阅读说明：本技术 一种山楂黄酮微胶囊及其制备方法和应用 (hawthorn flavone microcapsule and preparation method and application thereof ) 是由 韩雪 李研东 陶清泉 刘新明 赵丹丹 李丹丹 胡高爽 崔玥 孙宏晔 张薇 袁美玉 于 2019-10-23 设计创作，主要内容包括：本发明提供一种山楂黄酮微胶囊及其制备方法和应用,所述芯材包括山楂黄酮提取物和植物硒多肽,所述壁材包括酪蛋白磷酸肽、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,提高了山楂黄酮的包埋率和缓释效果,同时还能协同促进山楂黄酮降血压、降血脂等生物活性,提高山楂黄酮的生物利用度；芯材选择植物硒多肽与山楂黄酮进行复配,不但提高了产品的应用价值,而且,植物硒多肽还能协同促进山楂黄酮的生物活性,从而进一步提高微胶囊降血脂、抗氧化等功效。同时,山楂黄酮微胶囊的制备工艺简单,条件温和,制备得到的微胶囊的尺寸较小,稳定性好,成本低廉,适用于企业大规模生产。(The invention provides a hawthorn flavone microcapsule as well as a preparation method and application thereof, wherein a core material comprises hawthorn flavone extract and plant selenium polypeptide, and a wall material comprises casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose. According to the invention, casein phosphopeptide, gelatin, sodium carboxymethylcellulose and a calcium chloride curing agent are added into the wall material to be matched, so that the embedding rate and the slow-release effect of hawthorn flavone are improved, and the bioactivity of the hawthorn flavone, such as blood pressure reduction, blood fat reduction and the like, can be synergistically promoted, and the bioavailability of the hawthorn flavone is improved; the core material is compounded by the plant selenium polypeptide and the hawthorn flavone, so that the application value of the product is improved, and the plant selenium polypeptide can also synergistically promote the biological activity of the hawthorn flavone, so that the effects of reducing blood fat, resisting oxidation and the like of the microcapsule are further improved. Meanwhile, the preparation process of the hawthorn flavone microcapsule is simple, the conditions are mild, the size of the prepared microcapsule is small, the stability is good, the cost is low, and the preparation method is suitable for large-scale production of enterprises.)

1. The hawthorn flavone microcapsule comprises a core material and a wall material, and is characterized in that the core material comprises a hawthorn flavone extract and plant selenium polypeptide, and the wall material comprises casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose.

2. The hawthorn flavone microcapsule as claimed in claim 1, wherein the mass ratio of the casein phosphopeptide, the calcium chloride, the gelatin and the sodium carboxymethylcellulose is 4-6:4-6:75-85: 8-12; and/or

The mass ratio of the hawthorn flavone extract to the plant selenium polypeptide is 200-400: 1.

3. The hawthorn flavone microcapsule according to claim 1 or 2, wherein the mass ratio of the core material to the wall material is 1: 6-8.

4. the hawthorn flavone microcapsule of claim 1, wherein the preparation method of the hawthorn flavone extract comprises: freezing fructus crataegi with water content of 5-15%, pulverizing, and sieving to obtain fructus crataegi powder; adding 30-40 times of anhydrous ethanol, ultrasonic extracting at 50-60 deg.C for 30-40min, and filtering to obtain residue and filtrate; adding 15-20 times of anhydrous ethanol into the residue, ultrasonic extracting at 50-60 deg.C for 30-40min, filtering, mixing filtrates, and concentrating to obtain fructus crataegi flavone extract.

5. The method for preparing hawthorn flavone microcapsules of any one of claims 1 to 4, which is characterized by comprising the following steps:

Weighing the components according to a designed ratio, and respectively dissolving the weighed casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose in water to respectively obtain a casein phosphopeptide solution, a calcium chloride solution, a gelatin solution and a sodium carboxymethylcellulose solution;

Secondly, dissolving the weighed hawthorn flavone extract into an ethanol solution with the mass concentration of 70-90% to obtain a hawthorn flavone solution;

Dissolving the weighed plant selenium polypeptide in water to obtain a plant selenium polypeptide aqueous solution;

step four, uniformly mixing the hawthorn flavone solution and the plant selenium polypeptide aqueous solution, adjusting the pH value to 4.8-5.2, and stirring at 50-70 ℃ for 2-4h to obtain a core material;

And step five, adding an emulsifier into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the core material into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.3-4.7, adding the casein phosphopeptide solution and the calcium chloride solution at the temperature of 0-5 ℃, adjusting the pH to 8-9, curing for 50-70min, centrifuging, and freeze-drying to obtain the hawthorn flavone microcapsule.

6. The method for preparing hawthorn flavone microcapsules of claim 5, wherein in the first step, the concentration of the casein phosphopeptide solution is 15-25mg/mL, the concentration of the calcium chloride solution is 15-25mg/mL, the concentration of the gelatin solution is 12-18mg/mL, and the concentration of the sodium carboxymethylcellulose solution is 1.2-1.8 mg/mL.

7. The method for preparing hawthorn flavone microcapsules of claim 5, wherein the concentration of the hawthorn flavone solution is 35-45mg/mL, and the concentration of the plant selenium polypeptide aqueous solution is 180-220 μ g/mL.

8. The method for preparing hawthorn flavone microcapsules of claim 5, wherein the emulsifier is Tween 80.

9. The method for preparing hawthorn flavone microcapsules of claim 8, wherein the addition amount of the emulsifier is 0.8-1.2% of the mass of the gelatin solution.

10. Use of the hawthorn flavone microcapsules of any one of claims 1 to 4 in an antioxidant, hypolipidemic drug or health food.

Technical Field

The invention relates to the technical field of microcapsule preparation, in particular to a hawthorn flavone microcapsule and a preparation method and application thereof.

Background

The hawthorn fruit contains abundant flavonoids, has the effects of resisting oxidation, reducing blood pressure and blood fat, relieving pain and healing wounds by inhibiting the secretion of inflammatory biological enzymes and the like, and can be used as a functional factor to be added into food or medicines. However, the flavonoid compounds are not stable in nature and are susceptible to factors such as oxygen in the air, light in the storage environment, temperature and the like, so that the activity of the flavonoid compounds is reduced and even lost. The hawthorn flavone is embedded by microencapsulation technology, which is not only beneficial to the preservation of flavonoid substances, but also enables the flavonoid substances to stably play a role in organisms. Microencapsulation is a technique in which particles, droplets, bubbles, or the like are encapsulated into heterogeneous fine particles using a polymeric film-forming material. The technology can achieve the aims of protecting the physicochemical property of the microcapsule core material, keeping the functional activity of the microcapsule core material and achieving sustainable release. However, the existing preparation process of the hawthorn flavone microcapsules is complex, and the prepared microcapsules have incomplete structures, so that the stability of the microcapsules is poor, a large amount of hawthorn flavone is difficult to reach a specified absorption part after entering an organism, the organism cannot efficiently utilize the hawthorn flavone, and the bioavailability of the hawthorn flavone is to be further improved.

Disclosure of Invention

The invention provides a hawthorn flavone microcapsule and a preparation method and application thereof, aiming at the problems that the existing hawthorn flavone microcapsule is complex in preparation process, incomplete in prepared microcapsule structure and low in hawthorn flavone bioavailability.

In order to solve the technical problems, the technical scheme provided by the invention is as follows:

A hawthorn flavone microcapsule comprises a core material and a wall material, wherein the core material comprises hawthorn flavone extract and plant selenium polypeptide, and the wall material comprises casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose.

The existing microcapsule generally adopts gelatin, chitosan or sodium alginate and the like as wall materials, the prepared microcapsule has an incomplete structure and small strength of the wall, and the structure of the microcapsule is quickly destroyed after entering a body, so that hawthorn flavone is exposed under the conditions of gastric acid, pepsin and the like of the body, the activity of the hawthorn flavone is seriously influenced, and the hawthorn flavone is difficult to reach a designated absorption part in a large amount, and the oral bioavailability of the hawthorn flavone is low. According to the invention, casein phosphopeptide, gelatin, sodium carboxymethylcellulose and a calcium chloride curing agent are added into the wall material to be matched, so that the embedding rate and the slow-release effect of hawthorn flavone are improved, and the bioactivity of the hawthorn flavone, such as blood pressure reduction, blood fat reduction and the like, can be synergistically promoted, and the bioavailability of the hawthorn flavone is improved; the core material is compounded by the plant selenium polypeptide and the hawthorn flavone, so that the application value of the product is improved, and the plant selenium polypeptide can also synergistically promote the biological activity of the hawthorn flavone, so that the effects of reducing blood fat, resisting oxidation and the like of the microcapsule are further improved.

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 hawthorn 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 hawthorn flavone, so that the biological activity and water solubility of the hawthorn flavone compound are improved, the bioavailability of the hawthorn flavone is improved, and the effects of lowering blood pressure, reducing blood fat and the like of the hawthorn flavone are fully exerted.

the plant selenium polypeptide has the effects of resisting oxidation and cancer, enhancing immunity, regulating vitamin absorption and utilization, promoting protein synthesis and the like, is compounded with hawthorn flavone as a core material, not only improves the nutritional value of the microcapsule, but also promotes the synthesis of selenium protein in a human body, regulates the activity of immunocytes, regulates intestinal tracts and synergistically promotes the absorption and utilization of the hawthorn flavone by the intestinal tracts, thereby further improving the bioavailability of the hawthorn flavone.

Preferably, the mass ratio of the casein phosphopeptide to the calcium chloride to the gelatin to the sodium carboxymethyl cellulose is 4-6:4-6:75-85: 8-12.

Compared with the prior art, the casein phosphopeptide, the calcium chloride, the gelatin and the sodium carboxymethyl cellulose in a specific proportion are selected as wall materials of the microcapsule, and the wall materials and the calcium chloride can form a capsule wall with high polymerization degree and good stability after being solidified, so that the capsule wall has better compactness and integrity, the core material can be better protected, the core material is prevented from leaking, and the bioavailability of the hawthorn flavone is improved.

Preferably, the mass ratio of the hawthorn flavone extract to the plant selenium polypeptide is 200-400: 1.

The optimized mass ratio of the hawthorn flavone extract to the plant selenium polypeptide can enable the hawthorn flavone extract and the plant selenium polypeptide to synergistically exert the best biological activity, obviously promote the synthesis of matrix selenoprotein, improve the biological activity of the hawthorn flavone, promote the body to absorb and utilize the hawthorn flavone and improve the bioavailability of the hawthorn flavone.

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

The preferable mass ratio of the wall material to the core material can ensure that the microcapsule has better integrity and slow release performance and controllable release performance.

Preferably, the preparation method of the hawthorn flavone extract comprises the following steps: freezing fructus crataegi with water content of 5-15%, pulverizing, and sieving to obtain fructus crataegi powder; adding 30-40 times of anhydrous ethanol, ultrasonic extracting at 50-60 deg.C for 30-40min, and filtering to obtain residue and filtrate; adding 15-20 times of anhydrous ethanol into the residue, ultrasonic extracting at 50-60 deg.C for 30-40min, filtering, mixing filtrates, and concentrating to obtain fructus crataegi flavone extract.

the preferable preparation method of the hawthorn flavone can dissolve the hawthorn flavone in the raw materials into the extracting solution more, avoids the hawthorn flavone from being damaged due to high temperature, and simultaneously avoids the contradiction problem of poor quality of the extracted product caused by excessive entrainment of ineffective substances.

the invention also provides a preparation method of the hawthorn flavone microcapsule, which comprises the following steps:

weighing the components according to a designed ratio, and respectively dissolving the weighed casein phosphopeptide, calcium chloride, gelatin and sodium carboxymethylcellulose in water to respectively obtain a casein phosphopeptide solution, a calcium chloride solution, a gelatin solution and a sodium carboxymethylcellulose solution;

Dissolving the weighed plant selenium polypeptide in water to obtain a plant selenium polypeptide aqueous solution;

Step four, uniformly mixing the hawthorn flavone solution and the plant selenium polypeptide aqueous solution, adjusting the pH value to 4.8-5.2, and stirring at 50-70 ℃ for 2-4h to obtain a core material;

And step five, adding an emulsifier into the gelatin solution, uniformly mixing to obtain a gelatin emulsion, adding the core material into the gelatin emulsion, uniformly mixing, adding the sodium carboxymethylcellulose solution, uniformly mixing, adjusting the pH to 4.3-4.7, adding the casein phosphopeptide solution and the calcium chloride solution at the temperature of 0-5 ℃, adjusting the pH to 8-9, curing for 50-70min, centrifuging, and freeze-drying to obtain the hawthorn flavone microcapsule.

the microcapsule prepared by the preparation method has the particle size centralized distribution of about 2 μm, and the embedding rate of hawthorn flavone can reach more than 90%. The process for preparing the hawthorn flavone microcapsules is simple, the conditions are mild, the prepared microcapsules are small in size, high in separation degree, good in stability and low in cost, and the hawthorn flavone microcapsules are suitable for large-scale production of enterprises.

Preferably, the concentration of the casein phosphopeptide solution is 15-25mg/mL, the concentration of the calcium chloride solution is 15-25mg/mL, the concentration of the gelatin solution is 12-18mg/mL, and the concentration of the sodium carboxymethylcellulose solution is 1.2-1.8 mg/mL.

the optimized concentration of each wall material raw material is beneficial to the full and uniform mixing of the raw materials, and the microencapsulation efficiency is improved.

Preferably, the concentration of the hawthorn flavone solution is 35-45mg/mL, and the concentration of the plant selenium polypeptide aqueous solution is 180-220 mug/mL.

the optimized concentration of the hawthorn flavone solution and the plant selenium polypeptide aqueous solution is beneficial to the full emulsification of the core material, and the concentration of active substances in the core material of the microcapsule can be improved, so that the biological activity of the prepared microcapsule is improved.

Preferably, the emulsifier is tween 80.

preferably, the addition amount of the emulsifier is 0.8-1.2% of the mass of the gelatin solution.

The optimized dosage of the emulsifier can ensure that the hawthorn flavone is fully emulsified, achieve more excellent embedding effect and be beneficial to forming a stable microcapsule structure.

Optionally, in the fourth step, the stirring speed is 100-300 rpm/min.

the optimized stirring speed can ensure that the hawthorn flavone extract and the plant selenium polypeptide are fully and uniformly mixed, thereby being beneficial to subsequent emulsification to obtain emulsion with uniform size.

The invention also provides application of the hawthorn flavone microcapsule in antioxidant and blood fat reducing medicines or health-care foods.

The hawthorn flavone microcapsule prepared by the invention has good structural stability and strength, can resist the damage of gastrointestinal environment to hawthorn flavone activity, has good slow release effect, can improve the activity and solubility of the hawthorn flavone after inclusion, is easy to be absorbed by human body, further improves the bioavailability of the hawthorn flavone by selecting the plant selenium polypeptide and the hawthorn flavone for compounding in the core material, and has wide application prospect in the fields of antioxidant and blood fat reducing medicines or health-care foods.

Drawings

FIG. 1 is a scanning electron microscope image of the hawthorn flavone microcapsule prepared in example 1 of the present invention;

fig. 2 is a graph showing the sustained release effect of the hawthorn flavone microcapsules prepared in example 1 of the present invention in simulated gastrointestinal fluids.

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.