Composite nutritional oral liquid containing chestnut shell polyphenol and preparation method thereof

Through ultrasonic assisted leaching method and fermentation enzymatic method, combined with membrane separation and roll nanofiltration membrane filtration, efficient utilization of resources such as chestnut shells and green extraction of polyphenols are achieved, resource waste and pollution problems are solved, and polyphenol products with significant pharmacological activity are obtained.

CN119523093APending Publication Date: 2025-02-28李明军
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Patent Information

Application Number
CN202411475963.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-22
Publication Date
2025-02-28

AI Technical Summary

Technical Problem

The existing technology is difficult to effectively utilize resources such as chestnut shells, resulting in waste of resources. At the same time, the process of extracting polyphenols is complex and has a high pollution.

Method used

Ultrasonic assisted leaching method combined with fermentation and enzymatic decomposition, through membrane separation and roll nanofiltration membrane filtration, water extraction without organic solvents is achieved, green and environmentally friendly, and the original pure natural structure and properties of polyphenols are retained.

Benefits of technology

The efficient utilization of resources such as chestnut shells has been achieved. The extracted polyphenol products have significant antioxidant, anti-cancer, and improved microcirculation. The process is environmentally friendly and pollution-free.

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Abstract

The compound nutritional oral liquid containing chestnut shell polyphenol is prepared by compounding the following components in parts by weight: 1-2 parts of chestnut shell polyphenol extracting solution, 2-4 parts of hawthorn polyphenol extracting solution, 2-4 parts of grape polyphenol extracting solution and 8-10% of lycium barbarum polysaccharide. The plant polyphenol has remarkable effects in the aspects of scavenging free radicals, delaying senescence, inhibiting tumor and microorganism growth, regulating an immune system, preventing chronic diseases such as hyperglycemia and hyperlipidemia and the like, and is a natural product with unique physiological activity, pharmacological activity and good biological safety, and raw materials for production are wastes in production, so that the production cost is low, and the production cost is low. After treatment, the produced polyphenol oral liquid is free of any preservatives and is natural and pollution-free, all the materials can be completely utilized, the economic value is improved, and green cyclic utilization is achieved.
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Description

Technical Field

[0001] Studies have shown that plant polyphenols have significant effects in scavenging free radicals, delaying aging, inhibiting tumor and microbial growth, regulating the immune system, preventing chronic diseases such as hyperglycemia and hyperlipidemia, etc. They are natural products with unique physiological activity, pharmacological activity and good biosafety. The compound nutritional oral liquid is made of chestnut shell polyphenol extract, hawthorn polyphenol extract, grape polyphenol extract and wolfberry polysaccharide. It has balanced nutrition and effectively utilizes the polyphenol components of chestnut shell, hawthorn and grape. It plays a role in delaying the formation of atherosclerosis, reducing thrombosis and blood flow blockage caused by arterial narrowing. It has significant effects in scavenging free radicals in the human body, antioxidant activity, anti-mutagenic activity, reducing capillary permeability, enzyme inhibition activity, improving human microcirculation, anti-carcinogenic effect, preventing chronic diseases such as hyperglycemia and hyperlipidemia, etc. Background Art

[0002] Chestnut shell is the outer shell of chestnut. It is discarded as waste in production and has not been effectively utilized. Few products have been developed, resulting in a waste of resources. Chestnut shell is also called chestnut hair shell, chestnut thorn shell, wind chestnut shell, chestnut shell cup, chestnut shell, hair ball outer thorn package, chestnut ball, chestnut outer thorn package, hair ball, chestnut stalk, etc. Chestnut shell is spherical, with yellow-brown or brown outer surface, densely covered with antler-like sharp thorns branching from the base, densely covered with gray-white to gray-green soft hairs on the outer surface and thorns, and many have thick fruit stalks. According to the "Chinese Medicine Dictionary", chestnut shell has the effects of reducing adverse effects and resolving phlegm, clearing heat and dispersing knots, and stopping bleeding. Relevant literature shows that chestnut shell is sweet, astringent, and flat in nature, and can treat erysipelas, whooping cough, etc.; research on the chemical composition of chestnut shell shells shows that the main active ingredients are polyphenols and flavonoids. Its main active ingredients include cellulose, lignin, polysaccharides (or glycosides), organic acids, phenols, lactones, coumarins (or glycosides), flavonoids (or saponins), phytosterols (or triterpenes) and tannins. In addition, (Jiao Qiyang, Wu Lijun, Huang Jian, et al. Isolation and identification of chemical components of chestnut involucre [J]. Journal of Shenyang Pharmaceutical University, 2009, 1: 26-29) and (Jia Lu, Xi Fang, Wang Na, et al. Study on chemical components of chestnut shell [J]. Chinese Journal of Pharmaceutical Industry, 2010, 41(2): 98-102) 18 compounds were obtained by separating the alcohol extract of chestnut involucre and identifying it, and oleanolic acid was isolated for the first time. , 2-hydroxy-succinic acid dibutyl ester, stigmaster-4-ene-6β-3-one, and found that the alcohol extract had an antibacterial effect on Escherichia coli, Micrococcus luteus, and Staphylococcus aureus, especially the strongest antibacterial activity against Micrococcus luteus. It was separated and structurally identified, and it was confirmed that the main antibacterial component in the alcohol extract was gallic acid; (Lin Siwen, Yin Changchang, Yin Ming, et al. Inhibitory effect of total flavonoids from chestnut involucre on three different tumor cells [J]. Natural Product Research 2015, 27(01): 143-147). Total flavonoids from chestnut involucre have obvious anti-tumor effects in vitro, can inhibit tumor cell proliferation and induce cell apoptosis.

[0003] Grape polyphenols are mainly found in grape skins and grape seeds. Studies have shown that grape polyphenols account for about 1% of the total fruit, mainly in grape skins and grape seeds, of which the content of polyphenols in grape skins and grape seeds can reach 25% to 50% and 50% to 70% respectively. The antioxidant mechanism of grape polyphenols is that grape polyphenols themselves are excellent hydrogen donors, and the free radicals formed can be transformed into stable free radicals through resonance hybridization, thereby inactivating free radicals and cutting off chain reactions to play an antioxidant role, prevent various diseases, resist fatigue, delay aging, and have health care effects such as skin care and beauty. Studies have found that grape polyphenols can reduce hypertension caused by angiotensin II by reducing the subunits of NADPH oxidase. Foreign studies have also found that grape polyphenols have an anti-tumor effect in addition to improving Alzheimer's disease, Parkinson's disease, etc. Studies have confirmed that grape polyphenols have a significant inhibitory effect on 8 pathogenic bacteria, including Staphylococcus aureus, Proteus vulgaris, Salmonella typhi, Shigella dysenteriae, Bacillus subtilis, and Escherichia coli.

[0004] The polyphenols and flavonoids contained in hawthorn are mainly in hawthorn peel and hawthorn seeds. The polyphenols and flavonoids of hawthorn have a wide range of pharmacological effects, especially beneficial to the cardiovascular system. Experimental studies have shown that hawthorn polyphenols and flavonoids can lower blood pressure, reduce peripheral vascular resistance, dilate coronary arteries, increase coronary flow, reduce myocardial oxygen consumption, enhance heart function, increase cardiac output, resist myocardial ischemia, resist platelet aggregation, improve blood rheology, eliminate oxygen free radicals, lower blood lipids, enhance hypoxia tolerance and diuresis. In clinical practice, hawthorn polyphenols and flavonoids are used to prevent and treat coronary heart disease, angina pectoris, hypertension, arrhythmia, hyperlipidemia and atherosclerosis. Their application is safe and effective and worthy of promotion and application.

[0005] Lycium barbarum polysaccharide (LBP) is one of the effective ingredients of wolfberry and is one of the few protein-containing polysaccharides in plant polysaccharides. Lycium barbarum polysaccharide isolated from wolfberry has a polysaccharide side chain composed of six hexoses (rhamnose, arabinose, xylose, mannose, galactose, glucose) and a protein main chain composed of 18 amino acids, connected in the form of Glycml--O--Der. This glycoprotein has biological activity and is a high-intensity immunopotentiator. Lycium barbarum polysaccharide is generally used as a raw material for health food. It can improve human immunity, enhance hematopoietic function, protect the liver and lower blood pressure, and enhance cell activity. It is widely used in the fields of medicine and health food. Lycium barbarum polysaccharide has attracted much attention due to its different biological activities. Gal-3 (galactose lectin 3) is a lectin that specifically binds to β-galactose. It is related to many diseases such as immune response, cardiovascular disease, cancer, fibrosis, etc., and has become a molecular target for cancer treatment. Summary of the invention

[0006] At present, the main polyphenol extraction processes in production and research are: organic solvent extraction, adsorption separation, supercritical CO2 extraction, ultrasound-assisted leaching, microwave leaching, etc.; separation and purification methods include: column chromatography separation and purification, metal ion precipitation, macroporous resin adsorption, membrane separation, etc. This process adopts innovative ultrasound-assisted leaching plus fermentation and enzymatic hydrolysis, membrane separation and other processes, without using organic solvents, using water for extraction, which is green and environmentally friendly, pollution-free, and no preservatives are added to the product, which retains the original pure natural structure, performance and efficacy of the extracted product to the greatest extent.

[0007] Process flow: Material drying and crushing → microwave radiation extraction → fermentation → filtration of waste residue → alcoholization → filtration → mixing → coarse filtration → spiral nanofiltration membrane filtration → preparation → filling → sterilization → capping → inspection → finished product DETAILED DESCRIPTION

[0008] Remove impurities from the dried chestnut husks using a magnetic separator, and then crush them into 30-80 meshes for later use.

[0009] After the hawthorn juice is extracted, the hawthorn peel and hawthorn seeds are naturally dried to a moisture content of less than 5%, and then crushed to 30-50 meshes for later use.

[0010] After the juice is extracted from the grapes, the grape skins and grape seeds are naturally dried to a moisture content of less than 5%, and then crushed to 20-50 meshes for later use.

[0011] 1 part of crushed chestnut bud powder, 2 parts of hawthorn powder, 2 parts of grape powder, a solid-liquid ratio of 1:7 and deionized water with a pH value of 8-10 are added into a fermentation tank. The temperature in the tank is set to 100°C and stirred for 20-30 minutes.

[0012] The temperature in the fermentation tank was lowered to 40°C, the microwave power was 640 W, and the treatment was carried out for 30 min.

[0013] After cooling to 5°C, add white sugar to the mixed liquid prepared in the fermentation tank until the solution sugar content is 9%, inoculate 0.02% by weight of brewer's yeast, seal at room temperature 25-35°C, ferment for 5 days, and stir for 30 minutes every day.

[0014] The fermentation broth was then inoculated with composite lactic acid bacteria at 1000 CFU / mL by volume for secondary fermentation. The composite lactic acid bacteria ratio was (Lactobacillus plantarum, Lactobacillus paracasei, and Acetobacter aceticus were mixed in a ratio of 1:1:0.5). The broth was sealed and fermented at room temperature of 28-38°C for 10 days, with stirring at 10 rpm for 1 hour every day during the fermentation period.

[0015] The fermentation liquid was filtered with a 500-mesh filter cloth, and the filtrate was centrifuged at 8000 r / min for 10 minutes at 4°C using a Sigma (3K15) centrifuge. The pH of the obtained supernatant was adjusted to 6-7 to obtain a mixed fermentation liquid for use.

[0016] The mixed material residue after centrifugation is put back into the enzymolysis tank, and new deionized water is injected at a solid-liquid ratio of 1:5, and stirred for 20 to 30 minutes. Then, the composite enzyme is added and stirred evenly. The weight ratio of the composite enzyme is (pectinase addition amount 1.0%, cellulase addition amount 3.0%, neutral protease addition amount 3.0%, laccase addition amount 5.0%), pH 5.0, enzymolysis time 20min, temperature 30°C, and centrifugation at 30000rpm tubular high-speed centrifuge to obtain the mixed solution after enzymolysis for use.

[0017] The mixed fermentation liquid and the mixed liquid after enzymatic hydrolysis are put together, heated to 120℃ to remove the enzyme, and then micro-filtered and clarified with a ceramic membrane with an average pore size of 1um to remove suspended matter such as starch, protein, pectin, oil and various particulate impurities.

[0018] The permeate clarified by microfiltration was subjected to initial ultrafiltration separation using a ceramic membrane with an average pore size of 200 nm.

[0019] The retentate was concentrated and separated using a rolled nanofiltration membrane with a relative molecular weight range of 500, and the solutions were concentrated by reduced pressure evaporation to increase the solid content to more than 15%.

[0020] The extract is mixed with wolfberry polysaccharide powder in a weight ratio of 6% to 10%, stirred evenly to improve the taste, sterilized in a 95° C. high-temperature instant sterilizer for 15 seconds, and cooled to obtain the finished product.

[0021] The filtered waste residue can be dried and compressed into biomass fuel, or processed into humus soil for flower mud.

[0022] The compound nutritional oral liquid of chestnut shell polyphenols uses a variety of product waste for deep processing, maximizes the polyphenol components contained in the raw materials, uses fermentation and composite enzymatic hydrolysis to hydrolyze and separate the largest amount of polyphenols and other substances, and uses ceramic membranes and rolled nanofiltration membranes for filtration and separation, retaining the original pure natural structure, properties and efficacy of the extracted products to the greatest extent. The final waste can be dried and processed into biomass fuel, or processed into humus soil for flower mud. The whole process does not require organic solvents, is green and environmentally friendly, pollution-free, and does not generate waste.

[0023] It is characterized in that the raw material of claim 0020 can be concentrated by reduced pressure evaporation to reach a powder with a solid content of 50%, and can be made into granules, tablets, hard capsules, soft capsules, and powders by adding auxiliary materials and corresponding processes. Any modifications, equivalent substitutions or improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A composite nutritional oral liquid containing chestnut shell polyphenols, comprising: 1-2 parts of chestnut shell polyphenol extract, 2-4 parts of hawthorn polyphenol extract, 2-4 parts of grape polyphenol extract, and 8% to 10% wolfberry polysaccharide by weight; A composite nutritional oral liquid containing chestnut shell polyphenols and a preparation method thereof, which is characterized by comprising the following steps.

2. Remove impurities from the dried chestnut husks and crush them into 30-80 mesh size for later use.

3. After extracting the juice from hawthorn, dry and crush the hawthorn peel and seeds for 20-50 minutes and set aside.

4. After the grape juice is extracted, the grape skins and grape seeds should be dried and crushed for 20-50 minutes and set aside.

5. Add 1 part of chestnut bud powder, 2 parts of hawthorn powder, and 2 parts of grape powder in a solid-liquid ratio of 1:7 and deionized water with a pH value of 8-10 into the fermentation tank, and stir and extract for 20-30 minutes.

6. Add white sugar to the mixed liquid prepared in the fermentation tank to make the solution sugar content reach 9%, inoculate 0.02% by weight of brewer's yeast, seal at room temperature 20-35°C, and ferment for 5 days, stirring for 30 minutes every day.

7. In the fermented liquid, the composite lactic acid bacteria was inoculated with 1000CFU / mL by volume for secondary fermentation. The composite lactic acid bacteria was mixed with plant lactobacillus, Lactobacillus paracasei and acetobacter in a quantity ratio of 1:1:0.

5. The mixture was sealed and fermented at room temperature of 25-38°C for 10 days. During the fermentation, the mixture was stirred at 10 rpm for 1 h. It was 5.0% and pH 4.5 to measure the alcohol content of the fermented liquid. The fermented liquid was filtered through 60 mesh and 100 mesh successively, and a tubular high-speed centrifuge of 8000 rpm was used to centrifuge the mixture to obtain a mixed fermented liquid for standby use.

8. After centrifugation, the mixture residue is put back into the enzymolysis tank, and new deionized water is injected at a solid-liquid ratio of 1:8, stirred for 20 to 30 minutes, and then the composite enzyme is added and stirred evenly. The weight ratio of the composite enzyme is 1.0% pectinase, 3.0% cellulase, 3.0% neutral protease, and 5.0% laccase (neutral protease can efficiently hydrolyze protein, laccase can catalyze the degradation of lignin components, cellulase can catalyze the hydrolysis of cellulose, and pectinase has the effect of esterification, hydrolysis, and rupture of pectin), pH 5.0, enzymolysis time 20min, temperature 30°C. Centrifuge at 30000rpm in a tubular high-speed centrifuge to obtain a mixed solution for use.

9. After the two mixed solutions are heated to 120℃ to remove the enzyme, they are separated by microfiltration using a ceramic membrane with an average pore size of 1um to remove suspended matter such as starch, protein, pectin, oil and various particulate impurities.

10. The permeate clarified by microfiltration was initially separated by ultrafiltration using a ceramic membrane with an average pore size of 200 nm, and the retentate was concentrated and separated using a rolled nanofiltration membrane with a relative molecular weight range of 500. The solutions were concentrated by reduced pressure evaporation to increase the solid content to more than 15%.

11. Add 6% to 10% of the extract by weight into the wolfberry polysaccharide powder and stir evenly to improve the taste. Sterilize it in a 95°C high-temperature instant sterilizer for 15 seconds and cool it to below 40°C to obtain the finished product.

12. The filtered waste residue can be dried and compressed into biomass fuel, or processed into humus soil for flower mud.

13. The compound nutritional oral liquid of chestnut shell polyphenols uses a variety of product waste for deep processing to maximize the polyphenol components contained in the raw materials, and uses fermentation and composite enzymatic hydrolysis to hydrolyze and separate the largest amount of polyphenols and other substances. Ceramic membranes and rolled nanofiltration membranes are used for filtration and separation, which retains the original pure natural structure, performance and efficacy of the extracted products to the greatest extent. The final waste can be dried and processed into biomass fuel, or processed into humus soil for flower mud.

14. It is characterized in that The raw material of claim 9 can be concentrated by reduced pressure evaporation to achieve a powder with a solid content of 50%, and can be made into granules, tablets, hard capsules, soft capsules, and powders by adding auxiliary materials and corresponding processes. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.