CN111848567A - Method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn - Google Patents

Method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn Download PDF

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Publication number
CN111848567A
CN111848567A CN202010681730.8A CN202010681730A CN111848567A CN 111848567 A CN111848567 A CN 111848567A CN 202010681730 A CN202010681730 A CN 202010681730A CN 111848567 A CN111848567 A CN 111848567A
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polyphenol
purple corn
procyanidine
filtering
nanofiltration
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Inventor
张永利
安宣宇
董浩
张宝通
姜丽
寇玉锋
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Sanyuan Lihua Biotechnology Co ltd
Shaanxi Yuanbang Bio Tech Co ltd
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Sanyuan Lihua Biotechnology Co ltd
Shaanxi Yuanbang Bio Tech Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
    • C07D311/62Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/899Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • A61P39/06Free radical scavengers or antioxidants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/08Vasodilators for multiple indications
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/10Drugs for disorders of the cardiovascular system for treating ischaemic or atherosclerotic diseases, e.g. antianginal drugs, coronary vasodilators, drugs for myocardial infarction, retinopathy, cerebrovascula insufficiency, renal arteriosclerosis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/37Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
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  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention relates to a method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn, which comprises the following steps: s1: crushing raw materials: coating purple corn, air drying purple corn core, and crushing into coarse granules by a crusher for later use; s2: extraction: adding drinking water into the crushed raw materials obtained in the step S1, introducing carbon dioxide gas and nitrogen gas to enable the pressure in the reaction kettle to reach 1-2MPa, maintaining the pressure for 4-6 hours, and slowly releasing the pressure to obtain the product; s3: and (3) filtering: filtering the extracting solution obtained in the step S2 by a disc centrifuge and a tubular centrifuge respectively, filtering the filtrate by an ultrafiltration membrane to remove impurities, concentrating the clear solution by a nanofiltration membrane to remove small molecular impurities and redundant water, and reserving the nanofiltration concentrated solution for later use; s4: and (3) drying: and (S3) carrying out nanofiltration on the concentrated solution, and carrying out freeze drying to prepare a mixed product containing anthocyanin, procyanidine and polyphenol. The method has the advantages of good product quality, high yield and low cost.

Description

Method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn
Technical Field
The invention belongs to the technical field of extraction of plant active ingredients, and particularly relates to a method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn.
Background
Anthocyanins (also called anthocyanidins) are water-soluble natural pigments widely existing in plants in nature, and are colored aglycones obtained by hydrolyzing anthocyanins (anthocyanins). The main color-producing substances in fruits, vegetables and flowers are mostly related to the plants. Under the condition of different pH values of plant cell vacuoles, the anthocyanin enables the petals to present colorful colors. More than 20 anthocyanidins are known, and 6 important foods are pelargonidin, cyanidin, delphinidin, peonidin, morning glory pigment and malvidin. The natural anthocyanin exists in a glucoside form, is called anthocyanin, and rarely exists in a free anthocyanin. Anthocyanins are mainly used for coloring food, and can also be used in dye, medicine, and cosmetic.
Procyanidins, abbreviated as PC, is a mixture of bioflavonoids with a specific molecular structure, oligomers of which: oligomeric Proanthocyanidin (OPC) is a natural antioxidant which is internationally recognized at present and is effective in removing free radicals in human bodies. Generally a reddish brown powder, slightly smelling, astringent, soluble in water and most organic solvents. Researches show that the procyanidine extracted from the blueberry leaves can prevent the hepatitis C virus from replicating, is a bioflavonoid with a special molecular structure, and is an effective natural antioxidant capable of removing free radicals in a human body. The lipid antioxidant has strong functions of resisting oxidation and eliminating free radicals, can effectively eliminate superoxide anion free radicals and hydroxyl free radicals, also participates in metabolism of phosphoric acid and arachidonic acid and protein phosphorylation, and protects lipid from peroxidation damage; is a powerful metal chelating agent which can chelate metal ions and form inert compounds in vivo; protect and stabilize vitamin C, and is helpful for the absorption and utilization of vitamin C. The product can be used in cosmetics, and has effects of preventing sunburn, whitening skin, preventing wrinkle, resisting aging, keeping moisture, and resisting radiation.
Oxidative damage is a significant cause of many chronic diseases, such as cardiovascular diseases, cancer and aging. The antioxidant function of polyphenol can prevent these chronic diseases. In addition to the antioxidant effect, the polyphenol intake while eating high-fat food can reduce the threat of the high-fat food to the health of human bodies, which is the first discovery that the compound can effectively prevent the derivative generated by the high-fat food in the human bodies from generating adverse effect on the human bodies.
Purple corn is a unique corn variety of Peru, and corn cobs and corn kernels are purple and have extremely high phenolic compounds and anthocyanin. The purple corn contains eighteen amino acids, 21 trace elements, multiple vitamins and natural pigments which are necessary for human bodies, particularly contains anticancer element selenium, and intelligence-improving elements such as zinc, iron, calcium and the like, is excellent in taste, soft and tender, thin and smooth in skin and slightly sticky, and has special faint scent through detection of the Chinese agricultural grain quality supervision and test center, so that the food processed by the purple corn is superior natural and delicious nutritional health-care food. Meanwhile, researches find that the pigment of the purple corn has the effect of inhibiting the occurrence of cancers. In view of the effects of purple corn, the application provides a method for simultaneously extracting anthocyanin, procyanidine and polyphenol from purple corn, so as to achieve the aim of comprehensive utilization.
Disclosure of Invention
The invention aims to solve the problems and provides a method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn, and the method has the advantages of good product quality, high yield and low cost.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn comprises the following steps:
s1: crushing raw materials: coating purple corn, air drying purple corn core, and crushing into coarse granules by a crusher for later use;
s2: extraction: adding drinking water into the crushed raw materials obtained in the step S1, introducing carbon dioxide gas and nitrogen gas to enable the pressure in the reaction kettle to reach 1-2MPa, maintaining the pressure for 4-6 hours, and slowly releasing the pressure to obtain the product;
s3: and (3) filtering: filtering the extracting solution obtained in the step S2 by a disc centrifuge and a tubular centrifuge respectively, filtering the filtrate by an ultrafiltration membrane to remove impurities, concentrating the clear solution by a nanofiltration membrane to remove small molecular impurities and redundant water, and reserving the nanofiltration concentrated solution for later use;
s4: and (3) drying: and (S3) carrying out nanofiltration on the concentrated solution, and carrying out freeze drying to prepare a mixed product containing anthocyanin, procyanidine and polyphenol.
Preferably, the amount of the drinking water added in the step S2 is 5 to 10 times the amount of the crushed raw material.
Preferably, the proportion of the carbon dioxide and the nitrogen introduced in the step S2 is proportioned according to actual needs; wherein the carbon dioxide and nitrogen are combined, and can also comprise the combination of carbon dioxide and other inert gases; the ratio of 3:7 to 7:7 is preferred in the present embodiment.
Preferably, the membrane pore size of the ultrafiltration membrane in the step S3 is 1000 daltons.
Preferably, the membrane pore size of the nanofiltration membrane in the step S3 is 300 daltons.
Compared with the prior art, the invention has the beneficial effects that:
1) the traditional solvent extraction with methanol, ethanol and the like is changed, water is used as the solvent in the whole process, the problem of residual solvents such as methanol, ethanol, chloroform and the like in the product is avoided, the environmental pollution is avoided, and the cost of the product is greatly reduced;
2) carbon dioxide and nitrogen are used for pressurization, and simultaneously, part of carbon dioxide is dissolved in water to generate carbonic acid, so that the aqueous solution keeps acidic, the anthocyanin, the procyanidine and the polyphenol product are stably protected, and the use of inorganic acids such as sulfuric acid, hydrochloric acid and the like and other organic acids in the traditional method is avoided;
3) the extraction rate is improved by using gas for pressurized extraction;
4) carbon dioxide and nitrogen are used for pressurization, so that oxidative damage of oxygen and the like to anthocyanin, procyanidine and polyphenol products is avoided, and the content and yield of the products are improved;
5) Normal temperature and low temperature are used in the whole process, heating of each link in the traditional method is avoided, energy consumption is reduced, and product damage caused by temperature is reduced.
The technical scheme of the invention extracts three effective components from the coating and the core simultaneously, thus achieving the purpose of comprehensive utilization, and the product prepared by the method has good quality, high yield, low cost and wide market prospect.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described with reference to the following specific examples, which are provided for illustration only and are not intended to limit the present invention.
The technical scheme of the invention is to provide a method for simultaneously extracting and preparing anthocyanin, procyanidine and polyphenol from waste corn coatings and corncobs in the purple corn planting process, and the method is simple and easy to implement, low in cost and good in product quality.
The method is realized by the following steps:
s1: crushing raw materials: coating purple corn, air drying purple corn core, and crushing into coarse granules by a crusher for later use;
s2: extraction: adding 5-10 times of drinking water into the crushed raw materials, and then introducing carbon dioxide gas and nitrogen gas, wherein the ratio of the carbon dioxide gas to the nitrogen gas is 3: 7-7: 7; introducing gas to make the pressure in the reaction kettle reach 1-2MPa, maintaining the pressure for 4-6 hours, and then slowly releasing the pressure;
S3: and (3) filtering: filtering the above extractive solutions with disc centrifuge and tubular centrifuge respectively, filtering the filtrate with ultrafiltration membrane with membrane aperture of 1000 daltons to remove impurities such as protein and saccharide, concentrating the clear solution with nanofiltration membrane with membrane aperture of 300 daltons to remove small molecular impurities and excessive water, and collecting the nanofiltration concentrated solution;
s4: and (3) drying: and (4) carrying out nanofiltration on the concentrated solution in the previous step, and carrying out freeze drying to prepare a mixed product containing anthocyanin, procyanidine and polyphenol.
Example 1:
1. crushing raw materials: crushing 500kg of dried purple corn coatings into coarse particles by a crusher for later use;
2. extraction: adding 10 times of drinking water into the crushed raw materials, and then introducing carbon dioxide gas and nitrogen gas, wherein the ratio of the carbon dioxide gas to the nitrogen gas is 3: 7; introducing gas to enable the pressure in the reaction kettle to reach 1MPa, maintaining the pressure for 4 hours, and then slowly releasing the pressure to obtain the product;
3. and (3) filtering: filtering the above extractive solutions with disc centrifuge and tubular centrifuge respectively, filtering the filtrate with ultrafiltration membrane with membrane aperture of 1000 Dalton, concentrating the clear solution with nanofiltration membrane with membrane aperture of 300 Dalton, removing small molecular impurities and excessive water, and collecting the nanofiltration concentrated solution;
4. And (3) drying: and (3) carrying out nanofiltration on the concentrated solution in the previous step, and freeze-drying to obtain 5.3kg of a mixed product containing anthocyanin, procyanidin and polyphenol, wherein the anthocyanin content is 29.5%, the procyanidin content is 68%, and the polyphenol content is 75%.
Example 2:
1. crushing raw materials: crushing 500kg of dried purple corn cores into coarse particles by a crusher for later use;
2. extraction: adding 8 times of drinking water into the crushed raw materials, and then introducing carbon dioxide gas and nitrogen gas, wherein the ratio of the carbon dioxide gas to the nitrogen gas is 5: 7; introducing gas to enable the pressure in the reaction kettle to reach 2MPa, maintaining the pressure for 5 hours, and then slowly releasing the pressure to obtain the product;
3. and (3) filtering: filtering the above extractive solutions with disc centrifuge and tubular centrifuge respectively, filtering the filtrate with ultrafiltration membrane with membrane aperture of 1000 Dalton, concentrating the clear solution with nanofiltration membrane with membrane aperture of 300 Dalton, removing small molecular impurities and excessive water, and collecting the nanofiltration concentrated solution;
4. and (3) drying: and (3) carrying out nanofiltration on the concentrated solution in the previous step, and freeze-drying to obtain 6.8kg of a mixed product containing anthocyanin, procyanidin and polyphenol, wherein the anthocyanin content is 31.5%, the procyanidin content is 65%, and the polyphenol content is 73%.
Example 3:
1. Crushing raw materials: crushing 500kg of dried purple corn coatings into coarse particles by a crusher for later use;
2. extraction: adding 5 times of drinking water into the crushed raw materials, and then introducing carbon dioxide gas and nitrogen gas, wherein the ratio of the carbon dioxide gas to the nitrogen gas is 7: 7; introducing gas to enable the pressure in the reaction kettle to reach 1.5MPa, maintaining the pressure for 6 hours, and then slowly releasing the pressure to obtain the product;
3. and (3) filtering: filtering the above extractive solutions with disc centrifuge and tubular centrifuge respectively, filtering the filtrate with ultrafiltration membrane with membrane aperture of 1000 Dalton, concentrating the clear solution with nanofiltration membrane with membrane aperture of 300 Dalton, removing small molecular impurities and excessive water, and collecting the nanofiltration concentrated solution;
4. and (3) drying: and (3) carrying out nanofiltration on the concentrated solution in the previous step, and freeze-drying to obtain 5.6kg of a mixed product containing anthocyanin, procyanidin and polyphenol, wherein the anthocyanin content is 28.7%, the procyanidin content is 71%, and the polyphenol content is 74%.
The proportion of carbon dioxide and nitrogen is proportioned according to actual needs; wherein the carbon dioxide and nitrogen are combined, and can also comprise the combination of carbon dioxide and other inert gases; the ratio of 3:7 to 7:7 is preferred in the present embodiment.
The details of the present invention not described in detail are prior art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (5)

1. A method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn is characterized by comprising the following steps:
s1: crushing raw materials: coating purple corn, air drying purple corn core, and crushing into coarse granules by a crusher for later use;
s2: extraction: adding drinking water into the crushed raw materials obtained in the step S1, introducing carbon dioxide gas and nitrogen gas to enable the pressure in the reaction kettle to reach 1-2MPa, maintaining the pressure for 4-6 hours, and slowly releasing the pressure to obtain the product;
s3: and (3) filtering: filtering the extracting solution obtained in the step S2 by a disc centrifuge and a tubular centrifuge respectively, filtering the filtrate by an ultrafiltration membrane to remove impurities, concentrating the clear solution by a nanofiltration membrane to remove small molecular impurities and redundant water, and reserving the nanofiltration concentrated solution for later use;
s4: and (3) drying: and (S3) carrying out nanofiltration on the concentrated solution, and carrying out freeze drying to prepare a mixed product containing anthocyanin, procyanidine and polyphenol.
2. The method for simultaneously preparing anthocyanidin, procyanidine and polyphenol from purple corn as claimed in claim 1, wherein the amount of drinking water added in step S2 is 5-10 times of the amount of the crushed raw material.
3. The method for simultaneously preparing anthocyanidin, procyanidine and polyphenol from purple corn as claimed in claim 1, wherein the ratio of carbon dioxide and nitrogen introduced in step S2 is proportioned according to actual needs.
4. The method for simultaneously preparing anthocyanidin, procyanidin and polyphenol from purple corn as claimed in claim 1, wherein the membrane pore size of the ultrafiltration membrane in the step S3 is 1000 Dalton.
5. The method for simultaneously preparing anthocyanidin, procyanidin and polyphenol from purple corn as claimed in claim 1, wherein the membrane pore size of the nanofiltration membrane in step S3 is 300 Dalton.
CN202010681730.8A 2020-07-15 2020-07-15 Method for simultaneously preparing anthocyanin, procyanidine and polyphenol from purple corn Pending CN111848567A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113826736A (en) * 2021-08-23 2021-12-24 朱海英 Purple corn substituted tea and preparation method thereof
CN117530445A (en) * 2023-12-22 2024-02-09 广州泽力医药科技有限公司 Purple corn compound beverage and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105601686A (en) * 2016-02-02 2016-05-25 长沙蓝威生物制品有限公司 Method for extracting cyanidin from roselle
CN106008443A (en) * 2016-07-22 2016-10-12 河南科技大学 Extraction method of purple corn anthocyanin
CN107033118A (en) * 2017-04-19 2017-08-11 北海市韩能生物科技有限公司 The extracting method of OPC
CN107552536A (en) * 2017-09-05 2018-01-09 贵州慧静生物科技有限公司 Grape wine waste residue integrated extraction technique

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105601686A (en) * 2016-02-02 2016-05-25 长沙蓝威生物制品有限公司 Method for extracting cyanidin from roselle
CN106008443A (en) * 2016-07-22 2016-10-12 河南科技大学 Extraction method of purple corn anthocyanin
CN107033118A (en) * 2017-04-19 2017-08-11 北海市韩能生物科技有限公司 The extracting method of OPC
CN107552536A (en) * 2017-09-05 2018-01-09 贵州慧静生物科技有限公司 Grape wine waste residue integrated extraction technique

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113826736A (en) * 2021-08-23 2021-12-24 朱海英 Purple corn substituted tea and preparation method thereof
CN117530445A (en) * 2023-12-22 2024-02-09 广州泽力医药科技有限公司 Purple corn compound beverage and preparation method thereof

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