Ginkgo leaf chitosan oligosaccharide tablet capable of resisting oxidation and reducing blood fat and preparation method thereof

Abstract

The invention belongs to the technical field of functional foods and medicines, and discloses an antioxidant and blood fat-reducing ginkgo leaf chitosan oligosaccharide tablet, which is prepared from the following components in percentage by mass: 45 to 55 percent of chitosan oligosaccharide, 15 to 20 percent of ginkgo leaf extract, 10 to 15 percent of grape seed extract, 5 to 10 percent of chitosan and the balance of corn starch. According to the invention, through scientific proportioning and multi-target synergistic effect, and through accurate design of the mass percentage of the active ingredients such as chitosan oligosaccharide, ginkgo leaf extract and grape seed extract, a scientific multi-target synergistic effect mechanism is realized, and the anti-oxidation and blood fat-reducing effects of the product are significantly improved; the problems that the proportion design of active ingredients of related products in the market is unreasonable, and the effect exertion is limited are solved.

Description

Technical Field

[0001] This invention belongs to the field of functional food and pharmaceutical technology, specifically a ginkgo biloba oligosaccharide tablet with antioxidant and lipid-lowering properties and its preparation method. Background Technology

[0002] Chitosan oligosaccharide (COS), as a functional ingredient, has attracted widespread scientific research attention in recent years due to its multiple bioactive functions, including regulating lipid metabolism, antioxidation, and immune regulation. Meanwhile, flavonoids and proanthocyanidins in ginkgo biloba extract (GBE) and grape seed extract (GSE) have also been shown to have significant synergistic effects, further expanding their application potential in health products. However, some significant shortcomings exist in current market products. Specifically, many products have unreasonable active ingredient ratios and lack a scientific multi-target synergistic mechanism, which limits their full efficacy. Furthermore, chitosan oligosaccharide is easily degraded in acidic environments such as gastric acid, resulting in low bioavailability and failing to meet practical application needs. On the other hand, sensitive components such as proanthocyanidins are prone to oxidative browning reactions, which not only affect the sensory quality of the product but also significantly reduce its stability and shelf life, posing considerable challenges to both producers and consumers. Therefore, improvements are needed. Summary of the Invention

[0003] The purpose of this invention is to provide an antioxidant and lipid-lowering Ginkgo biloba oligosaccharide tablet and its preparation method, so as to solve the problems mentioned in the background art.

[0004] To achieve the above objectives, the present invention provides the following technical solution: an antioxidant and lipid-lowering ginkgo biloba oligosaccharide tablet, composed of the following components by weight percentage: The composition consists of 45%-55% chitosan oligosaccharide, 15%-20% ginkgo leaf extract, 10%-15% grape seed extract, 5%-10% chitosan, and the remainder is corn starch.

[0005] Preferably, the molecular weight of the chitosan oligosaccharide is ≤2000 Da and the degree of deacetylation is ≥90%; the ginkgo leaf extract is treated with vegetable oil to remove acidity, and the total flavonoid content is ≥24% and the terpene lactone content is ≥6%; the proanthocyanidin purity of the grape seed extract is ≥95%.

[0006] Preferably, it includes the following steps: Step 1: Raw material pretreatment and sieving. Chitosan oligosaccharide, chitosan, and corn starch are sieved through an 80-mesh vibrating screen to remove lumps and large particles, ensuring uniform particle size. Ginkgo leaf extract and grape seed extract are subjected to air jet milling to control the fineness of the raw materials to ≤50μm, avoiding difficulties in subsequent granulation. Step 2, Inner layer granulation: Mix chitosan oligosaccharide and chitosan, granulate with hydroxypropyl methylcellulose ethanol solution, and dry to obtain inner layer particles with a particle size of 150μm-200μm; Step 3, outer layer granulation: Ginkgo biloba extract, grape seed extract and anti-browning agent are mixed and granulated with polyvinylpyrrolidone aqueous solution. After drying, outer layer particles are obtained with a particle size of 80μm-120μm. Step 4, Overall Mixing and Tableting: Mix the inner layer particles and the outer layer particles in a ratio of 6:4 to 8:2. Put the two types of particles into a V-type mixer and mix at 15 rpm for 20 minutes. Use a rotary tablet press and set the tablet weight difference to ±3% and the hardness to be controlled at 60-80N. During the tableting process, the tablet thickness and disintegration time need to be continuously monitored. Step 5, coating and packaging: Use a stomach-soluble film coating premix, and control the coating weight gain to 2%-3%; Coating parameters: air inlet temperature 50℃, tablet bed temperature 38-42℃, spray rate 8-10g / min; Use an aluminum-plastic blister packaging machine with a heat sealing temperature of 160℃ to ensure airtightness.

[0007] Preferably, during the granulation of the inner layer particles, the concentration of the hydroxypropyl methylcellulose ethanol solution is 3-5%, and the spray rate is 8-12 mL / min; during the granulation of the outer layer particles, the concentration of the polyvinylpyrrolidone aqueous solution is 2-3%, and the spray rate is 5-8 mL / min.

[0008] Preferably, the coating is enteric coating, the coating material is Eudragit L100-55, the coating weight gain is 2.5-3.5%, the coating solution concentration is 10-15% w / v, the spray rate is 2-3 g / min, and the inlet air temperature is 40-50℃.

[0009] Preferably, the chitosan oligosaccharide is prepared by a hydrogen peroxide-enzymatic hydrolysis combined method, specifically comprising: dissolving chitosan in 2.5% H2O2 solution, treating at 60℃ for 2 h, adding 1.5 U / g - 2.0 U / g chitosanase, enzymatically hydrolyzing for 4 h, and ultrafiltration fractionation to obtain chitosan oligosaccharide with a molecular weight ≤2000 Da.

[0010] Preferably, the Ginkgo biloba oligosaccharide tablets further include an active ingredient protective layer, wherein the protective layer is nanoparticles formed by cross-linking chitosan and sodium tripolyphosphate, with an encapsulation rate ≥85%, a particle size ≤100 nm, and an encapsulation amount accounting for 10%-15% of the total mass of chitosan oligosaccharides.

[0011] Preferably, the preparation method of the ginkgo leaf extract includes the following steps: first, pre-treating the ginkgo leaves, then refluxing and extracting them three times with 70% ethanol at about 80°C, with the ethanol added being 6 times, 4 times, and 4 times the amount added respectively, and the extraction time being 3 hours, 2 hours, and 2 hours respectively. Next, filtering and concentrating are performed, and then the concentrate is loaded onto a polyamide column and eluted with 70% ethanol, followed by vacuum concentration. Then, it is spray-dried with an inlet temperature of 180±5°C and an outlet temperature of 70±5°C. Finally, the dried product is passed through a 100-mesh sieve and packaged.

[0012] Preferably, the preparation method of the grape seed extract includes the following steps: first, the raw material is crushed and sieved, defatted three times with petroleum ether at 60-90°C, then the residue is added to 7 times the amount of 80% ethanol and refluxed at 80°C for 1.5 hours each time, followed by filtration and concentration, and then extracted four times with an equal amount of ethyl acetate. Subsequently, the ethyl acetate is recovered under reduced pressure, and then the extract is loaded onto a polyamide column. First, purified water is used for elution and the water eluent is discarded, then 80% ethanol is used for elution, followed by ethanol recovery under reduced pressure, concentration, drying, and finally crushing and sieving.

[0013] Preferably, the daily intake is 1-2 tablets, each containing ≥250 mg of chitosan oligosaccharide, ≥75 mg of ginkgo leaf extract, and ≥50 mg of grape seed extract.

[0014] The beneficial effects of this invention are as follows: 1. This invention, through scientific formulation and multi-target synergistic effects, and by precisely designing the mass percentages of active ingredients such as chitosan oligosaccharide, ginkgo biloba extract, and grape seed extract, achieves a scientific multi-target synergistic mechanism, significantly enhancing the product's antioxidant and lipid-lowering efficacy. This solves the problem of unreasonable active ingredient ratios and limited efficacy in related products on the market.

[0015] 2. This invention effectively protects chitosan oligosaccharides from degradation in acidic environments such as gastric acid by employing chitosan oligosaccharides with specific molecular weight control (≤2000 Da) and high degree of deacetylation (≥90%), as well as enteric coating technology, thereby improving their bioavailability. This solves the problem of chitosan oligosaccharides being easily degraded and having low bioavailability in acidic environments.

[0016] 3. This invention, through optimized preparation processes, such as treating Ginkgo biloba leaf extract and grape seed extract with anti-browning agents, and using chitosan-formed nanoparticles as a protective layer for active ingredients, effectively prevents oxidative browning reactions of sensitive components, thereby improving product stability and shelf life. This solves the problem of sensitive components easily undergoing oxidative browning, affecting the sensory quality and stability of the product.

[0017] 4. This invention, by employing gradient granulation and mixed compression technology, ensures uniform distribution of product components and good tablet quality. Simultaneously, by precisely controlling various parameters during the granulation and coating processes, such as spray rate and coating solution concentration, it further improves product preparation efficiency and quality control. Attached Figure Description

[0018] Figure 1 This is a flowchart illustrating the preparation process of the Ginkgo biloba oligosaccharide tablets of the present invention. Detailed Implementation

[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] like Figure 1 As shown, this embodiment of the invention provides an antioxidant and lipid-lowering Ginkgo biloba oligosaccharide tablet, composed of the following components by weight percentage: The composition consists of 45%-55% chitosan oligosaccharide, 15%-20% ginkgo leaf extract, 10%-15% grape seed extract, 5%-10% chitosan, and the remainder is corn starch.

[0021] The chitosan oligosaccharide has a molecular weight ≤2000 Da and a degree of deacetylation ≥90%; the ginkgo leaf extract is treated with vegetable oil to remove acidity, and has a total flavonoid content ≥24% and a terpene lactone content ≥6%; the grape seed extract has a proanthocyanidin purity ≥95%.

[0022] This includes the following steps: Step 1: Raw material pretreatment and sieving. Chitosan oligosaccharide, chitosan, and corn starch are sieved through an 80-mesh vibrating screen to remove lumps and large particles, ensuring uniform particle size. Ginkgo leaf extract and grape seed extract are subjected to air jet milling to control the fineness of the raw materials to ≤50μm, avoiding difficulties in subsequent granulation. Step 2, Inner layer granulation: Mix chitosan oligosaccharide and chitosan, granulate with hydroxypropyl methylcellulose ethanol solution, and dry to obtain inner layer particles with a particle size of 150μm-200μm; Step 3, outer layer granulation: Ginkgo biloba extract, grape seed extract and anti-browning agent are mixed and granulated with polyvinylpyrrolidone aqueous solution. After drying, outer layer particles are obtained with a particle size of 80μm-120μm. Step 4, Overall Mixing and Tableting: Mix the inner layer particles and the outer layer particles in a ratio of 6:4 to 8:2. Put the two types of particles into a V-type mixer and mix at 15 rpm for 20 minutes. Use a rotary tablet press and set the tablet weight difference to ±3% and the hardness to be controlled at 60-80N. During the tableting process, the tablet thickness and disintegration time need to be continuously monitored. Step 5, coating and packaging: Use a stomach-soluble film coating premix, and control the coating weight gain to 2%-3%; Coating parameters: air inlet temperature 50℃, tablet bed temperature 38-42℃, spray rate 8-10g / min; Use an aluminum-plastic blister packaging machine with a heat sealing temperature of 160℃ to ensure airtightness.

[0023] When granulating the inner layer particles, the concentration of the hydroxypropyl methylcellulose ethanol solution is 3-5%, and the spraying rate is 8-12 mL / min; when granulating the outer layer particles, the concentration of the polyvinylpyrrolidone aqueous solution is 2-3%, and the spraying rate is 5-8 mL / min.

[0024] The coating is an enteric coating, the coating material is Eudragit L100-55, the coating weight gain is 2.5-3.5%, the coating solution concentration is 10-15% w / v, the spray rate is 2-3 g / min, and the inlet air temperature is 40-50℃.

[0025] The chitosan oligosaccharide is prepared by a hydrogen peroxide-enzymatic hydrolysis combined method, specifically including: dissolving chitosan in 2.5% H2O2 solution, treating at 60℃ for 2 h, adding 1.5 U / g - 2.0 U / g chitosanase, hydrolyzing for 4 h, and ultrafiltration fractionation to obtain chitosan oligosaccharide with a molecular weight ≤2000 Da.

[0026] The Ginkgo biloba oligosaccharide tablets also include an active ingredient protective layer, which is a nanoparticle formed by cross-linking chitosan and sodium tripolyphosphate, with an encapsulation rate of ≥85%, a particle size of ≤100 nm, and an encapsulation amount accounting for 10%-15% of the total mass of chitosan oligosaccharides.

[0027] The preparation method of the ginkgo leaf extract includes the following steps: first, pre-treating the ginkgo leaves, then refluxing and extracting them three times with 70% ethanol at about 80°C, with the ethanol added being 6 times, 4 times, and 4 times the amount added respectively, and the extraction time being 3 hours, 2 hours, and 2 hours respectively. Next, filtering and concentrating are performed, and then the concentrate is loaded onto a polyamide column and eluted with 70% ethanol, followed by vacuum concentration. Then, it is spray-dried with an inlet temperature of 180±5°C and an outlet temperature of 70±5°C. Finally, the dried product is passed through a 100-mesh sieve and packaged.

[0028] The preparation method of the grape seed extract includes the following steps: first, the raw material is crushed and sieved, defatted three times with petroleum ether at 60-90°C, then the residue is added to 7 times the amount of 80% ethanol and refluxed at 80°C for 1.5 hours each time, followed by filtration and concentration, and then extracted four times with an equal amount of ethyl acetate. Subsequently, the ethyl acetate is recovered under reduced pressure, and then the extract is loaded onto a polyamide column. First, purified water is used for elution and the water eluent is discarded, then 80% ethanol is used for elution, followed by recovery of ethanol under reduced pressure, concentration, drying, and finally crushing and sieving.

[0029] The recommended daily intake is 1-2 tablets, each containing ≥250 mg of chitosan oligosaccharide, ≥75 mg of ginkgo biloba extract, and ≥50 mg of grape seed extract.

[0030] The types, names, and standards of packaging materials that come into direct contact with the product should comply with the provisions of YBB00122002 for high-density polyethylene bottles used for oral solid medicines.

[0031] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0032] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A ginkgo biloba oligosaccharide tablet with antioxidant and lipid-lowering properties, characterized in that: It consists of the following components by weight percentage: The composition consists of 45%-55% chitosan oligosaccharide, 15%-20% ginkgo leaf extract, 10%-15% grape seed extract, 5%-10% chitosan, and the remainder is corn starch.

2. The Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claim 1, characterized in that: The chitosan oligosaccharide has a molecular weight ≤2000 Da and a degree of deacetylation ≥90%; the ginkgo leaf extract is treated with vegetable oil to remove acidity, and has a total flavonoid content ≥24% and a terpene lactone content ≥6%; the grape seed extract has a proanthocyanidin purity ≥95%.

3. The method for preparing an antioxidant and lipid-lowering Ginkgo biloba oligosaccharide tablet according to claim 1, characterized in that: Includes the following steps: Step 1: Raw material pretreatment and sieving. Chitosan oligosaccharide, chitosan, and corn starch are sieved through an 80-mesh vibrating screen to remove lumps and large particles, ensuring uniform particle size. Ginkgo leaf extract and grape seed extract are subjected to air jet milling to control the fineness of the raw materials to ≤50μm, avoiding difficulties in subsequent granulation. Step 2, Inner layer granulation: Mix chitosan oligosaccharide and chitosan, granulate with hydroxypropyl methylcellulose ethanol solution, and dry to obtain inner layer particles with a particle size of 150μm-200μm; Step 3, outer layer granulation: Ginkgo biloba extract, grape seed extract and anti-browning agent are mixed and granulated with polyvinylpyrrolidone aqueous solution. After drying, outer layer particles are obtained with a particle size of 80μm-120μm. Step 4, Overall Mixing and Tableting: Mix the inner layer particles and the outer layer particles in a ratio of 6:4 to 8:

2. Put the two types of particles into a V-type mixer and mix at 15 rpm for 20 minutes. Use a rotary tablet press and set the tablet weight difference to ±3% and the hardness to be controlled at 60-80N. During the tableting process, the tablet thickness and disintegration time need to be continuously monitored. Step 5, coating and packaging: Use a stomach-soluble film coating premix, and control the coating weight gain to 2%-3%; Coating parameters: air inlet temperature 50℃, tablet bed temperature 38-42℃, spray rate 8-10g / min; Use an aluminum-plastic blister packaging machine with a heat sealing temperature of 160℃ to ensure airtightness.

4. The method for preparing an antioxidant and lipid-lowering Ginkgo biloba oligosaccharide tablet according to claim 3, characterized in that: When granulating the inner layer particles, the concentration of the hydroxypropyl methylcellulose ethanol solution is 3-5%, and the spray rate is 8-12 mL / min; when granulating the outer layer particles, the concentration of the polyvinylpyrrolidone aqueous solution is 2-3%, and the spray rate is 5-8 mL / min.

5. The method for preparing an antioxidant and lipid-lowering Ginkgo biloba oligosaccharide tablet according to claim 3, characterized in that: The coating is enteric coating, the coating material is Eudragit L100-55, the coating weight gain is 2.5-3.5%, the coating solution concentration is 10-15% w / v, the spray rate is 2-3 g / min, and the inlet air temperature is 40-50℃.

6. The Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claim 1, characterized in that: The chitosan oligosaccharide was prepared by a hydrogen peroxide-enzymatic hydrolysis combined method, specifically including: dissolving chitosan in 2.5% H2O2 solution, treating at 60℃ for 2 h, adding 1.5 U / g-2.0 U / g chitosanase, hydrolyzing for 4 h, and ultrafiltration fractionation to obtain chitosan oligosaccharide with a molecular weight ≤2000 Da.

7. The Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claim 1, characterized in that: The Ginkgo biloba oligosaccharide tablets also include an active ingredient protective layer, which is chitosan nanoparticles with an encapsulation rate of ≥85%, a particle size of ≤100nm, and an encapsulation amount accounting for 10%-15% of the total mass of chitosan oligosaccharides.

8. The Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claim 1, characterized in that: The preparation method of the Ginkgo biloba extract includes the following steps: first, pre-treating the Ginkgo biloba leaves, then refluxing and extracting them three times with 70% ethanol at about 80°C, with the ethanol added being 6 times, 4 times, and 4 times the amount of ethanol, and the extraction times being 3 hours, 2 hours, and 2 hours, respectively. Next, filtering and concentrating are performed, and then the concentrate is loaded onto a polyamide column and eluted with 70% ethanol, followed by vacuum concentration. Then, it is spray-dried with an inlet temperature of 180±5°C and an outlet temperature of 70±5°C. Finally, the dried product is passed through a 100-mesh sieve and packaged.

9. The Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claim 1, characterized in that: The preparation method of the grape seed extract includes the following steps: first, the raw material is crushed and sieved, defatted three times with petroleum ether at 60-90℃, then the residue is added to 7 times the amount of 80% ethanol and refluxed at 80℃ for 1.5 hours each time, followed by filtration and concentration, and then extracted four times with an equal amount of ethyl acetate. Subsequently, the ethyl acetate is recovered under reduced pressure, and then the extract is loaded onto a polyamide column. First, purified water is used for elution and the water eluent is discarded, then 80% ethanol is used for elution, followed by ethanol recovery under reduced pressure, concentration, drying, and finally crushing and sieving.

10. The application of the Ginkgo biloba oligosaccharide tablets with antioxidant and lipid-lowering properties according to claims 1-9, characterized in that: The daily intake is 1-2 tablets, each containing ≥250mg of chitosan oligosaccharide, ≥75mg of ginkgo leaf extract, and ≥50mg of grape seed extract.

Images