阅读说明：本技术 一种葛根黄酮微胶囊的制备方法 (Preparation method of pueraria flavone microcapsules ) 是由 曹鸿霞 马铭泽 马云峰 于 2020-05-22 设计创作，主要内容包括：一种葛根黄酮微胶囊的制备方法,所述芯材为葛根黄酮提取物,所述壁材为酪蛋白磷酸肽、氯化钙、明胶和羧甲基纤维素钠。本发明在壁材中加入酪蛋白磷酸肽、明胶和羧甲基纤维素钠与氯化钙固化剂进行配合,提高了葛根黄酮的包埋率和缓释效果,同时还能协同促进葛根黄酮降血压、降血脂等生物活性,提高葛根黄酮的生物利用度。本发明制备的葛根黄酮微胶囊的工艺简单,条件温和,制备得到的微胶囊的尺寸较小,分离度高,稳定性好,成本低廉,适用于企业大规模生产。(A preparation method of pueraria flavone microcapsules comprises the steps of taking pueraria flavone extract as a core material and taking casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose as wall materials. According to the invention, casein phosphopeptide, gelatin, sodium carboxymethylcellulose and a calcium chloride curing agent are added into the wall material for matching, so that the embedding rate and the slow-release effect of pueraria flavone are improved, and the biological activities of pueraria flavone for reducing blood pressure, blood fat and the like can be synergistically promoted, and the bioavailability of pueraria flavone is improved. The pueraria flavone microcapsule prepared by the invention has the advantages of simple process, mild conditions, small size, high separation degree, good stability and low cost, and is suitable for large-scale production of enterprises.)

1. A preparation method of pueraria flavone microcapsules is characterized by comprising the following steps: the preparation method comprises the following steps:

s1, preparing a wall material solution:

weighing wall materials according to a design ratio, wherein the wall materials comprise casein phosphopeptides, calcium chloride, gelatin and sodium carboxymethylcellulose;

mixing casein phosphopeptide with water to obtain casein phosphopeptide solution; mixing calcium chloride with water to obtain a calcium chloride solution; mixing gelatin with water to obtain gelatin solution; mixing sodium carboxymethylcellulose with water to obtain sodium carboxymethylcellulose solution;

s2, preparing a core material solution:

weighing a certain amount of core materials, wherein the core materials comprise pueraria flavone extracts, and dissolving the pueraria flavone extracts in an ethanol solution to obtain a pueraria flavone solution;

s3, preparing pueraria flavone microcapsules:

adding an emulsifier into the gelatin solution, and uniformly mixing to obtain a gelatin emulsion;

adding the pueraria flavone solution into the gelatin emulsion, and uniformly mixing to obtain a mixed solution 1;

adding the sodium carboxymethylcellulose solution into the mixed solution 1, and uniformly mixing to obtain a mixed solution 2;

adjusting the pH value of the mixed solution 2 to 4.3-4.7, adjusting the temperature of the mixed solution 2 to be kept at 0-5 ℃, adding the casein phosphopeptide solution and the calcium chloride solution into the mixed solution 2, and uniformly mixing to obtain a mixed solution 3;

adjusting the pH value of the mixed solution 3 to 8-9, and then sequentially carrying out solidification-centrifugation-freeze drying treatment on the mixed solution 3 to obtain the pueraria flavone microcapsule.

2. The preparation method of pueraria flavonid microcapsule according to claim 1, which is characterized by comprising the following steps of: in the S1, the mass ratio of the casein phosphopeptide to the calcium chloride to the gelatin to the sodium carboxymethyl cellulose is as follows: 70-80: 6-10: 4-6: 3-5.

3. The method for preparing pueraria flavonid microcapsule according to claim 1 or 2, wherein the steps of: the mass ratio of the core material to the wall material is 1: 6-8.

4. The preparation method of pueraria flavonid microcapsule according to claim 1, which is characterized by comprising the following steps of: in S3, the curing time of the mixed solution 3 is 50 to 70 min.

5. The preparation method of pueraria flavonid microcapsule according to claim 1, which is characterized by comprising the following steps of: in S3, the freeze-drying time of the mixed solution 3 is 10-13 h.

Technical Field

The invention belongs to the technical field of preparation of pueraria flavone, and particularly relates to a preparation method of pueraria flavone microcapsules.

Background

The pueraria flavone contained in the pueraria has various pharmacological activities, such as expanding coronary artery blood vessels, increasing coronary artery blood flow, reducing blood pressure and blood sugar, improving cerebral circulation, inhibiting platelet aggregation and the like. The product enters domestic and foreign markets, is sold in international markets such as south-east Asia, Europe and America and the like, is used as a functional factor to be added into food or medicines, but the flavonoid compound is unstable in property and is easily influenced by factors such as oxygen in the air, illumination in a storage environment, temperature and the like, so that the activity of the flavonoid compound is reduced and even lost;

in the existing medicines, capsules are often used for protecting the medicines so that the medicines can enter a designated position and then be absorbed by a human body, but the wall materials of the existing capsules generally adopt gelatin, chitosan or sodium alginate and the like as wall materials, the prepared microcapsules have incomplete structures and small strength of the capsule walls, and the structures of the microcapsules can be quickly destroyed after entering an organism, so that pueraria flavone is exposed under the conditions of gastric acid, pepsin and the like of the organism, the activity of the pueraria flavone is seriously influenced, and a large amount of pueraria flavone cannot reach the designated absorption position easily, and the oral bioavailability of the pueraria flavone is low; therefore, the existing capsule wall material cannot be suitable for pueraria flavone;

in conclusion, the existing pueraria flavone is lack of a better activity protection structure, so that the application of the pueraria flavone is limited.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a preparation method of pueraria flavone microcapsules, which has the following specific technical scheme:

a preparation method of pueraria flavone microcapsules comprises the following steps:

s1, preparing a wall material solution:

weighing wall materials according to a design ratio, wherein the wall materials comprise casein phosphopeptides, calcium chloride, gelatin and sodium carboxymethylcellulose;

mixing casein phosphopeptide with water to obtain casein phosphopeptide solution; mixing calcium chloride with water to obtain a calcium chloride solution; mixing gelatin with water to obtain gelatin solution; mixing sodium carboxymethylcellulose with water to obtain sodium carboxymethylcellulose solution;

s2, preparing a core material solution:

weighing a certain amount of core materials, wherein the core materials comprise pueraria flavone extracts, and dissolving the pueraria flavone extracts in an ethanol solution to obtain a pueraria flavone solution;

s3, preparing pueraria flavone microcapsules:

adding an emulsifier into the gelatin solution, and uniformly mixing to obtain a gelatin emulsion;

adding the pueraria flavone solution into the gelatin emulsion, and uniformly mixing to obtain a mixed solution 1;

adding the sodium carboxymethylcellulose solution into the mixed solution 1, and uniformly mixing to obtain a mixed solution 2;

adjusting the pH value of the mixed solution 2 to 4.3-4.7, adjusting the temperature of the mixed solution 2 to be kept at 0-5 ℃, adding the casein phosphopeptide solution and the calcium chloride solution into the mixed solution 2, and uniformly mixing to obtain a mixed solution 3;

adjusting the pH value of the mixed solution 3 to 8-9, and then sequentially solidifying and centrifuging the mixed solution 3

Freeze drying to obtain pueraria flavone microcapsule.

Further, in the S1, the mass ratio of the casein phosphopeptide to the calcium chloride to the gelatin to the sodium carboxymethyl cellulose is: 70-80: 6-10: 4-6: 3-5.

Furthermore, the mass ratio of the core material to the wall material is 1: 6-8.

Further, in S3, the curing time of the mixed liquid 3 is 50 to 70 min.

Further, in the S3, the freeze-drying time is 10-13 h.

The invention has the beneficial effects that: the pueraria flavone microcapsule prepared by the invention has good structural stability and strength, can resist the damage of gastrointestinal environment to flavone activity, has good slow release effect, can improve the activity and solubility of the flavone after inclusion, is easy to be absorbed by human body, improves the bioavailability of the pueraria flavone, and has wide application prospect in the field of lipid-lowering drugs or health-care foods.

Drawings

Fig. 1 shows a flow chart of a preparation process of pueraria flavone microcapsules of the invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

As shown in fig. 1, a preparation method of pueraria flavone microcapsules comprises the following steps:

s1, preparing a wall material solution:

weighing wall materials according to a design ratio, wherein the wall materials comprise casein phosphopeptides, calcium chloride, gelatin and sodium carboxymethylcellulose; the mass ratio of the casein phosphopeptide to the calcium chloride to the gelatin to the sodium carboxymethylcellulose is as follows: 70-80: 6-10: 4-6: 3-5; by adopting casein phosphopeptide, gelatin and sodium carboxymethylcellulose as wall material raw materials, the wall material can form a capsule wall with high polymerization degree and good stability after being solidified, so that the capsule wall has better tightness and integrity, the core material can be better protected, the core material is prevented from leaking, and the bioavailability of pueraria flavone is improved; the wall material raw materials adopt the proportion, so that the structural strength of the wall material and the tightness among all raw material molecules can be ensured; the casein phosphopeptide can obviously improve the binding rate of calcium ions and wall materials, improve the integrity and strength of a microcapsule capsule wall structure, simultaneously, the casein phosphopeptide structure contains a large number of phosphoserine residues, can prevent the further action of digestive enzymes in the alkalescent environment of intestinal pH, improve the stability of the pueraria flavone microcapsule in the intestinal tract of a human body and improve the slow release effect in the intestinal tract; more importantly, the casein phosphopeptide can also interact with pueraria flavone, so that the biological activity and water solubility of the pueraria flavone compound are improved, the bioavailability of the pueraria flavone is improved, and the efficacies of the pueraria flavone for reducing blood pressure, blood fat and the like are fully exerted;

mixing casein phosphopeptide with water to obtain casein phosphopeptide solution; mixing calcium chloride with water to obtain a calcium chloride solution; mixing gelatin with water to obtain gelatin solution; mixing sodium carboxymethylcellulose with water to obtain sodium carboxymethylcellulose solution;

s2, preparing a core material solution:

weighing a certain amount of core materials, wherein the core materials comprise pueraria flavone extracts, and dissolving the pueraria flavone extracts in an ethanol solution to obtain a pueraria flavone solution; the mass ratio of the core material to the wall material is 1: 6-8; under the condition of the mass ratio of the core material to the wall material, the microcapsule has better integrity and slow release performance and controllable release performance.

S3, preparing pueraria flavone microcapsules:

adding an emulsifier into the gelatin solution, and uniformly mixing to obtain a gelatin emulsion;

adding the pueraria flavone solution into the gelatin emulsion, and uniformly mixing to obtain a mixed solution 1;

adding the sodium carboxymethylcellulose solution into the mixed solution 1, and uniformly mixing to obtain a mixed solution 2;

adjusting the pH value of the mixed solution 2 to 4.3-4.7, adjusting the temperature of the mixed solution 2 to be kept at 0-5 ℃, adding the casein phosphopeptide solution and the calcium chloride solution into the mixed solution 2, and uniformly mixing to obtain a mixed solution 3;

adjusting the pH value of the mixed solution 3 to 8-9, and then sequentially carrying out solidification-centrifugation-freeze drying treatment on the mixed solution 3 to obtain pueraria flavone microcapsules; the curing time is 50-70min, and the freeze-drying time is 10-13 h.

The particle size of the microcapsule obtained by the preparation method is intensively distributed about 2um, and the embedding rate of the pueraria flavone reaches more than 90 percent; the preparation method of the pueraria flavone microcapsule is simple in process, mild in condition, small in size, high in separation degree, good in stability and low in cost, and is suitable for large-scale production of enterprises.

To verify the above beneficial effects, the following comparative tests are now provided:

inventive example 1

Weighing gelatin, sodium carboxymethylcellulose, casein phosphopeptide and calcium chloride according to a mass ratio of 80:10:5:5, respectively dissolving the components in water, and respectively obtaining a casein phosphopeptide solution with a mass concentration of 20mg/mL, a calcium chloride solution with a mass concentration of 20mg/mL, a gelatin solution with a mass concentration of 16mg/mL and a sodium carboxymethylcellulose solution with a mass concentration of 1.6 mg/mL;

step two, weighing pueraria flavone extract according to the mass ratio of the core material to the wall material of 1:7, dissolving the weighed pueraria flavone extract into 90% ethanol solution by mass concentration to prepare pueraria flavone solution with the concentration of 40 mg/mL;

adding Tween 80 with the mass of 1 wt% into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the pueraria flavone solution into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.5, adding the casein phosphopeptide solution and the calcium chloride solution at the temperature of 0 ℃, adjusting the pH to 8.5, solidifying for 60min, carrying out centrifugal separation, and carrying out freeze drying for 12h to obtain the pueraria flavone microcapsule.

The pueraria flavone extract is prepared from pueraria powder producing waste liquid through nano-filtering, ultra-filtering and concentrating.

The pueraria flavone microcapsules obtained in the above embodiments are analyzed, and the quality data are as follows: the submicron microcapsule with good form has the particle size mainly distributed about 2um, high separation degree of the microcapsule, good capsule forming effect and embedding rate of the microcapsule of 91.6 percent.

Inventive example 2

Step one, weighing gelatin, sodium carboxymethylcellulose, casein phosphopeptide and calcium chloride according to a mass ratio of 72:8:6:4, respectively dissolving the components in water, and respectively obtaining a casein phosphopeptide solution with a mass concentration of 25mg/mL, a calcium chloride solution with a mass concentration of 15mg/mL, a gelatin solution with a mass concentration of 18mg/mL and a sodium carboxymethylcellulose solution with a mass concentration of 1.2 mg/mL;

step two, weighing the pueraria flavone extract according to the mass ratio of the core material to the wall material of 1:8, and dissolving the weighed pueraria flavone extract into an ethanol solution with the mass concentration of 70% to prepare a pueraria flavone solution with the concentration of 45 mg/mL;

adding Tween 80 with the mass of 1.2 wt% into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the pueraria flavone solution into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.5, adding the casein phosphopeptide solution and the calcium chloride solution at the temperature of 0 ℃, adjusting the pH to 8.0, solidifying for 70min, carrying out centrifugal separation, and carrying out freeze drying for 12h to obtain the pueraria flavone microcapsule.

The pueraria flavone extract is prepared from pueraria powder producing waste liquid through nano-filtering, ultra-filtering and concentrating.

The pueraria flavone microcapsules obtained in the above embodiments are analyzed, and the quality data are as follows: the submicron microcapsule with good form has the particle size mainly distributed about 2um, high separation degree of the microcapsule, good capsule forming effect and embedding rate of the microcapsule of 91.5 percent.

Comparative example 1

Step one, weighing gelatin, sodium carboxymethylcellulose and calcium chloride according to a mass ratio of 85:10:5, respectively dissolving the above components in water, and respectively obtaining a calcium chloride solution with a mass concentration of 20mg/mL, a gelatin solution with a mass concentration of 16mg/mL and a sodium carboxymethylcellulose solution with a mass concentration of 1.6 mg/mL;

step two, weighing pueraria flavone extract according to the mass ratio of the core material to the wall material of 1:7, dissolving the weighed pueraria flavone extract into 90% ethanol solution by mass concentration to prepare pueraria flavone solution with the concentration of 40 mg/mL;

adding Tween 80 with the mass of 1 wt% into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the pueraria flavone solution into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.5, adding the calcium chloride solution at the temperature of 0 ℃, adjusting the pH to 8.5, solidifying for 60min, performing centrifugal separation, and performing freeze drying for 12h to obtain the pueraria flavone microcapsules.

The pueraria flavone microcapsules obtained in the above embodiments are analyzed, and the quality data are as follows: the particle diameter of the submicron microcapsule with a sunken structure part is mainly distributed about 2um, the separation degree of the microcapsule is general, the capsule forming structure is incomplete, the strength is low, and the embedding rate of the microcapsule is 90.5%.

Comparative example 2

Step one, weighing gelatin, sodium carboxymethylcellulose and calcium chloride according to a mass ratio of 80:13:7, respectively dissolving the above components in water, and respectively obtaining a calcium chloride solution with a mass concentration of 15mg/mL, a gelatin solution with a mass concentration of 18mg/mL and a sodium carboxymethylcellulose solution with a mass concentration of 1.9 mg/mL;

step two, weighing pueraria flavone extract according to the mass ratio of the core material to the wall material of 1:8, dissolving the weighed pueraria flavone extract into 90% ethanol solution by mass concentration to prepare pueraria flavone solution with the concentration of 40 mg/mL;

adding Tween 80 with the mass of 1 wt% into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the pueraria flavone solution into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.5, adding the calcium chloride solution at the temperature of 0 ℃, adjusting the pH to 8.5, solidifying for 60min, performing centrifugal separation, and performing freeze drying for 12h to obtain the pueraria flavone microcapsules.

The pueraria flavone microcapsules obtained in the above embodiments are analyzed, and the quality data are as follows: the particle diameter of the submicron microcapsule with a sunken structure part is mainly distributed about 2um, the separation degree of the microcapsule is general, the capsule forming structure is incomplete, the strength is low, and the embedding rate of the microcapsule is 89.2%.

The comparison tests show that the method for preparing pueraria flavone microcapsules into Erbi can effectively improve the structural integrity, strength and embedding rate of the microcapsules.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.