CN107582430B - Preparation and application method of highland barley beta-glucan-polyaspartic acid compound - Google Patents
Preparation and application method of highland barley beta-glucan-polyaspartic acid compound Download PDFInfo
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- CN107582430B CN107582430B CN201711054169.5A CN201711054169A CN107582430B CN 107582430 B CN107582430 B CN 107582430B CN 201711054169 A CN201711054169 A CN 201711054169A CN 107582430 B CN107582430 B CN 107582430B
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Abstract
The invention discloses a preparation and application method of highland barley beta-glucan-polyaspartic acid compound, which comprises the following steps: after the highland barley beta-glucan and the polyaspartic acid are fully swelled and dissolved by water, ethylene glycol or glycerol is added to react for a period of time at the temperature of 80-100 ℃, reaction liquid is subjected to freeze drying, and freeze-dried powder is placed in the environment with the temperature of 55-85 ℃, the relative humidity of 65-85% and saturated potassium bromide or saturated potassium iodide solution to react for 10-20 days, so that the highland barley beta-glucan-polyaspartic acid compound is obtained. The compound can be applied to the fields of cosmetics and moisturizing agents and medicines such as biological adhesion preparations. The invention has the advantages that: the compound has good moisture retention performance and biological adhesion performance.
Description
Technical Field
The invention relates to the technical field of biological medicines, in particular to a preparation and application method of a highland barley beta-glucan-polyaspartic acid compound.
Background
The highland barley beta-glucan is a high molecular non-starch polysaccharide extracted from highland barley, and the chemical structure of the highland barley beta-glucan is a polymer formed by glucose units through beta- (1 → 3) and beta- (1 → 4) glycosidic bonds. The highland barley beta-glucan has certain water absorption and viscoelasticity, so the highland barley beta-glucan has potential application in cosmetic moisturizing agents and bioadhesive pharmaceutical preparations.
Polyaspartic acid is a polyamino acid whose structure is a polymer of aspartic acid units formed by peptide bonds. Polyaspartic acid has strong water absorption, is often used for synthesizing super absorbent resin, and is also used as a cosmetic moisturizing agent.
The highland barley beta-glucan and the polyaspartic acid are prepared into a compound through proper reaction, certain properties of the highland barley beta-glucan can be improved, and the application field of the highland barley beta-glucan is expanded, but the preparation and application method of the highland barley beta-glucan-polyaspartic acid compound is not available in the prior art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation and application method of a highland barley beta-glucan-polyaspartic acid compound, which can effectively solve the problems in the prior art.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of highland barley beta-glucan-polyaspartic acid compound comprises the following steps:
step 1, taking 5-9 parts of highland barley beta-glucan and 0.5-3 parts of polyaspartic acid according to the weight part ratio range;
step 2, adding 100-200 parts by weight of water, and stirring for 10-15 hours to fully swell and dissolve;
step 3, adding ethylene glycol accounting for 5-15% of the weight of the highland barley beta-glucan, controlling the temperature to be 80-100 ℃, keeping the temperature constant, stirring for 4-8 hours, and cooling;
step 4, freeze-drying the reaction solution to obtain freeze-dried powder;
and 5, placing the freeze-dried powder in a constant-temperature closed container, controlling the temperature to be 55-85 ℃, keeping the temperature constant, keeping the relative humidity to be 65-85%, placing a saturated potassium bromide or saturated potassium iodide solution at the bottom of the container, and placing for 10-20 days.
Preferably, the ethylene glycol described in step 3 is replaced with glycerol.
The invention also discloses an application formula of the highland barley beta-glucan-polyaspartic acid compound, which is applied to a humectant of cosmetics and a medicinal auxiliary material which is used as a biological adhesive and applied to biological adhesive preparation medicines.
Compared with the prior art, the invention has the advantages that: improves the performance of the highland barley beta-glucan, and prepares a new compound (namely the highland barley beta-glucan-polyaspartic acid compound), and the compound has strong biological adhesion and strong moisture-preserving capability.
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 by the following embodiments.
Example 1
Taking 6 parts of highland barley beta-glucan and 1 part of polyaspartic acid, adding 180 parts of water, stirring at 100rpm for 12 hours, adding 0.5 part of glycerol, stirring at 90 ℃ and 100rpm for 5 hours, then freeze-drying the reaction solution, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 75 ℃ and the relative humidity at 80%, placing a saturated potassium bromide solution at the bottom of the container, and placing at constant temperature for 15 days.
Example 2:
taking 8 parts of highland barley beta-glucan and 1.5 parts of polyaspartic acid, adding 200 parts of water, stirring at 100rpm for 15 hours, adding 0.8 part of ethylene glycol, stirring at 80 ℃ and 100rpm for 6 hours, then freeze-drying the reaction solution, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 65 ℃ and the relative humidity at 70%, placing a saturated potassium bromide solution at the bottom of the container, and standing at constant temperature for 20 days.
Example 3:
taking 6 parts of highland barley beta-glucan and 1 part of polyaspartic acid, adding 150 parts of water, stirring at 100rpm for 11 hours, adding 0.9 part of glycerol, stirring at 85 ℃ and 100rpm for 6 hours, then freeze-drying the reaction solution, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 70 ℃ and the relative humidity at 82%, placing a saturated potassium iodide solution at the bottom of the container, and standing at constant temperature for 12 days.
Example 4:
a moisturizing essence: taking 2.0g of highland barley beta-glucan-polyaspartic acid compound, 0.5g of D-panthenol, 1.0g of aloe extract, 1.0g of licorice extract, 3.0g of water-soluble agastache/bave oil, 0.5g of magnesium ascorbyl phosphate, 5.0g of 1, 4-butanediol, 0.1g of xanthan gum, 0.2g of allantoin, 2.0g of caprylyl glycol and 84.7g of water, and preparing 100g of essence.
Example 5:
a bioadhesive tablet: taking 5.0g of ginseng extract (or other traditional Chinese medicine extract), 8.0g of highland barley beta-glucan-polyaspartic acid compound, 1.0g of polyvinylpyrrolidone, 8.0g of microcrystalline cellulose and 8.0g of lactose, and preparing into 100 tablets.
Examination of reaction effect:
the effect of the reaction was evaluated according to the literature method (Kato A, Sasaki Y, Furuta R, et al. functional protein-polysaccharide conjugate prepared by controlled drive-height of the above-mentioned methods, Agricaultural and Biological Chemistry,1990,54(1):107-112.), the absorbance at 470nm of the product of the partial reaction or the complete reaction of the present invention was determined and compared with the absorbance at 470nm of the product of the reaction of glucose with polyaspartic acid, and the calculation was carried out according to the following formula:
R＝(Asample/AGlc)×100％
wherein R is a ratio of the degree of reaction (the reaction is completed as the value is larger), and AsampleThe absorbance of the partial reaction or complete reaction product at 470nm, AGlcIs the absorbance at 470nm of the reaction product of glucose and polyaspartic acid.
Determination of reaction product of glucose and polyaspartic acid: taking 6.0g of glucose and 1.0g of polyaspartic acid, adding 180ml of water, stirring at 100rpm for 12h, adding 0.5g of glycerol, stirring at 90 ℃ and 100rpm for 5h, then freeze-drying the reaction solution, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 75 ℃ and the relative humidity at 80%, placing a saturated potassium bromide solution at the bottom of the container, and standing at constant temperature for 15 d. Taking the reaction product to prepare 10mg/ml aqueous solution, and measuring A at 470nmGlc。
Firstly, reacting highland barley beta-glucan (adding a cross-linking agent glycerol): taking 6.0g of highland barley beta-glucan and 1.0g of polyaspartic acid, adding 180ml of water, stirring at 100rpm for 12h, adding 0.5g of glycerol, stirring at 90 ℃ and 100rpm for 5h, then freeze-drying the reaction solution, taking the freeze-dried powder to prepare 10mg/ml aqueous solution, measuring A at 470nmsampleThe R value was calculated, and as a result, R was 23.7%.
② highland barley beta-glucan reaction II (dry heat treatment): taking 6.0g of highland barley beta-glucan and 1.0g of polyaspartic acid, adding 180ml of water, stirring at 100rpm for 12h, then freeze-drying, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 75 ℃ and the relative humidity at 80%, placing a saturated potassium bromide solution at the bottom of the container, and standing at constant temperature for 15 d. Taking the reaction product to prepare 10mg/ml aqueous solution, and measuring A at 470nmsample. Calculation of RThe result, R, was 41.3%.
③ reacting the highland barley beta-glucan: taking 6.0g of highland barley beta-glucan and 1.0g of polyaspartic acid, adding 180ml of water, stirring at 100rpm for 12 hours, adding 0.5g of glycerol, stirring at 90 ℃ and 100rpm for 5 hours, then freeze-drying the reaction solution, placing the freeze-dried powder in a constant-temperature closed container, keeping the temperature at 75 ℃ and the relative humidity at 80%, placing a saturated potassium bromide solution at the bottom of the container, and standing at constant temperature for 15 days. Taking the reaction product to prepare 10mg/ml aqueous solution, and measuring A at 470nmsample. The R value was calculated and found to be 73.6%.
The experimental results show that the reaction degree of the highland barley beta-glucan and the polyaspartic acid is lower than that of the reaction of adding glycerol and carrying out dry heat treatment only by adding the cross-linking agent glycerol or carrying out the dry heat treatment only.
In addition, experiments show that in the above "reaction three", the result is similar when glycerol is replaced by ethylene glycol and potassium bromide is replaced by potassium iodide, and R is 71.9%.
Moisture retention study of the product:
the moisture absorption and retention capacity of highland barley beta-glucan, polyaspartic acid and highland barley beta-glucan-polyaspartic acid compound is measured according to the literature method (Gaorui, Zhang Xiuyu, Mudan, and the like, measurement of moisture absorption and retention performance of bioactive polysaccharide for cosmetics such as hyaluronic acid, and the like, Guangdong chemical industry, 2009,36(10): 230-. Moisture absorption rate when left in an environment with a relative humidity of 81% for 72 hours: 16.1 percent of highland barley beta-glucan, 22.4 percent of polyaspartic acid and 34.6 percent of compound; moisture absorption rate when left in an environment with a relative humidity of 43% for 72 hours: 6.6 percent of highland barley beta-glucan, 7.4 percent of polyaspartic acid and 8.2 percent of compound. Moisture retention rate of 72h of silica gel desiccant treatment: 58.7 percent of highland barley beta-glucan, 66.3 percent of polyaspartic acid and 75.8 percent of compound.
The experiment result shows that the moisture absorption and retention capacity of the highland barley beta-glucan-polyaspartic acid compound is stronger than that of the highland barley beta-glucan and polyaspartic acid.
Bioadhesive investigation of the product:
respectively taking highland barley beta-glucan, polyaspartic acid and highland barley beta-glucan-polyaspartic acid compound as adhesives, and preparing the adhesive into tablets according to the following formula: 6g of adhesive, 12g of dextrin and 12g of lactose, and preparing 100 tablets in total. Tablets prepared according to the formulation without addition of adhesive (15 g dextrin, 15g lactose, made up to 100 tablets in total) were used as reference. The bioadhesion was measured according to the literature (study on the in vitro tissue adhesion and release of the Gegen Total Flavonoids bioadhesive sustained release tablet in great Male, Lihuan, Rojiying, et al. China pharmacy 2002,13(8): 459) 461.), and as a result, the adhesivity to the rabbit in vitro small intestine tissue was 0g/cm2 for the tablet without the addition of the adhesive, 5.3g/cm2 for the tablet made of highland barley beta-glucan, 6.8g/cm2 for the tablet made of polyaspartic acid, and 10.6g/cm2 for the tablet made of highland barley beta-glucan-polyaspartic acid complex.
The experimental result shows that the biological adhesion of the highland barley beta-glucan-polyaspartic acid compound is stronger than that of the highland barley beta-glucan and polyaspartic acid.
It will be appreciated by those of ordinary skill in the art that the examples described herein are intended to assist the reader in understanding the manner in which the invention is practiced, and it is to be understood that the scope of the invention is not limited to such specifically recited statements and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (4)
1. A preparation method of highland barley beta-glucan-polyaspartic acid compound is characterized by comprising the following steps:
step 1, taking 5-9 parts of highland barley beta-glucan and 0.5-3 parts of polyaspartic acid according to the weight part ratio range;
step 2, adding 100-200 parts by weight of water, and stirring for 10-15 hours to fully swell and dissolve;
step 3, adding ethylene glycol accounting for 5-15% of the weight of the highland barley beta-glucan, controlling the temperature to be 80-100 ℃, keeping the temperature constant, stirring for 4-8 hours, and cooling;
step 4, freeze-drying the reaction solution to obtain freeze-dried powder;
and 5, placing the freeze-dried powder in a constant-temperature closed container, controlling the temperature to be 55-85 ℃, keeping the temperature constant, keeping the relative humidity to be 65-85%, placing a saturated potassium bromide or saturated potassium iodide solution at the bottom of the container, and placing for 10-20 days.
2. The method for preparing highland barley beta-glucan-polyaspartic acid compound as claimed in claim 1, wherein the method comprises the following steps: replacing the ethylene glycol described in step 3 with glycerol.
3. The method for preparing highland barley beta-glucan-polyaspartic acid compound as claimed in claim 1 or 2, wherein the method comprises the following steps: the compound is applied to a moisturizing agent of cosmetics.
4. The method for preparing highland barley beta-glucan-polyaspartic acid compound as claimed in claim 1 or 2, wherein the method comprises the following steps: the compound is used as a biological adhesive and is applied to pharmaceutic adjuvants of biological adhesive preparation medicines.
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| US20140236082A1 (en) * | 2002-03-15 | 2014-08-21 | Abbott Cardiovascular Systems Inc. | Biocompatible Carrier Containing A Bioadhesive Material |
| CN104592522A (en) * | 2014-10-30 | 2015-05-06 | 中山大学 | Degradable acid-sensitive polyaspartamide copolymer and its preparation method and use |
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| US20140236082A1 (en) * | 2002-03-15 | 2014-08-21 | Abbott Cardiovascular Systems Inc. | Biocompatible Carrier Containing A Bioadhesive Material |
| CN103463453A (en) * | 2013-09-04 | 2013-12-25 | 贵州仙草生物科技有限公司 | Dendrobium stem tablets and extraction and preparation methods thereof |
| CN104592522A (en) * | 2014-10-30 | 2015-05-06 | 中山大学 | Degradable acid-sensitive polyaspartamide copolymer and its preparation method and use |
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| 以青稞β-葡聚糖为基质的白藜芦醇鼻用凝胶剂研究;杨文宇等;《中国实验方剂学杂志》;20110630;第17卷(第12期);第6-11页 * |
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