阅读说明：本技术 一种提高生物利用度的蓝莓活性成分包埋物及其制备方法 (Blueberry active ingredient embedding substance capable of improving bioavailability and preparation method thereof ) 是由 吴元锋 孙娟 许子艺 关荣发 邹礼根 汪娟 马全民 于 2020-06-15 设计创作，主要内容包括：一种提高生物利用度的蓝莓活性成分包埋物及其制备方法,属于植物中天然成分提取和包埋技术领域。包括：(1)蓝莓粉碎,热回流浸提,收集第一次上清液和第一次滤渣；(2)第一次滤渣酸化乙醇溶液浸提,收集第二次上清液和第二次滤渣；(3)第二次滤渣乙酸乙酯浸提,收集第三次上清液；(4)第一、二和三次上清液分别真空浓缩；(5)第一次浓缩液真空冷冻干燥,得干燥粉末A,第二和三次浓缩液混合包埋后真空冷冻干燥,得干燥粉末B；(6)将干燥粉末A、干燥粉末B、微晶纤维素、甘露醇、柠檬酸和硬脂酸镁充分混合压片,得到高生物利用度的蓝莓活性成分包埋物。本发明根据蓝莓活性物极性不同,分段提取,分段包埋,有效提高其生物利用度。(A blueberry active ingredient inclusion compound for improving bioavailability and a preparation method thereof belong to the technical field of natural ingredient extraction and embedding in plants. The method comprises the following steps: (1) crushing blueberries, extracting under hot reflux, and collecting primary supernatant and primary filter residue; (2) leaching the first filter residue by using an acidified ethanol solution, and collecting second supernatant and second filter residue; (3) leaching the second filter residue by ethyl acetate, and collecting the supernatant of the third time; (4) respectively vacuum concentrating the first, second and third supernatants; (5) vacuum freeze drying the first concentrated solution to obtain dry powder A, mixing and embedding the second concentrated solution and the third concentrated solution, and vacuum freeze drying to obtain dry powder B; (6) and fully mixing and tabletting the dry powder A, the dry powder B, the microcrystalline cellulose, the mannitol, the citric acid and the magnesium stearate to obtain the blueberry active ingredient embedded substance with high bioavailability. According to the invention, the blueberry active substances have different polarities, and are extracted in a segmented manner and embedded in a segmented manner, so that the bioavailability of the blueberry active substances is effectively improved.)

1. The blueberry active ingredient inclusion compound for improving bioavailability is characterized by being prepared through the following steps:

(1) crushing dried blueberries to 30-60 meshes, uniformly mixing, carrying out hot reflux extraction by using distilled water as a solvent, cooling to room temperature after extraction, carrying out plate-and-frame filter pressing, and respectively collecting primary supernatant and primary filter residues;

(2) leaching the first filter residue obtained in the step (1) by using an acidified ethanol solution, cooling to room temperature after leaching is finished, performing plate-and-frame filter pressing, and respectively collecting second supernatant and second filter residue;

(3) leaching the second filter residue obtained in the step (2) with ethyl acetate, cooling to room temperature after leaching is completed, performing plate-and-frame filter pressing, and collecting supernatant liquid of the third time respectively;

(4) vacuum concentrating the primary supernatant obtained in the step (1) to a specific gravity of 1.20-1.40 g/ml to obtain a primary concentrated solution, vacuum concentrating the secondary supernatant obtained in the step (2) to a specific gravity of 0.95-1.10 g/ml to obtain a secondary concentrated solution, and vacuum concentrating the tertiary supernatant obtained in the step (3) to a specific gravity of 1.08-1.26 g/ml to obtain a tertiary concentrated solution for later use;

(5) adding maltodextrin into the first concentrated solution according to the weight ratio of 1:0.6-0.8, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder A, mixing the second concentrated solution and the third concentrated solution, weighing hydroxypropyl-beta-cyclodextrin according to the weight ratio of 1:0.3-0.4 to prepare into saturated aqueous solution, stirring and mixing, standing at room temperature after ultrasonic treatment, carrying out plate-and-frame filter pressing, collecting filtrate, adding maltodextrin according to the weight ratio of 1:0.3-0.4, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder B;

(6) and fully mixing the dry powder A, the dry powder B, microcrystalline cellulose, mannitol, citric acid and magnesium stearate, and tabletting to obtain the blueberry active ingredient embedded substance with high bioavailability.

2. The blueberry active ingredient inclusion complex for improving bioavailability as claimed in claim 1, wherein the hot reflux extraction conditions in step (1) are as follows: the temperature is 70-90 ℃, the time is 100-140 min/time, and the ratio of leaching materials to leaching liquids is 1: 8-1: 10 w/v.

3. The blueberry active ingredient inclusion complex capable of improving bioavailability as claimed in claim 1, wherein the acidified ethanol solution in step (2) is prepared by adjusting the pH of 50% -70% ethanol to 2.5-3.5 with glacial acetic acid, and the acidified ethanol solution is extracted under the following conditions: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 5-1: 7 w/v.

4. The blueberry active ingredient inclusion complex for improving bioavailability as claimed in claim 1, wherein the ethyl acetate leaching conditions in the step (3) are as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 3-1: 5 w/v.

5. A preparation method of a blueberry active ingredient inclusion compound for improving bioavailability is characterized by comprising the following steps:

(1) crushing dried blueberries to 30-60 meshes, uniformly mixing, carrying out hot reflux extraction by using distilled water as a solvent, cooling to room temperature after extraction, carrying out plate-and-frame filter pressing, and respectively collecting primary supernatant and primary filter residues;

(2) leaching the first filter residue obtained in the step (1) by using an acidified ethanol solution, cooling to room temperature after leaching is finished, performing plate-and-frame filter pressing, and respectively collecting second supernatant and second filter residue;

(3) leaching the second filter residue obtained in the step (2) with ethyl acetate, cooling to room temperature after leaching is completed, performing plate-and-frame filter pressing, and collecting supernatant liquid of the third time respectively;

(4) vacuum concentrating the primary supernatant obtained in the step (1) to a specific gravity of 1.20-1.40 g/ml to obtain a primary concentrated solution, vacuum concentrating the secondary supernatant obtained in the step (2) to a specific gravity of 0.95-1.10 g/ml to obtain a secondary concentrated solution, and vacuum concentrating the tertiary supernatant obtained in the step (3) to a specific gravity of 1.08-1.26 g/ml to obtain a tertiary concentrated solution for later use;

(5) adding maltodextrin into the first concentrated solution according to the weight ratio of 1:0.6-0.8, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder A, mixing the second concentrated solution and the third concentrated solution, weighing hydroxypropyl-beta-cyclodextrin according to the weight ratio of 1:0.3-0.4 to prepare into saturated aqueous solution, stirring and mixing, standing at room temperature after ultrasonic treatment, carrying out plate-and-frame filter pressing, collecting filtrate, adding maltodextrin according to the weight ratio of 1:0.3-0.4, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder B;

(6) and fully mixing the dry powder A, the dry powder B, microcrystalline cellulose, mannitol, citric acid and magnesium stearate, and tabletting to obtain the blueberry active ingredient embedded substance with high bioavailability.

6. The preparation method of the blueberry active ingredient inclusion compound for improving bioavailability as claimed in claim 5, wherein the hot reflux extraction conditions in the step (1) are as follows: the temperature is 70-90 ℃, the time is 100-140 min/time, and the ratio of leaching materials to leaching liquids is 1: 8-1: 10 w/v.

7. The preparation method of the blueberry active ingredient inclusion complex with improved bioavailability as claimed in claim 5, wherein the acidified ethanol solution in step (2) is prepared by adjusting the pH of 50% -70% ethanol to 2.5-3.5 with glacial acetic acid.

8. The preparation method of the blueberry active ingredient inclusion compound for improving bioavailability as claimed in claim 5, wherein the acidified ethanol solution leaching condition in the step (2) is as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 5-1: 7 w/v.

9. The preparation method of the blueberry active ingredient inclusion compound for improving bioavailability as claimed in claim 5, wherein the ethyl acetate leaching condition in the step (3) is as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 3-1: 5 w/v.

10. The preparation method of the blueberry active ingredient inclusion complex for improving bioavailability as claimed in claim 5, wherein the method for inclusion of hydroxypropyl- β -cyclodextrin in step (5) comprises the following steps:

(a) dissolving hydroxypropyl-beta-cyclodextrin in water to obtain a saturated solution of hydroxypropyl-beta-cyclodextrin;

(b) mixing the first concentrated solution and the second concentrated solution, and slowly adding into the hydroxypropyl-beta-cyclodextrin saturated solution while continuously stirring;

(c) performing ultrasonic treatment for 20min, standing at room temperature for 24h, performing plate and frame filter pressing, and collecting filtrate.

Technical Field

The invention belongs to the technical field of extraction and embedding of natural ingredients in plants, and particularly relates to a blueberry active ingredient embedded substance capable of improving bioavailability and a preparation method thereof.

Background

Blueberry, also known as bilberry, is a plant of the genus Vaccinium of the family Ericaceae. The blueberry has good taste and also has obvious effects of nutrition and health promotion, because the blueberry is very rich in nutrition and is rich in nutritional and functional components such as anthocyanin, procyanidine, flavonoid, superoxide dismutase (SOD), ursolic acid, sugar, acid, lipid, protein, vitamin, mineral elements and the like. To date, 15 anthocyanins, 20 flavonols and their glycosides, 19 phenolic acids, 6 procyanidins, 5 saccharides, 12 organic acids, 67 volatile aroma components have been identified from blueberries. The extraction method of blueberry active substances comprises an extraction method, an enzymolysis method, an ultrasonic extraction method, a microwave-assisted extraction method and the like, and common extraction solvents comprise methanol, ethanol, water and the like. The commonly used embedding wall materials of the active substances comprise soybean protein isolate, maltodextrin, Arabic gum, ethyl cellulose and the like, but because the blueberry active substances are more and have great polarity difference, the active substances are difficult to extract by using one solvent, and the embedding effect by using one embedding substance is not ideal.

The bioavailability of an active substance depends mainly on 3 factors: bioassays, absorptivities and biotransformations. The bioassaability is influenced by the release of the active substance from the food matrix and its solubility in gastric juices. Some components in the blueberries such as anthocyanin, flavonol glycoside, phenolic acid and the like have good solubility, but other components such as cyanidin and the like, flavonol and procyanidine and the like have very poor water solubility, so that the bioavailability of the blueberry is greatly limited. At present, in blueberry extraction and process, only one effective component or nutrient substance is obtained by one extraction process and then is embedded by one embedding process. In addition, antioxidant activity, stability and the like are generally considered during extraction and embedding, but the bioavailability is rarely considered, so that the blueberry active ingredient embedded substance capable of improving the bioavailability and the preparation method thereof are very necessary.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to design and provide a blueberry active ingredient inclusion compound for improving bioavailability and a preparation method thereof. According to the invention, the blueberry active substances have different polarities, and are extracted in a segmented manner and embedded in a segmented manner, so that the bioavailability of the blueberry active substances is effectively improved.

The blueberry active ingredient inclusion compound for improving bioavailability is characterized by being prepared through the following steps:

(1) crushing dried blueberries to 30-60 meshes, uniformly mixing, carrying out hot reflux extraction by using distilled water as a solvent, cooling to room temperature after extraction, carrying out plate-and-frame filter pressing, and respectively collecting primary supernatant and primary filter residues;

(2) leaching the first filter residue obtained in the step (1) by using an acidified ethanol solution, cooling to room temperature after leaching is finished, performing plate-and-frame filter pressing, and respectively collecting second supernatant and second filter residue;

(3) leaching the second filter residue obtained in the step (2) with ethyl acetate, cooling to room temperature after leaching is completed, performing plate-and-frame filter pressing, and collecting supernatant liquid of the third time respectively;

(4) vacuum concentrating the primary supernatant obtained in the step (1) to a specific gravity of 1.20-1.40 g/ml to obtain a primary concentrated solution, vacuum concentrating the secondary supernatant obtained in the step (2) to a specific gravity of 0.95-1.10 g/ml to obtain a secondary concentrated solution, and vacuum concentrating the tertiary supernatant obtained in the step (3) to a specific gravity of 1.08-1.26 g/ml to obtain a tertiary concentrated solution for later use;

(5) adding maltodextrin into the first concentrated solution according to the weight ratio of 1:0.6-0.8, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder A, mixing the second concentrated solution and the third concentrated solution, weighing hydroxypropyl-beta-cyclodextrin according to the weight ratio of 1:0.3-0.4 to prepare into saturated aqueous solution, stirring and mixing, standing at room temperature after ultrasonic treatment, carrying out plate-and-frame filter pressing, collecting filtrate, adding maltodextrin according to the weight ratio of 1:0.3-0.4, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder B;

(6) and fully mixing the dry powder A, the dry powder B, microcrystalline cellulose, mannitol, citric acid and magnesium stearate, and tabletting to obtain the blueberry active ingredient embedded substance with high bioavailability.

The blueberry active ingredient inclusion compound for improving bioavailability is characterized in that the hot reflux extraction conditions in the step (1) are as follows: the temperature is 70-90 ℃, the time is 100-140 min/time, and the ratio of leaching materials to leaching liquids is 1: 8-1: 10 w/v.

The blueberry active ingredient inclusion compound for improving bioavailability is characterized in that in the step (2), the acidified ethanol solution is prepared by adjusting the pH value of 50-70% ethanol to 2.5-3.5 through glacial acetic acid, and the extraction conditions of the acidified ethanol solution are as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 5-1: 7 w/v.

The blueberry active ingredient embedded substance capable of improving bioavailability is characterized in that the ethyl acetate leaching conditions in the step (3) are as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 3-1: 5 w/v.

A preparation method of a blueberry active ingredient inclusion compound for improving bioavailability is characterized by comprising the following steps:

(1) crushing dried blueberries to 30-60 meshes, uniformly mixing, carrying out hot reflux extraction by using distilled water as a solvent, cooling to room temperature after extraction, carrying out plate-and-frame filter pressing, and respectively collecting primary supernatant and primary filter residues;

(2) leaching the first filter residue obtained in the step (1) by using an acidified ethanol solution, cooling to room temperature after leaching is finished, performing plate-and-frame filter pressing, and respectively collecting second supernatant and second filter residue;

(3) leaching the second filter residue obtained in the step (2) with ethyl acetate, cooling to room temperature after leaching is completed, performing plate-and-frame filter pressing, and collecting supernatant liquid of the third time respectively;

(4) vacuum concentrating the primary supernatant obtained in the step (1) to a specific gravity of 1.20-1.40 g/ml to obtain a primary concentrated solution, vacuum concentrating the secondary supernatant obtained in the step (2) to a specific gravity of 0.95-1.10 g/ml to obtain a secondary concentrated solution, and vacuum concentrating the tertiary supernatant obtained in the step (3) to a specific gravity of 1.08-1.26 g/ml to obtain a tertiary concentrated solution for later use;

(5) adding maltodextrin into the first concentrated solution according to the weight ratio of 1:0.6-0.8, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder A, mixing the second concentrated solution and the third concentrated solution, weighing hydroxypropyl-beta-cyclodextrin according to the weight ratio of 1:0.3-0.4 to prepare into saturated aqueous solution, stirring and mixing, standing at room temperature after ultrasonic treatment, carrying out plate-and-frame filter pressing, collecting filtrate, adding maltodextrin according to the weight ratio of 1:0.3-0.4, uniformly stirring, then carrying out vacuum freeze drying to obtain dry powder B;

(6) and fully mixing the dry powder A, the dry powder B, microcrystalline cellulose, mannitol, citric acid and magnesium stearate, and tabletting to obtain the blueberry active ingredient embedded substance with high bioavailability.

The preparation method of the blueberry active ingredient inclusion compound for improving the bioavailability is characterized in that the hot reflux extraction conditions in the step (1) are as follows: the temperature is 70-90 ℃, the time is 100-140 min/time, and the ratio of leaching materials to leaching liquids is 1: 8-1: 10 w/v.

The preparation method of the blueberry active ingredient inclusion compound for improving the bioavailability is characterized in that the pH of 50-70% ethanol in the acidified ethanol solution in the step (2) is adjusted to 2.5-3.5 through glacial acetic acid to prepare the blueberry active ingredient inclusion compound.

The preparation method of the blueberry active ingredient inclusion compound for improving the bioavailability is characterized in that the extraction conditions of the acidified ethanol solution in the step (2) are as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 5-1: 7 w/v.

The preparation method of the blueberry active ingredient embedded substance for improving bioavailability is characterized in that the ethyl acetate leaching conditions in the step (3) are as follows: the leaching temperature is 70-90 ℃, the leaching time is 100-140 min/time, and the leaching material-liquid ratio is 1: 3-1: 5 w/v.

The preparation method of the blueberry active ingredient inclusion compound for improving bioavailability is characterized in that the method for inclusion of hydroxypropyl-beta-cyclodextrin in the step (5) specifically comprises the following steps:

(a) dissolving hydroxypropyl-beta-cyclodextrin in water to obtain a saturated solution of hydroxypropyl-beta-cyclodextrin;

(b) mixing the first concentrated solution and the second concentrated solution, and slowly adding into the hydroxypropyl-beta-cyclodextrin saturated solution while continuously stirring;

(c) performing ultrasonic treatment for 20min, standing at room temperature for 24h, performing plate and frame filter pressing, and collecting filtrate.

The invention has the following beneficial effects: according to the invention, the blueberry active substances have different polarities, and are extracted in a segmented manner and embedded in a segmented manner, so that the bioavailability of the blueberry active substances is effectively improved.

Detailed Description

The present invention will be further illustrated by the following examples.