condition to obtain the non-denatured type II collagen-containing solid beverage with the specification of 5 g/bag.
The eating method comprises the following steps: the picture of the non-denatured type II collagen-containing suspension type solid beverage brewed with 100mL of 10 ℃ water at 0s, 10s, 20s and 30s is shown in FIG. 3, and the colloidal suspension can be obtained for drinking after fully stirring for 30 s.
Example 5
Colloidal suspension stability and storage Properties of non-denatured type II collagen
Using the product obtained in example 1 as a test sample and three control groups simultaneously, as shown in Table 1, the stability was measured by a Turbiscan Lab stability analyzer, and the curves of the transmitted light intensity and the backscattered light intensity with time were measured at 25 ℃ for each of the four samples. Firstly, setting a required testing temperature, placing a sample to be tested in a sample cell, balancing for 30min at the temperature with the sample height of 0-42mm, then adopting a continuous scanning mode, collecting a group of data every 25s, and continuously scanning for 30min to obtain the change curve of the intensity of transmitted light and backscattered light along with time. The test results show that the transmitted light signal is almost 0, and therefore, the time-dependent change of the intensity of backscattered light is analyzed as shown in fig. 4-a to 4-d, and the time-dependent change curve of the TSI value at a given measurement time is calculated and plotted as shown in fig. 5.
As can be seen from the figure, the stability of the samples of the experimental group and the control group is significantly different. The change trend of the delta BS values of the three of the control group is similar along with the time, namely precipitation appears at the bottom, the fluctuation in the middle is large, clarification appears at the top, and the stability of the sample of the control group is known to be poor. In comparison, the untreated non-denatured type II collagen was the least stable, with the Δ BS image showing a more pronounced bulge at the bottom, indicating more precipitation, and a pronounced valley at the top, indicating a clear top, again demonstrating that the untreated non-denatured type II collagen has very poor solubility in water, not favorable for use as a liquid formulation (see fig. 4-a); if a proper amount of glue is simply added for dissolution, and the non-denatured type II collagen is prepared into a suspension, the dispersibility (as shown in figure 4-b) cannot be better changed, and the precipitation and delamination phenomena still occur; the peak of the non-denatured type II collagen treated by the method is shifted to the right (as shown in fig. 4-c), which indicates that the dispersibility of the sample is enhanced and the precipitation is reduced, and the method has an effect on improving the suspension type of the non-denatured type II collagen, but the phenomenon of upper layer clarification still occurs. The data of the experimental group show that the bottom of the treated non-denatured type II collagen colloidal suspension delta BS image has no obvious bulge, the change condition of the middle section delta BS is not obvious, the top has no obvious layering phenomenon, and the uniformity stability is good (as shown in figure 4-d). Finally, to characterize the overall stability of the samples, the relative stability of each system was compared by the stability kinetics index (TSI) defined by the Turbiscan Easysoft software, and the results are shown in fig. 5; the smaller the TSI value, the more stable the system, and the TSI result is consistent with the analysis, which shows the uniqueness and effectiveness of the method.
TABLE 1 methods for setting up experimental and control groups
Also, using the product obtained in example 1 as an experimental group, as shown in table 1, three samples were prepared as a control group, and the particle size distribution thereof was measured by a static light scattering particle sizer, and the result is shown in fig. 6, which shows that the method can significantly reduce the particle size of the system, and the particle size distribution of the experimental group is in a relatively "thin" monomodal shape, which is more favorable for the dispersion stability of the system, while the particle size of the control group is larger, and the peak area is wider, which is unfavorable for the stability of the system, and is consistent with the above results.
The samples of the experimental group were placed in citric acid solutions of pH3.8 and pH5 and sucrose aqueous solutions with soluble solid content of 10 ° Brix, respectively, and subjected to storage experiments at 35 ℃ for 30 days under dark conditions. Samples were taken before and after storage respectively for testing. The test items were sensory analyses, and the test results are shown in table 2.
TABLE 2 stability test results for colloidal suspensions containing non-denatured type II collagen
The test results of the Turbiscan Lab stability and the particle size distribution show that the colloidal suspension has good stability and particle size distribution. The stability test results of the non-denatured type II collagen colloidal suspensions before and after storage (shown in FIGS. 7 and 8) as a control show that the colloidal suspensions can be stored in a low-acid, high-acid and neutral environment and at a temperature of less than 35 ℃ in the dark for 30 days, and still maintain good stability.
Claims (10)
1. A liquid preparation of non-denatured type II collagen, characterized in that the liquid preparation is a colloidal suspension or a suspended solid beverage that can be prepared into a colloidal suspension by water at a temperature of 35 ℃ or lower.
2. The liquid non-denatured type II collagen preparation according to claim 1, wherein the colloidal suspension is homogeneous and transparent, and has a suspension stability of at least 30 days and a pH of 3-7.
3. The liquid non-denatured type II collagen preparation according to claim 1, wherein said colloidal suspension is composed of the following raw materials: 2-10 parts of non-denatured II type collagen powder, 1-5 parts of hydrophilic colloid, 1-3 parts of oligosaccharide, 1-5 parts of hydrolyzed II type collagen, and the balance of water to 100 parts.
4. The liquid preparation of non-denatured type II collagen according to claim 1, characterized in that said solid beverage in suspension type is composed of the following raw materials: 25-70 parts of the colloidal suspension of claim 2, from which water has been removed; 10-20 parts of fish collagen peptide, 5-10 parts of sea buckthorn powder, 0-10 parts of citric acid, 0-5 parts of vitamin C, 0-3 parts of sodium citrate, 0.1-1 part of turmeric and 0-1 part of essence.
5. The liquid preparation of non-denatured type II collagen according to claim 1, characterized in that said solid beverage in suspension type is composed of the following raw materials: 5-30 parts of hydrophilic colloid, 10-15 parts of non-denatured II type collagen powder, 0-15 parts of oligosaccharide, 10-20 parts of fish collagen peptide, 10-20 parts of hydrolyzed II type collagen, 5-10 parts of sea buckthorn powder, 0-10 parts of citric acid, 0-5 parts of vitamin C, 0-3 parts of sodium citrate, 0.1-1 part of turmeric and 0-1 part of essence.
6. A liquid preparation of non-denatured type II collagen according to claim 3, 4 or 5,
the hydrophilic colloid is one or more of xanthan gum, carrageenan, gellan gum, konjac gum, pectin, sodium alginate or sodium carboxymethylcellulose;
the oligosaccharide is one or more of inulin, fructo-oligosaccharide, malto-oligosaccharide and xylo-oligosaccharide.
7. A method of preparing the colloidal suspension of claim 3, comprising the steps of:
a. preparing materials: adding non-denatured type II collagen powder, oligosaccharide and hydrolyzed type II collagen into sterile water according to a ratio, and shearing and dispersing for 10-60min under the condition of 3000 plus 5000rpm to obtain a crude dispersion;
b. high-pressure homogenization: feeding the coarse dispersion liquid into a high-pressure homogenizer, circulating for 2-5 times under the homogenizing pressure of 20-60 MPa to obtain dispersion liquid, and controlling the temperature at 18-28 ℃;
c. sol: adding hydrophilic colloid into hot water with the temperature of more than 80 ℃ according to the material-liquid ratio of 1:50-1:100, shearing for 5-30min under the condition of 3000-;
d. mixing: uniformly mixing the dispersion liquid in the step b with the colloidal solution in the step c to obtain a mixed liquid;
e. high-pressure micro-jet homogenization: homogenizing the mixed solution in a high-pressure micro-jet homogenizer at 80-150MPa for 1-3 times, and controlling the temperature at 28-38 deg.C to obtain suspension;
f. cooling and standing: standing the suspension, and cooling to obtain gel;
g. shearing the gel: the gel was dispersed by shearing at 1000-5000rpm to obtain a colloidal suspension.
8. A method for preparing a suspended solid beverage according to claim 4, comprising the steps of:
1) the method as defined in claim 1Freeze drying the colloidal suspension at a pre-freezing temperature of-80 deg.C to-20 deg.C for 24-72 hr, pulverizing for 5-15min at an impact speed of 10-20 times s -1 The crushing temperature is controlled at 5-18 ℃, and a product with the average grain diameter smaller than 40 mu m and the water removed from the colloidal suspension is obtained, namely the non-denatured II type collagen colloidal suspension freeze-dried powder;
2) weighing the freeze-dried powder of the colloidal suspension and the raw materials in the step 1) according to the proportion, mixing the freeze-dried powder and the raw materials in a gradient manner step by step from light weight to heavy weight, fully mixing the raw materials uniformly, and subpackaging the mixture by using a composite membrane in an aseptic environment to obtain the suspension type solid beverage.
9. A method for preparing a suspended solid beverage according to claim 5, comprising the steps of:
1) weighing raw materials of fish collagen peptide, sea buckthorn powder, citric acid, vitamin C, sodium citrate, turmeric and essence according to a ratio, fully and uniformly mixing, adding the mixture into the colloidal suspension of claim 1, and uniformly stirring to obtain a mixed solution;
2) freeze drying the mixed solution in the step 1) at a pre-freezing temperature of-60 ℃, for 24-72h, for 5-15min, at an impact speed of 10-20 times · s -1 And controlling the crushing temperature to be 5-18 ℃, and subpackaging the crushed materials by a composite membrane in a sterile environment to obtain the suspension type solid beverage.
10. A method for preparing a suspended solid beverage according to claim 5, comprising the steps of:
1) mixing the non-denatured II type collagen powder and the hydrophilic colloid according to the mass ratio of 1:9-9:1, and crushing for 15-120min at the rotation speed of 100-500r/min and the crushing temperature of 5-18 ℃ to prepare non-denatured II type collagen/hydrophilic colloid composite powder with the average particle size of less than 40 mu m;
2) weighing the non-denatured type II collagen/hydrophilic colloid-containing composite powder and the rest raw materials according to the proportion, mixing the raw materials in a gradient manner from light to heavy step by step, fully mixing the raw materials uniformly, and subpackaging the mixture by using a composite membrane in an aseptic environment to obtain the suspended solid beverage.
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