Glycerophosphorylcholine-collagen peptide microcapsule as well as preparation method and application thereof

Abstract

The invention provides a glycerophosphorylcholine-collagen peptide microcapsule and a preparation method and application thereof.The glycerophosphorylcholine-collagen peptide microcapsule takes glycerophosphorylcholine as a core material and takes a compound formed by polysaccharide containing galacturonic acid and hydrolyzed collagen peptide as a wall material, the preparation method comprises the following steps: preparing a glycerophosphorylcholine solution, activating polysaccharide containing galacturonic acid, reacting hydrolyzed collagen peptide with the polysaccharide containing galacturonic acid to prepare a wall material solution, homogenizing the glycerophosphorylcholine solution and the wall material solution, and performing spray drying to obtain the microcapsule. The microcapsule is applied to fruit juice beverages, oral liquid, solid beverages and tablets. By wrapping the glycerophosphorylcholine in the wall material, the problems that the glycerophosphorylcholine is easy to absorb moisture and poor in acid-base stability are solved.

Description

Technical Field

[0001] The present application belongs to the field of food technology, and specifically relates to a glycerol phosphorylcholine-collagen peptide microcapsule and a preparation method and application thereof. Background Art

[0002] Glycerophosphatidylcholine (GPC), also known as glycerophosphatidylcholine, is one of the products of phospholipid metabolism in the body and is also a biosynthetic precursor of the important neurotransmitter acetylcholine. Glycerophosphatidylcholine is less distributed in plants. In the body, the most important physiological function of GPC is to cross the blood-brain barrier and provide the necessary choline for the biosynthesis of acetylcholine and phosphatidylcholine (PC). Acetylcholine is an important neurotransmitter in the central nervous system, helping the brain complete learning, memory and cognitive activities, and can control light sleep and motor activity.

[0003] The research and development of anti-dementia drugs has attracted great attention from the medical community of all countries in the world. In recent years, with the continuous deepening of research on the neurophysiology, biochemistry, and pharmacology of the elderly, the development and research of related drugs have made continuous progress. Glycerylphosphorylcholine can be called the "transporter" of choline and the "pioneer" of phosphate choline. It has the potential to prevent and treat various biochemical lesions, and has the unique effect of reducing body tension and changing the structure of phosphate lipid compounds in neuronal membranes.

[0004] Chinese patent application number 202410519134.8 discloses a method for preparing deoiled egg yolk powder rich in glycerolphosphatidylcholine, which takes fresh poultry egg yolk liquid rich in phosphatidylcholine as the starting material, adds water in a certain proportion, takes the supernatant after centrifugation, and obtains a reaction liquid rich in glycerolphosphatidylcholine through composite enzymolysis with phospholipase A1 and lysophospholipase, and then obtains the target product through spray drying and supercritical CO2 extraction.

[0005] The Chinese patent application number 202180008381.6 discloses a dietary supplement composition containing collagen, and the dietary supplement composition of the invention contains collagen (preferably in the form of hydrolyzed collagen peptides) in combination with branched-chain amino acids (BCAA), creatine nitrate, arginine nitrate, N-acetyl-L-carnitine, L-citrulline, anhydrous betaine, α-glycerophosphorylcholine, ancient peat extract containing apple fruit extract, and caffeine.

[0006] Chinese patent application number 201210050798.1 discloses a soft capsule for improving brain nerve function and a preparation method thereof. The soft capsule comprises two parts: contents and capsule shell material. The contents comprise glycerol phosphoryl choline and solvent, wherein the glycerol phosphoryl choline accounts for 60-95% of the total weight of the contents, and the solvent accounts for 5-40% of the total weight of the contents. The solvent comprises one or more of water, glycerol, sorbitol, anhydrous sorbitol, triacetin, polyethylene glycol 200, polyethylene glycol 400, and propylene glycol. The capsule shell material comprises one or more of gelatin, water, glycerol, sorbitol, anhydrous sorbitol, sodium methyl paraben, sodium ethyl paraben, sodium propyl paraben, titanium dioxide, and yellow iron oxide. The preparation method comprises the following steps: a solution A made of glycerol phosphoryl choline and solvent and a solution B made of capsule shell material are passed through a soft capsule machine to be pressed into soft capsules, and then dried to obtain the soft capsules.

[0007] However, glycerylphosphorylcholine is highly hygroscopic. It is very easy to absorb moisture in the development of tablets, granules and solid beverages, which makes the finished product extremely easy to absorb moisture during the shelf life, thus causing the product to be unstable. At the same time, glycerylphosphorylcholine is stable in neutral water, but its potency gradually decreases in acidic or alkaline conditions, especially in alkaline solutions. In the development of fruit juice drinks, oral liquids, solid beverages, and suspensions, the above-mentioned instability of glycerylphosphorylcholine is a problem that needs to be solved urgently. Summary of the invention

[0008] In view of the problems existing in the prior art, the present invention provides a glyceryl phosphorylcholine-collagen peptide microcapsule and a preparation method thereof. The microcapsule has a capsule shell structure, with glyceryl phosphorylcholine as a core material, and a mesh complex formed by a polysaccharide containing galacturonic acid and a hydrolyzed collagen peptide as a wall material. The microcapsule is embedded by homogenization and drying to prepare the glyceryl phosphorylcholine-collagen peptide microcapsule. Due to the unique capsule shell structure of the microcapsule, the problems of easy moisture absorption and poor acid-base stability of glyceryl phosphorylcholine are solved.

[0009] The present invention is achieved through the following technical solutions.

[0010] The first object of the present invention is to provide a glycerylphosphorylcholine-collagen peptide microcapsule, which has a core-shell structure, wherein glycerylphosphorylcholine is used as a core material to form a microcapsule core, and a complex formed by a polysaccharide containing galacturonic acid and a hydrolyzed collagen peptide is used as a wall material to form a microcapsule shell, wherein the weight ratio of the core material to the wall material is 1:1-20, preferably 1:1-10, and the weight ratio of the hydrolyzed collagen peptide to the polysaccharide containing galacturonic acid is 1:1-10, preferably 1:1-5.

[0011] As a further technical solution, the polysaccharide containing galacturonic acid is any one or more of soluble soybean polysaccharide, citrus fiber, soybean fiber, apple fiber, beet fiber, and chicory fiber.

[0012] As a further technical solution, any one of the polysaccharides containing galacturonic acid is selected; any two of the polysaccharides containing galacturonic acid are selected, and the weight ratio of the two polysaccharides is 1:1-10; any three of the polysaccharides containing galacturonic acid are selected, and the weight ratio of the three polysaccharides is 1:1-10:1-10.

[0013] As a further technical solution, the reaction temperature of the composite is 25-85° C., preferably 45-65° C., and the reaction time is 0.5-10 hours, preferably 2-4 hours.

[0014] As a further technical solution, the core-shell structure is achieved by spray drying, the injection port temperature of the spray drying is 150-200°C, preferably 175-195°C, and the outlet temperature is 60-120°C, preferably 80-100°C.

[0015] The second object of the present invention is to provide a method for preparing the above-mentioned glycerol phosphorylcholine-collagen peptide microcapsules, the method comprising: S1. preparing a glycerol phosphorylcholine solution; S2, swelling the polysaccharide containing galacturonic acid in water, and adjusting the acidity of the swelling solution to activate it; dissolving the hydrolyzed collagen peptide in the activated swelling solution, and then adjusting the pH to 3.5-6.5, preferably 4.5-5.5, heating to 25-95° C., preferably 40-60° C., and keeping warm for 0.5-10 hours, preferably 2-4 hours, to obtain a wall material solution; S3, mixing the glycerol phosphorylcholine solution and the wall material solution, adjusting the pH to 3.5-6.5, preferably 4.5-5.5, and homogenizing the acid-adjusted solution; S4. The homogenized solution is spray-dried to obtain glycerol phosphorylcholine-collagen peptide microcapsules.

[0016] As a further technical solution, in step S2, the polysaccharide containing galacturonic acid is any one or more of soluble soybean polysaccharide, citrus fiber, soybean fiber, apple fiber, beet fiber, and chicory fiber, the weight ratio of the polysaccharide containing galacturonic acid to water is 1:5-30, preferably 1:10-20, and the weight ratio of the hydrolyzed collagen peptide to the polysaccharide containing galacturonic acid is 1:1-20, preferably 1:1-10, calculated on a dry matter basis.

[0017] As a further technical solution, in step S2, the acid adjustment and activation treatment process of the swelling liquid is: adjusting the pH of the swelling liquid to 2.0-6.0, preferably 3-5, heating to 25-95°C, preferably 45-75°C, and keeping warm for 0.5-10 hours, preferably 2-4 hours, and the acid adjustment solvent is any one or more of lactic acid, citric acid, tartaric acid, acetic acid, and sodium citrate.

[0018] As a further technical solution, in step S3, based on dry matter, the weight ratio of glycerolphosphorylcholine to wall material is 1:1-20, preferably 1:1-10, the homogenization temperature is 25-90°C, preferably 45-75°C, the homogenization pressure is 5-30 MPa, preferably 15-25 MPa, and the homogenization time is 1-30 minutes, preferably 5-15 minutes.

[0019] As a further technical solution, in step S3, a liquid microcapsule suspension is obtained after homogenization.

[0020] As a further technical solution, in step S1, the concentration of the glycerol phosphorylcholine solution is 50%-90%, preferably 75-85%.

[0021] As a further technical solution, in step S4, the injection port temperature of the spray drying is 150-200°C, preferably 175-195°C, and the outlet temperature is 60-120°C, preferably 80-100°C.

[0022] The third object of the present invention is to provide a glycerol phosphorylcholine-collagen peptide microcapsule and the use of the glycerol phosphorylcholine-collagen peptide microcapsule prepared by the above preparation method in fruit juice drinks, oral liquids, solid drinks and compressed tablets.

[0023] Compared with the prior art, the present invention has the following advantages and beneficial effects.

[0024] 1. The glycerol phosphorylcholine-collagen peptide microcapsules provided by the present invention use a complex formed by a polysaccharide containing galacturonic acid and a hydrolyzed collagen peptide as a wall material to encapsulate glycerol phosphorylcholine, and external small molecules such as water or solvents cannot enter the interior of the shell, thereby solving the defects of glycerol phosphorylcholine's moisture absorption and acid-base instability.

[0025] 2. The polysaccharide containing galacturonic acid carries negative charge, and the hydrolyzed collagen peptide carries positive charge. When heated, the two form a wall material with a network structure, which is then spray dried to form a spherical embedding. Spray drying evaporates the water wrapped in the wall material at the same time, and the glycerolphosphorylcholine is retained in the shell to protect the glycerolphosphorylcholine.

[0026] 3. The polysaccharides containing galacturonic acid are selected from soluble soybean polysaccharides and fiber substances. The selected soluble soybean polysaccharides and fiber substances are both high-quality dietary fibers. Hydrolyzed collagen peptides are the hydrolyzate of collagen and are small molecule polypeptides, which are easy for human body to digest. When glyceryl phosphorylcholine-collagen peptide microcapsules are used in fruit juice drinks, oral liquids, solid drinks and compressed tablets, the hydrolyzed collagen peptides and the polysaccharides containing galacturonic acid have synergistic effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The electron microscope of the glycerol phosphorylcholine-collagen peptide microcapsule of the present invention Figure 1 .

[0028] Figure 2 The electron microscope of the glycerol phosphorylcholine-collagen peptide microcapsule of the present invention Figure 2 . DETAILED DESCRIPTION

[0029] In order to better understand the present invention, the glycerol phosphorylcholine-collagen peptide microcapsules and the preparation method and application thereof of the present invention are described in detail below in combination with examples and comparative examples.

[0030] The purpose of the present invention is to solve the problems of glycerol phosphorylcholine being easy to absorb moisture and having poor acid-base stability by preparing a glycerol phosphorylcholine-collagen peptide microcapsule with a core-shell structure. Glycerol phosphorylcholine is used as a core material, and a mesh complex formed by a polysaccharide containing galacturonic acid and a hydrolyzed collagen peptide is used as a wall material. Glycerol phosphorylcholine is wrapped inside the wall material. The mesh structure formed by the wall material prevents small molecules from outside, such as water molecules or other solvents, from entering the shell. Since small molecules from outside cannot contact glycerol phosphorylcholine, the stability and potency of glycerol phosphorylcholine are guaranteed. In addition, the galacturonic acid-containing microcapsule contains The polysaccharides used are soluble soybean polysaccharides and fiber substances. The soluble soybean polysaccharides and fiber substances used are both high-quality dietary fibers, which have the benefits of regulating the gastrointestinal tract, losing weight, preventing and treating diabetes, preventing and treating cardiovascular diseases, and relieving constipation. Another component of the wall material is hydrolyzed collagen peptides, which are the hydrolyzates of collagen and are small molecule polypeptides. Hydrolyzed collagen peptides can be directly absorbed by the epithelial cells of the small intestinal villi, making them easy for the human body to digest. Hydrolyzed collagen peptides have multiple biological effects such as anti-oxidation, anti-inflammatory, and promoting fibroblast proliferation. Hydrolyzed collagen peptides synergize with polysaccharides containing galacturonic acid.

[0031] It should be noted that the experimental methods used in the examples are conventional methods unless otherwise specified. The materials, reagents, methods and instruments used are conventional materials, reagents, methods and instruments in the art unless otherwise specified, and can be obtained by those skilled in the art through commercial channels.

[0032] Equipment: YC-015 small spray dryer Shanghai Yacheng Instrument Equipment Co., Ltd.

[0033] The molecular weight of the hydrolyzed collagen peptide used is 500-5000 Daltons, preferably 1000-3000 Daltons.

[0034] Example 1 A method for preparing glycerol phosphorylcholine-collagen peptide microcapsules, the method comprising: S1. Prepare core material solution: add glycerol phosphorylcholine to distilled water, stir and dissolve evenly to form a glycerol phosphorylcholine solution with a concentration of 50%; S2. Prepare wall material solution: add soybean fiber to distilled water, stir and swell, the weight ratio of soybean fiber to distilled water is 1:5, adjust the pH of the swelling solution to 6.0 with citric acid, heat to 25°C and keep warm for 0.5 hours, so that the original pectin molecules in the soybean fiber are Ca 2+ Mg 2+ Insoluble carboxylates in the form of activated partially hydrophilic carboxylic acids and carboxylates.

[0035] Dissolve hydrolyzed collagen peptide (molecular weight 1000 Dalton) in the activated soybean fiber solution, the weight ratio of hydrolyzed collagen peptide to soybean fiber is 1:1 based on dry matter, adjust the pH to 6.5 with sodium citrate solution so that the amino group of the collagen peptide carries positive charge, heat to 25°C, keep warm for 0.5 hour, so that the amino group of the collagen peptide carries positive charge and the negative charge carried by the carboxyl group on the galacturonic acid of the soybean fiber forms a network structure, and prepare a wall material solution; S3, the core material solution and the wall material solution are mixed and homogenized: the glycerophosphorylcholine solution prepared in step 1 is added to the wall material solution prepared in step 2, and stirred evenly. The weight ratio of glycerophosphorylcholine to the wall material is 1:1 based on dry matter. Sodium citrate is used to adjust the pH to 6.5. The mixed solution after acid adjustment is poured into the processing chamber of the homogenizing equipment for homogenization to obtain a liquid microcapsule suspension. The homogenization conditions are: the preheating temperature of the homogenizing equipment is 25°C, the homogenization pressure is 5MPa, and the homogenization time is 1 minute; S4, spray drying: spray drying the homogenized solution in step 3, the wall material forms a spherical embedding of the core material, and the glycerol phosphorylcholine-collagen peptide microcapsule powder is prepared. The spray drying conditions are: the injection port temperature is 150°C, the outlet temperature is 60°C, and the injection speed is 1L / hour.

[0036] The glyceryl phosphorylcholine-collagen peptide microcapsules prepared by the above steps have a weight ratio of core material to wall material of 1:1, a weight ratio of hydrolyzed collagen peptide to soybean fiber of 1:1, a moisture content of 5.0%, an embedding rate of glyceryl phosphorylcholine in the microcapsules of 30.1%, and after a hygroscopicity test, the microcapsules are slightly clumped, with a weight gain percentage of 14.8%.

[0037] Embodiment 2-8 A method for preparing glycerol phosphorylcholine-collagen peptide microcapsules. The process of the method is the same as that of Example 1. The wall material type, ratio parameters, and control parameters of the preparation process in the process are shown in Table 1.

[0038] The embedding rate, moisture content, state of the microcapsules after the hygroscopicity test and weight gain percentage of the glycerol phosphorylcholine-collagen peptide microcapsules prepared by the method of Examples 2-8 are shown in Table 2.

[0039] Comparative Example A glycerol phosphorylcholine solution with a concentration of 50% was prepared and poured into the processing chamber of the homogenizer. The preheating temperature of the homogenizer was 60°C, the homogenization pressure was 25 MPa, and the homogenization time was 10 minutes. The homogenized solution was spray dried to obtain solid glycerol phosphorylcholine. The spray drying conditions were: inlet temperature 190°C, outlet temperature 80°C, and injection speed 1 L / hour. The moisture content of the obtained glycerol phosphorylcholine and the state and weight gain percentage of the microcapsules after the hygroscopicity test are shown in Table 2.

[0040] Table 1 Group Glycerylphosphorylcholine solution concentration Wall material type and weight ratio Fiber activation parameters Process parameters of wall material solution The weight ratio of the core material to the wall material, and the pH of the core material solution and the wall material solution after mixing Homogenization process parameters Process parameters of spray drying Example 1 50% Hydrolyzed collagen peptides: soy fiber 1:1 The weight ratio of soybean fiber to distilled water is 1:5, the pH is adjusted to 6.0 with citric acid, and the temperature is kept at 25℃ for 0.5 hours pH 6.5, 25℃ for 0.5 hours 1:1, pH 6.5 The preset temperature is 25°C, the homogenization pressure is 5MPa, and the homogenization time is 1 minute. The injection port temperature is 150°C, the outlet temperature is 60°C, and the injection speed is 1L / hour. Example 2 90% Hydrolyzed collagen peptides: citrus fiber 1:10 The weight ratio of citrus fiber to distilled water is 1:30, the pH is adjusted to 2.0 with lactic acid, and the mixture is kept at 95℃ for 10 hours. pH 6.5, 95℃ for 10 hours 1:20, pH 6.5 The preset temperature is 90°C, the homogenization pressure is 30MPa, and the homogenization time is 30 minutes. The injection port temperature is 200°C, the outlet temperature is 120°C, and the injection speed is 0.5L / hour. Example 3 90% Hydrolyzed collagen peptides: apple fiber 1:2 The weight ratio of apple fiber to distilled water is 1:6, tartaric acid is used to adjust the pH to 5.8, and the mixture is kept at 30℃ for 10 hours. pH 3.5, keep warm at 40℃ for 1.5 hours 1:1, pH 3.5 The preset temperature is 45°C, the homogenization pressure is 10MPa, and the homogenization time is 5 minutes. The injection temperature is 200°C, the outlet temperature is 60°C, and the injection speed is 1.8L / hour. Example 4 60% Hydrolyzed collagen peptides: beet fiber 1:6 The weight ratio of beet fiber to distilled water is 1:15, the pH is adjusted to 3.5 with acetic acid, and the mixture is kept at 65℃ for 3 hours pH 5.2, keep warm at 45℃ for 2.5 hours 1:5, pH 4.5 The preset temperature is 48°C, the homogenization pressure is 25MPa, and the homogenization time is 10 minutes. Inlet temperature 150°C, outlet temperature 120°C, injection speed 0.8L / hour Example 5 85% Hydrolyzed collagen peptides: soy fiber: citrus fiber 1:2:2 The weight ratio of citrus fiber, soybean fiber and distilled water is 1:1:25, pH is adjusted to 3.1 with citric acid, and kept at 50℃ for 3 hours pH 5.5, 60℃ for 3 hours 1:5, pH 5.2 The preset temperature is 60°C, the homogenization pressure is 20MPa, and the homogenization time is 8 minutes. The injection port temperature is 180°C, the outlet temperature is 90°C, and the injection speed is 1.5L / hour. Example 6 75% Hydrolyzed collagen peptides: soy fiber: soluble soy polysaccharides are 1:1:1 The weight ratio of soybean fiber, soluble soybean polysaccharide and distilled water is 1:1:35, lactic acid and tartaric acid are used to adjust the pH to 4.0, and the mixture is kept at 70℃ for 4 hours. pH 4.5, 50℃ for 4 hours 1:10, pH 4.8 The preset temperature is 65°C, the homogenization pressure is 18MPa, and the homogenization time is 12 minutes. The injection port temperature is 190°C, the outlet temperature is 70°C, and the injection speed is 1.6L / hour. Example 7 75% Hydrolyzed collagen peptides: citrus fiber: apple fiber: beet fiber 1:1:2:3 The weight ratio of citrus fiber, apple fiber, beet fiber and distilled water is 1:2:3:100, the pH is adjusted to 3.6 with acetic acid, and the mixture is kept at 58℃ for 2.5 hours pH 5.8, 55°C, keep warm for 1 hour 1:8, pH 5.0 The preset temperature is 28°C, the homogenization pressure is 6MPa, and the homogenization time is 2 minutes. The injection port temperature is 185°C, the outlet temperature is 95°C, and the injection speed is 1.8L / hour. Example 8 85% Hydrolyzed collagen peptides: soluble soy polysaccharides: citrus fiber 1:3:1 The weight ratio of soluble soybean polysaccharide, citrus fiber and distilled water is 3:1:40, citric acid and acetic acid are used to adjust the pH to 4.1, and the mixture is kept at 45℃ for 3 hours. pH 4.8, keep warm at 48℃ for 2 hours 1:5, pH 4.8 The preset temperature is 70°C, the homogenization pressure is 21MPa, and the homogenization time is 8 minutes. The injection port temperature is 150°C, the outlet temperature is 60°C, and the injection speed is 1.2L / hour. Comparative Example 50% The preset temperature is 70°C, the homogenization pressure is 25MPa, and the homogenization time is 10 minutes. The injection port temperature is 190°C, the outlet temperature is 80°C, and the injection speed is 1.5L / hour. Table 2 Group Embedding rate Moisture Hygroscopicity (weight gain percentage) Example 1 30.1% 5.0% 14.8%, slight clumping Example 2 38.3% 1.1% 9.6%, slight clumping Example 3 40.2% 4.8% 13.6%, slight clumping Example 4 65.7% 1.5% 9.8%, powder, good fluidity Example 5 80.1% 2.6% 8.0%, powder, excellent fluidity Example 6 82.9% 3.2% 7.8%, powder, excellent fluidity Example 7 65.4% 1.6% 8.2%, powder, good fluidity Example 8 55.3% 5.2% 13.7%, slight clumping Comparative Example 0 3.1% 37.1%, deliquesced and formed liquid It can be seen from Table 2 that the higher the embedding rate of the microcapsule, the weaker the hygroscopicity. From the comparison between the embodiment and the comparative example, it can be seen that the embedded glycerolphosphorylcholine has not deliquesced, while the unembedded glycerolphosphorylcholine has strong hygroscopicity and has deliquesced into a liquid state.

[0041] The embedding rate, water content and hygroscopicity test are all carried out using conventional techniques well known to those skilled in the art.

[0042] The formula for calculating the embedding rate is as follows: R(%)=(1-M / N)×100% Where R is the embedding rate, M is the amount of glycerolphosphorylcholine on the surface of the microcapsule per unit mass, and N is the amount of all glycerolphosphorylcholine in the microcapsule per unit mass.

[0043] Determination of glycerol phosphorylcholine on the surface of microcapsules per unit mass: accurately weigh 30 mg of microcapsule product, and wash quickly three times with 20 mL, 20 mL, and 20 mL of anhydrous ethanol in a 0°C ice-water melting pot to clean the glycerol phosphorylcholine on the surface of the microcapsules. Filter the supernatant, combine the filtrates, and distill under reduced pressure at 30°C and 0.085 MPa vacuum. Dissolve the residue with a small amount of deionized water and transfer it to a 10 mL volumetric flask, fix the volume, and draw a certain amount of solution from it. Use HPLC·ELSD to determine its content. The chromatographic column is C 18 Column (250 mm *4.6 mm, 5 µm), mobile phase acetonitrile-water (60:40), flow rate 0.7 mL min -1 The carrier gas was air, with a flow rate of 3.5 mL min -1 , the drift tube temperature is 110°C. Calculate its mass.

[0044] Determination of all glycerolphosphorylcholine in unit mass of microcapsules: accurately weigh 30 mg of microcapsule product, add deionized water to dissolve it completely, transfer it to a 10 mL volumetric flask, adjust the volume, draw a certain amount of solution from it, and determine its content by HPLC·ELSD. The chromatographic column is C 18 Column (250 mm *4.6 mm, 5 µm), mobile phase acetonitrile-water (60:40), flow rate 0.7 mL min -1 The carrier gas was air, with a flow rate of 3.5 mL min -1 , the drift tube temperature is 110°C. Calculate its mass.

[0045] Hygroscopicity test: Guidelines for hygroscopicity test of drugs in 9103 of the 2020 edition of the Chinese Pharmacopoeia.

[0046] The specific test method is as follows.

[0047] 1. Take a dry stoppered glass weighing bottle (outer diameter 50mm, height 15mm), place it in a suitable 25℃±1℃ constant temperature dryer (with ammonium chloride or ammonium sulfate saturated solution placed at the bottom) or artificial climate box (set temperature 25℃±1℃, relative humidity 80%±2%) one day before the test, and accurately weigh the weight (m1).

[0048] 2. Take an appropriate amount of the test sample and spread it evenly in the above-mentioned weighing bottle. The thickness of the test sample is generally about 1mm. Accurately weigh the weight (m2).

[0049] 3. Open the weighing bottle and place it with the bottle cap under the above constant temperature and humidity conditions for 24 hours.

[0050] 4. Cover the weighing bottle and accurately weigh the weight (m3).

[0051] Percentage of weight gain = (m3-m2) / (m2-m1) × 100%.

[0052] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A glycerylphosphorylcholine-collagen peptide microcapsule, characterized in that: It is a core-shell structure, with glycerylphosphorylcholine as the core material to form the microcapsule core, and a complex formed by a polysaccharide containing galacturonic acid and hydrolyzed collagen peptide as the wall material to form the microcapsule shell, the weight ratio of the core material to the wall material is 1:1-20, preferably 1:1-10, and the weight ratio of the hydrolyzed collagen peptide to the polysaccharide containing galacturonic acid is 1:1-10, preferably 1:1-5.

2. The glycerol phosphorylcholine-collagen peptide microcapsule according to claim 1, characterized in that: The polysaccharide containing galacturonic acid is any one or more of soluble soybean polysaccharide, citrus fiber, soybean fiber, apple fiber, beet fiber and chicory fiber.

3. The glycerol phosphorylcholine-collagen peptide microcapsule according to claim 2, characterized in that: The polysaccharides containing galacturonic acid are selected at any one; the polysaccharides containing galacturonic acid are selected at any two, and the weight ratio of the two polysaccharides is 1:1-10; the polysaccharides containing galacturonic acid are selected at any three, and the weight ratio of the three polysaccharides is 1:1-10:1-10.

4. The glycerol phosphorylcholine-collagen peptide microcapsule according to claim 1 or 2, characterized in that: The reaction temperature of the composite is 25-85° C., preferably 45-65° C., and the reaction time is 0.5-10 hours, preferably 2-4 hours.

5. The glycerol phosphorylcholine-collagen peptide microcapsule according to claim 1 or 2, characterized in that: The core-shell structure is achieved by spray drying, wherein the injection port temperature of the spray drying is 150-200°C, preferably 175-195°C, and the outlet temperature is 60-120°C, preferably 80-100°C.

6. A method for preparing the glyceryl phosphorylcholine-collagen peptide microcapsules according to any one of claims 1 to 5, characterized in that: The method includes: S1. preparing a glycerol phosphorylcholine solution; S2, swelling the polysaccharide containing galacturonic acid in water, and adjusting the acidity of the swelling solution to activate it; dissolving the hydrolyzed collagen peptide in the activated swelling solution, and then adjusting the pH to 3.5-6.5, preferably 4.5-5.5, heating to 25-95° C., preferably 40-60° C., and keeping warm for 0.5-10 hours, preferably 2-4 hours, to obtain a wall material solution; S3, mixing the glycerol phosphorylcholine solution and the wall material solution, adjusting the pH to 3.5-6.5, preferably 4.5-5.5, and homogenizing the acid-adjusted solution; S4. The homogenized solution is spray-dried to obtain glycerol phosphorylcholine-collagen peptide microcapsules.

7. The method according to claim 6, characterized in that In step S2, the polysaccharide containing galacturonic acid is any one or more of soluble soybean polysaccharide, citrus fiber, soybean fiber, apple fiber, beet fiber, and chicory fiber. The weight ratio of the polysaccharide containing galacturonic acid to water is 1:5-30, preferably 1:10-20. On a dry matter basis, the weight ratio of the hydrolyzed collagen peptide to the polysaccharide containing galacturonic acid is 1:1-20, preferably 1:1-10.

8. The method according to claim 6 or 7, characterized in that: In step S2, the acid adjustment and activation treatment process of the swelling liquid is as follows: the pH of the swelling liquid is adjusted to 2.0-6.0, preferably 3-5, heated to 25-95° C., preferably 45-75° C., and kept warm for 0.5-10 hours, preferably 2-4 hours, and the acid adjustment solvent is any one or more of lactic acid, citric acid, tartaric acid, acetic acid, and sodium citrate.

9. The method according to claim 6, characterized in that In step S3, based on dry matter, the weight ratio of glycerolphosphorylcholine to wall material is 1:1-20, preferably 1:1-10, the homogenization temperature is 25-90°C, preferably 45-75°C, the homogenization pressure is 5-30 MPa, preferably 15-25 MPa, and the homogenization time is 1-30 minutes, preferably 5-15 minutes.

10. The method according to claim 9, characterized in that In step S3, a liquid microcapsule suspension is obtained after homogenization.

11. The method according to claim 6, characterized in that In step S1, the concentration of the glycerol phosphorylcholine solution is 50%-90%, preferably 75-85%.

12. The method according to claim 6, characterized in that In step S4, the injection port temperature of the spray drying is 150-200°C, preferably 175-195°C, and the outlet temperature is 60-120°C, preferably 80-100°C.

13. Use of the glycerol phosphorylcholine-collagen peptide microcapsules according to any one of claims 1 to 5 and the glycerol phosphorylcholine-collagen peptide microcapsules produced by the preparation method according to any one of claims 6 to 12 in fruit juice drinks, oral liquids, solid drinks and compressed tablets.

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