CN101301319A - Preparation of granada flower polyphenol and uses thereof - Google Patents

Preparation of granada flower polyphenol and uses thereof Download PDF

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Publication number
CN101301319A
CN101301319A CNA2008100729105A CN200810072910A CN101301319A CN 101301319 A CN101301319 A CN 101301319A CN A2008100729105 A CNA2008100729105 A CN A2008100729105A CN 200810072910 A CN200810072910 A CN 200810072910A CN 101301319 A CN101301319 A CN 101301319A
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polyphenol
water
extract
granada
acetone
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CNA2008100729105A
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Chinese (zh)
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阿吉艾克拜尔·艾萨
热依木古丽·阿布都拉
黄昀
刘力
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Priority to CNA2008100729105A priority Critical patent/CN101301319A/en
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Abstract

The invention relates to a preparation method and an application of pomegranate polyphenol. The method is as follows: fresh pomegranate follows are collected, washed and smashed. An organic solvent is used to extract soluble material containing pomegranate polyphenol from the smashed pomegranate flowers. Then a pomegranate polyphonol concentrated solution is obtained form polyphenol extract by enrichment through a macroporous absorption resin method. The polyphonol concentrated solution is subject to spray drying and freeze drying to obtain high-purity pomegranate polyphenol. The pomegranate polyphenol obtained by the method is more than 70 percent, with a yield rate more than 10.3/100g (pomegranate flower), has non-oxidizability, is particularly suitable for food, health care product or medicine and provides an effective way for the comprehensive application of plant pomegranate polyphenol.

Description

The preparation method of granada flower polyphenol and application thereof
Technical field
The present invention relates to a kind of preparation method of granada flower polyphenol, lose weight, increase the medicinal usage of immunity, antioxidative functional food adjuvant and auxiliary treatment atherosclerosis, diabetes, hypertension and cancer by the granada flower polyphenol of this method acquisition as preparation.
Background technology
The flower of Punica granatum L. Pittosporum Punicaceae plant Punica granatum L. (punica grantum L.), alabastrum are red.Contain glucose, fructose, tannic acid (tannin) etc. in the Flos Granati.In ethnomedicine plain with the title of " Gu Li moves " people's medicine, have antidiarrheal, hemostasis, effect such as antipruritic, can be used as the drug use of treatment halitosis, bromhidrosis; Ancients usually will spend battalion's sugaring to make extractum, in order to treatment gastric ulcer and straightforward words tripe; Flos Granati removes and can be used to treat diseases such as neurasthenia, insomnia, also has the effect of building body.
Punica granatum L. polyphenol is the general name that a class has the polyphenol hydroxyl chemical compound, comprise multiple chemical compounds such as elladitannin, Galla Turcica (Galla Helepensis) tannin, ellagic acid, gallic acid, catechin, anthocyanidin, chlorogenic acid, ferulic acid, at present pharmaceutical research shows that Punica granatum L. polyphenol just has biological activitys such as antioxidation, defying age, antibiotic, antiviral, blood pressure lowering, blood fat reducing and arteriosclerosis.Therefore, aspect the treatment cardiovascular diseases DEVELOPMENT PROSPECT is widely being arranged.
Flos Granati is being bloomed to forming in alabastrum, the outcome procedure, because the influence of natural phenomenas such as wind, rain, only having 1/3 can the result, and all the other 2/3 are wasted because of landing.Therefore from Flos Granati, extract and the preparation medicinal ingredient for increasing additional value of farm products and its very big effect of comprehensive utilization ratio aspect.
At present Flos Granati is had only flavonoid and pigment aspect are had research, as patent of invention (application number: 200610045466.9) " from Flos Granati, extract the method for Flavonoid substances, ellagic acid ", disclosing a kind of is raw material with the Flos Granati, drench through dashing, dry, use methods such as deionized water heating extraction, filtration, reverse osmosis concentration, spray drying, finally obtain the method for Flavonoid substances, ellagic acid.
And preparing the granada flower polyphenol compounds, relevant employing macroporous resin do not appear in the newspapers.
Summary of the invention
The object of the invention is, a kind of solvent method or macroporous adsorbent resin method or solvent method and macroporous adsorbent resin method combined preparation polyphenol compound of adopting from Flos Granati is provided.The granada flower polyphenol that obtains by this method is used to lose weight, increase the purposes of immunity, antioxidative functional food adjuvant and the purposes that conduct prepares the medicine of auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.Prepare the quality safety authentication requesting that polyphenol compound is nontoxic, meet fields such as food, medicine by the inventive method.Thereby provide effective way for the comprehensive utilization of this characteristic plant of Flos Granati.From Flos Granati, extract and prepare polyphenol compound and play a big part for increasing additional value of farm products and comprehensive utilization ratio aspect.
The preparation method of a kind of granada flower polyphenol of the present invention follows these steps to carry out:
A, gather fresh Flos Granati, clean broken, water or alcohol or water and the mixture of alcohol or the mixture of acetone and water that 6-40 doubly measures will be added in the broken Flos Granati, soak and extract the solable matter that contains granada flower polyphenol, extract 20-60 ℃ of temperature, extraction time 0.5-3 hour, extract 1-3 time, filter, merging filtrate is removed medicinal residues;
B, with filtrate under 40 ℃, concentrating under reduced pressure, drying obtains the crude extract that polyphenol content is 30-40%;
C, with the crude extract of step b, after being dissolved in water, by macroporous adsorbent resin, behind the water eluting impurity, the aqueous mixtures eluting of reuse 20-95% ethanol or acetone, effluent are through concentrating under reduced pressure, drying obtains the Flos Granati total phenols, content reaches 60-80%;
D or with the filtrate of step a, concentrate recovery alcohol or acetone down to tasteless in 40 ℃ of temperature, behind the thin up, by macroporous adsorbent resin, behind the water eluting impurity, the aqueous mixtures eluting of reuse 20-95% ethanol or acetone, effluent is through concentrating under reduced pressure, drying obtains the Flos Granati total phenols, and content reaches 60-80%.
The concentration of pure and mild acetone is 20-80% among the step a, and alcohol comprises methanol, ethanol or butanols, preferred alcohol.
Step b, c and d dry employing vacuum drying or cryogenic vacuum spray drying or lyophilization concentrate and the vacuum drying temperature all is advisable at 30-40 ℃.
Step c and d amount of water are 1-5 times;
Step c and d eluting impurity water consumption are 2-5 times of volume.
Step c and d macroporous adsorbent resin are the nonpolar of styrene skeleton or low pole macroporous adsorbent resin, as: D101 type, HPD-750 type, HPD-450 type, HPD-100 type AB-8 or X-5 type.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at fat-reducing, increase immunity or antioxidative functional food adjuvant.
The granada flower polyphenol that described preparation method obtains is as the purposes of the medicine of preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
The specific embodiment
Embodiment 1:
Gather fresh Flos Granati 500g, clean fragmentation, will add the water of 6 times of amounts in the broken Flos Granati, soak extraction and contain granada flower polyphenol, extract 20 ℃ of temperature, 0.5 hour extraction time, to extract 1 time, medicinal residues are removed in filtration;
With filtrate under 40 ℃ of temperature, concentrating under reduced pressure, in 40 ℃ of following vacuum dryings of temperature, polyphenol content is 30% crude extract;
With crude extract, after adding 5 times of water dissolutioies, by the 1kg that has handled well, D101 type macroporous adsorbent resin, behind 2 times of volume pure water eluting impurity, reuse 40% alcoholic acid aqueous mixtures eluting, concentration is 20%, effluent obtains granada flower polyphenol at 40 ℃ of following vacuum dryings of temperature, and content reaches 60%.
The granada flower polyphenol that is obtained is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 2:
Gather fresh Flos Granati, clean fragmentation, will add 20% methanol of 10 times of amounts in the broken Flos Granati, soak and extract the solable matter that contains granada flower polyphenol, extract 30 ℃ of temperature, 2 hours extraction times, extract 2 times, filtration, merging filtrate is removed medicinal residues;
With filtrate, concentrate recovery methanol down to tasteless in 30 ℃ of temperature, after adding 2 times of water gaging dilutions, by 1k g, the HPD-750 type macroporous adsorbent resin of having handled well, behind 3 times of volume water elution impurity, reuse 20% alcoholic acid aqueous mixtures eluting, effluent is through concentrating under reduced pressure, adopt lyophilization, obtain granada flower polyphenol, content reaches 66%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 3:
Gather fresh Flos Granati 500g, clean fragmentation, will add 60% acetone of 30 times of amounts in the broken Flos Granati, soak and extract granada flower polyphenol, extract 45 ℃ of temperature, 1.5 hours extraction times, extract 2 times, filtration, merging filtrate is removed medicinal residues;
With filtrate under 40 ℃ of temperature, concentrating under reduced pressure, the cryogenic vacuum spray drying, polyphenol content is 35% crude extract;
With crude extract, after adding 4 times of water dissolutioies, by the 1kg that has handled well, the macroporous adsorbent resin of AB-8 type, behind 4 times of volume pure water eluting impurity, the aqueous mixtures eluting of reuse 60% acetone, effluent adopt the cryogenic vacuum spray drying through concentrating under reduced pressure, obtain the Flos Granati total phenols, content reaches 70%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 4:
Gather fresh Flos Granati 500g, clean fragmentation, will add 60% butanols of 40 times of amounts in the broken Flos Granati, soak and extract granada flower polyphenol, extract 60 ℃ of temperature, 3 hours extraction times, extract 3 times, filtration, merging filtrate is removed medicinal residues;
With filtrate, concentrate the recovery butanols down to tasteless in 30 ℃, after adding 4 times of water dilutions, by the 1kg that has handled, X-5 type macroporous adsorbent resin, behind 5 times of volume pure water eluting impurity, reuse 95% alcoholic acid aqueous mixtures eluting, effluent adopt lyophilization through concentrating under reduced pressure, obtain the Flos Granati total phenols, content reaches 75%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 5:
Gather fresh Flos Granati 500g, clean fragmentation, will add 80% ethanol of 35 times of amounts in the broken Flos Granati, immersion extraction granada flower polyphenol, extract 50 ℃ of temperature, 2 hours extraction times, extract 2 times, filtration, merging filtrate is removed medicinal residues;
With filtrate under 40 ℃ of temperature, concentrating under reduced pressure, in 40 ℃ of following vacuum dryings of temperature, polyphenol content is 40% crude extract;
With crude extract, add 3 times water dissolution after, by the 1kg that has handled, HPD-100 type macroporous adsorbent resin, behind 4 times of volume pure water eluting impurity, reuse 70% alcoholic acid aqueous mixtures eluting, effluent is through concentrating under reduced pressure, adopt vacuum drying, obtain the Flos Granati total phenols, content reaches 79%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 6:
Gather fresh Flos Granati 500g, clean fragmentation, will add 40% acetone of 10 times of amounts in the broken Flos Granati, soak and extract granada flower polyphenol, extract 40 ℃ of temperature, 3 hours extraction times, extract 3 times, filtration, merging filtrate is removed medicinal residues;
With filtrate, concentrate recovery acetone down to tasteless in 35 ℃ of temperature, after adding 2 times of water dilutions, by the 1kg that has handled, XB-8 type macroporous adsorbent resin, behind 3 times of volume pure water eluting impurity, the aqueous mixtures eluting of reuse 30% acetone, effluent adopt 30 ℃ of vacuum dryings of temperature through concentrating under reduced pressure, obtain the Flos Granati total phenols, content reaches 78%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 7:
Gather fresh Flos Granati 500g, clean fragmentation, will add 50% methanol of 28 times of amounts and the mixture of water in the broken Flos Granati, immersion extraction granada flower polyphenol, extract 50 ℃ of temperature, 2 hours extraction times, extract 2 times, filtration, merging filtrate is removed medicinal residues;
With filtrate under 40 ℃ of temperature, concentrating under reduced pressure, lyophilization, polyphenol content is 38% crude extract;
With crude extract, add 4 times water dissolution after, by the 1kg that has handled, D101 type macroporous adsorbent resin, behind 4 times of volume pure water eluting impurity, reuse 50% alcoholic acid aqueous mixtures eluting, effluent is through concentrating under reduced pressure, adopt lyophilization, obtain the Flos Granati total phenols, content reaches 80%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 8:
Gather fresh Flos Granati 500g, clean fragmentation, will add 70% acetone of 15 times of amounts and the mixture of water in the broken Flos Granati, soak and extract granada flower polyphenol, extract 55 ℃ of temperature, 2.5 hours extraction times, extract 3 times, filtration, merging filtrate is removed medicinal residues;
With filtrate, concentrate recovery acetone down to tasteless in 30 ℃, after adding 1 times of water dilution, by the 1kg that has handled, HPD-450 type macroporous adsorbent resin, behind 2 times of volume pure water eluting impurity, the aqueous mixtures eluting of reuse 95% acetone, effluent are used in 40 ℃ of following vacuum dryings of temperature through concentrating under reduced pressure, obtain the Flos Granati total phenols, content reaches 68%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 9:
Gather fresh Flos Granati 500g, clean fragmentation, will add 30% ethanol of 8 times of amounts and the mixture of water in the broken Flos Granati, immersion extraction granada flower polyphenol, extract 25 ℃ of temperature, 0.5 hour extraction time, to extract 1 time, medicinal residues are removed in filtration;
With filtrate under 40 ℃ of temperature, concentrating under reduced pressure, the cryogenic vacuum spray drying, polyphenol content is 40% crude extract;
With crude extract, after adding 5 times water dissolution, by the 1kg that has handled, HPD-750 type macroporous adsorbent resin, behind 5 times of volume pure water eluting impurity, reuse 85% alcoholic acid aqueous mixtures eluting, effluent is through concentrating under reduced pressure, adopt the cryogenic vacuum spray drying, obtain the Flos Granati total phenols, content reaches 80%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
Embodiment 10:
Gather fresh Flos Granati 500g, clean fragmentation, will add 70% butanols of 36 times of amounts and the mixture of water in the broken Flos Granati, immersion extraction granada flower polyphenol, extract 25 ℃ of temperature, 2.5 hours extraction times, extract 3 times, filtration, merging filtrate is removed medicinal residues;
With filtrate, concentrate the recovery butanols down to tasteless in 30 ℃ of temperature, after adding 2 times of water dilutions, by the 1kg that has handled, X-5 type macroporous adsorbent resin, behind 2 times of volume pure water eluting impurity, the aqueous mixtures eluting of reuse 80% acetone, effluent are used in 40 ℃ of following vacuum dryings of temperature through concentrating under reduced pressure, obtain the Flos Granati total phenols, content reaches 79%.
The granada flower polyphenol that described preparation method obtains is as the purposes of preparation at the medicine of fat-reducing, the purposes that increases immunity, anti-oxidation functional food adjuvant or conduct preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.

Claims (8)

1, a kind of preparation method of granada flower polyphenol is characterized in that following these steps to carrying out:
A, gather fresh Flos Granati, clean broken, water or alcohol or water and the mixture of alcohol or the mixture of acetone and water that 6-40 doubly measures will be added in the broken Flos Granati, soak and extract the solable matter that contains granada flower polyphenol, extract 20-60 ℃ of temperature, extraction time 0.5-3 hour, extract 1-3 time, filter, merging filtrate is removed medicinal residues;
B, with filtrate under 40 ℃, concentrating under reduced pressure, drying obtains the crude extract that polyphenol content is 30-40%;
C, with the crude extract of step b, after being dissolved in water, by macroporous adsorbent resin, behind the water eluting impurity, the aqueous mixtures eluting of reuse 20-95% ethanol or acetone, effluent are through concentrating under reduced pressure, drying obtains the Flos Granati total phenols, content reaches 60-80%;
D or with the filtrate of step a, concentrate recovery alcohol or acetone down to tasteless in 40 ℃ of temperature, behind the thin up, by macroporous adsorbent resin, behind the water eluting impurity, the aqueous mixtures eluting of reuse 20-95% ethanol or acetone, effluent is through concentrating under reduced pressure, drying obtains the Flos Granati total phenols, and content reaches 60-80%.
2, preparation method according to claim 1, the concentration that it is characterized in that pure and mild acetone among the step a is 20-80%, alcohol comprises methanol, ethanol or butanols, preferred alcohol.
3, require 1 described preparation method according to patent, it is characterized in that step b, c and d dry employing vacuum drying or cryogenic vacuum spray drying or lyophilization, concentrate with the vacuum drying temperature and all be advisable at 30-40 ℃.
4, preparation method according to claim 1 is characterized in that step c and d amount of water are 1-5 times.
5, preparation method according to claim 1 is characterized in that step c and d eluting impurity water consumption are 2-5 times of volume.
6, preparation method according to claim 1, it is characterized in that step c and d macroporous adsorbent resin are the nonpolar of styrene skeleton or low pole macroporous adsorbent resin, as: D101 type, HPD-750 type, HPD-450 type, HPD-100 type, AB-8 or X-5 type.
7, the granada flower polyphenol of preparation method acquisition according to claim 1 is as the purposes of preparation at fat-reducing, increase immunity or antioxidative functional food adjuvant.
8, the granada flower polyphenol of preparation method acquisition according to claim 1 is as the purposes of the medicine of preparation auxiliary treatment atherosclerosis, diabetes, hypertension or cancer.
CNA2008100729105A 2008-07-09 2008-07-09 Preparation of granada flower polyphenol and uses thereof Pending CN101301319A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
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CN101838292A (en) * 2010-06-22 2010-09-22 屏南健青生物科技有限公司 Method for extracting and separating polyphenol from plants
CN102641312A (en) * 2012-05-21 2012-08-22 新疆医科大学 Use of polyphenols from pomegranate flowers in preparation of medicaments for treating non-alcoholic fatty liver
WO2012088519A3 (en) * 2010-12-23 2012-09-13 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodenegenerative diseases and cognitive disorders
CN102755360A (en) * 2012-07-24 2012-10-31 西华大学 Method for extracting pomegranate peel polyphenols from pomegranate peel
CN104814505A (en) * 2015-04-21 2015-08-05 昆明学院 Natural compound antioxidant preparation method and application
CN110585324A (en) * 2019-09-24 2019-12-20 上海应用技术大学 Extraction and purification method of hemerocallis fulva flower polyphenol
CN111471307A (en) * 2020-03-19 2020-07-31 江西师范大学 Preparation method of degradable collagen packaging material
CN111529556A (en) * 2020-05-15 2020-08-14 陕西师范大学 Application of punicosides in health food or medicine for improving obesity-related adipose tissue remodeling
US11166937B2 (en) 2018-06-18 2021-11-09 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838292A (en) * 2010-06-22 2010-09-22 屏南健青生物科技有限公司 Method for extracting and separating polyphenol from plants
CN101838292B (en) * 2010-06-22 2013-01-23 屏南健青生物科技有限公司 Method for extracting and separating polyphenol from plants
US10857126B2 (en) 2010-12-23 2020-12-08 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
WO2012088519A3 (en) * 2010-12-23 2012-09-13 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodenegenerative diseases and cognitive disorders
US10485782B2 (en) 2010-12-23 2019-11-26 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
US10028932B2 (en) 2010-12-23 2018-07-24 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
AU2011348068B2 (en) * 2010-12-23 2016-05-05 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
US9872850B2 (en) 2010-12-23 2018-01-23 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
CN102641312B (en) * 2012-05-21 2013-10-30 新疆医科大学 Use of polyphenols from pomegranate flowers in preparation of medicaments for treating non-alcoholic fatty liver
CN102641312A (en) * 2012-05-21 2012-08-22 新疆医科大学 Use of polyphenols from pomegranate flowers in preparation of medicaments for treating non-alcoholic fatty liver
CN102755360A (en) * 2012-07-24 2012-10-31 西华大学 Method for extracting pomegranate peel polyphenols from pomegranate peel
CN104814505A (en) * 2015-04-21 2015-08-05 昆明学院 Natural compound antioxidant preparation method and application
CN104814505B (en) * 2015-04-21 2019-06-04 昆明学院 A kind of preparation method and applications of natural composite antioxidant
US11166937B2 (en) 2018-06-18 2021-11-09 Amazentis Sa Compositions and methods for improving mitochondrial function and treating neurodegenerative diseases and cognitive disorders
CN110585324A (en) * 2019-09-24 2019-12-20 上海应用技术大学 Extraction and purification method of hemerocallis fulva flower polyphenol
CN111471307A (en) * 2020-03-19 2020-07-31 江西师范大学 Preparation method of degradable collagen packaging material
CN111529556A (en) * 2020-05-15 2020-08-14 陕西师范大学 Application of punicosides in health food or medicine for improving obesity-related adipose tissue remodeling

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