CN101041675A - Method for extracting glutinous rehmannia oligose and glutinous rehmannia polysaccharide from glutinous rehmannia - Google Patents
Method for extracting glutinous rehmannia oligose and glutinous rehmannia polysaccharide from glutinous rehmannia Download PDFInfo
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Abstract
The invention discloses an extracting method of oligosaccharide and polysaccharide of glutinous rehmannia from rehmannia root, which comprises the following steps: washing fresh rehmannia root through clean water; grinding; or immersing dry rehmannia root for 1-10h; grinding; centrifuging through high-speed centrifuger to obtain filtrate of glutinous rehmannia and slag of glutinous rehmannia; hyperfiltering through 50000D hyperfilter film,10000D hyperfilter film, 1000D nano-filter film and 500D nano-filter film grade by grade; condensing liquid on the film until the sugar content is about 10-50%; cooling; adding alcohol to stir 0.1-1h; filtering; drying the filter slag under 100deg.c to obtain the polysaccharide product; spraying to dry after condensing liquid in the vacuum evaporator until the sugar content is 10-50%; spraying to dry; obtaining the oligosaccharide product with stachyose not less than 80%.
Description
Technical field
The present invention relates to a kind of glutinous rehmannia and extract the method for rehmannia root oligose, Dihuang polysaccharide.
Background technology
Glutinous rehmannia is a kind of Chinese medicinal materials, has another name called the dried rhizome of rehmannia, and sweet-bitter flavor is cold in nature; Heat-clearing, promote the production of body fluid, moisturize, cool blood, hemostasis; The dried rhizome of rehmannia is further concocted the back and is cultivated land.The dried root of Shi Xuan Ginseng section plant bosom glutinous rehmannia.Effects such as that the dried rhizome of rehmannia has is nourishing Yin and clearing heat, cooling blood for hemostasis; Control deficiency of Yin low-heat, pyreticosis agitation, body fluid few, send out diseases such as spot dermexanthesis, hemoptysis, haematemesis, menoxenia, hematuria, uterine bleeding.The cultivated land flavor is sweet, warm in nature; Return liver, kidney channel; Effects such as nourishing YIN and supplementing blood strengthening and nourishing marrow and essence are arranged; Control diseases such as deficiency of Yin blood is few, the deficiency of blood is weak, the frightened dizziness of the heart, dim eyesight, emission due to deficiency of the kidney, deficiency of Yin hemoptysis, soreness of the waist and knees, uterine bleeding.Glutinous rehmannia contains multiple glycoside composition and carbohydrate, can extract rehmannia root oligose, Dihuang polysaccharide from glutinous rehmannia.Carbohydrate has the branch of polysaccharide, oligose, monose according to the difference of glycan molecule.It is all that can not to be hydrolyzed to more micromolecular sugar again be monose; The sugar of 10 above unit molecule compositions is polysaccharide; By 2～9 molecular sugar of monose then is oligose, claims oligosaccharides again.Dihuang polysaccharide has the effect that improves immunity function, suppresses tumour; Rehmannia root oligose can strengthen hemopoietic function and promote immunity, the effect of lowering blood glucose, can promote the hyperplasia of bifidus bacillus in the human intestinal, can be used for treating acute and chronic diarrhoea, hepatogenic encephalopathy, particularly the glutinous rehmannia oligose can and be regulated intestinal microecology and constipation is produced the comprehensive therapy effect by its hypertonicity, makes rehmannia root oligose, Dihuang polysaccharide are familiar with by people more and more and utilize.But the glutinous rehmannia of prior art is extracted the method complex technical process of rehmannia root oligose, Dihuang polysaccharide, cost of manufacture height.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the method that provides a kind of glutinous rehmannia to extract rehmannia root oligose, Dihuang polysaccharide has the advantages that extraction process is simple, reasonable, cost of manufacture is cheap.
The technical solution adopted for the present invention to solve the technical problems is: a kind of glutinous rehmannia is extracted the method for rehmannia root oligose, Dihuang polysaccharide, and it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. with filtrate by 50000D (dalton) ultra-filtration membrane be separated into 〉=the A liquid of 50000D and≤the B liquid of 50000D;
D. with B liquid by the 10000D ultra-filtration membrane be separated into 10000～50000D C liquid and≤the D liquid of 10000D;
E. with D liquid by 1000D sodium filter membrane be separated into 1000～10000D E liquid and≤the F liquid of 1000D;
F. with F liquid by 500D sodium filter membrane be separated into 500～1000D G liquid and≤the H liquid of 500D;
G. C liquid is concentrated into sugar degree 10～50% with vacuum-evaporator heating, adds 1～9 times of ethanol after the cooling and stirred 0.1～1 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product;
H. G liquid is concentrated into sugar degree 10～50% with vacuum-evaporator, spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
A kind of glutinous rehmannia is extracted the method for rehmannia root oligose, and it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. filtrate is separated by 50000D (dalton) ultra-filtration membrane and obtain on the film liquid under the liquid and film;
D. getting under the film that above-mentioned steps c obtains liquid separates by the 10000D ultra-filtration membrane and obtains on the film liquid under the liquid and film;
E. getting under the film that above-mentioned steps d obtains liquid separates by 1000D sodium filter membrane and obtains on the film liquid under the liquid and film;
F. getting under the film that above-mentioned steps e obtains liquid separates by 500D sodium filter membrane and obtains on the film liquid under the liquid and film;
G. get that liquid is concentrated into sugar degree 10～50% with vacuum-evaporator on the film that above-mentioned steps f obtains, spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
A kind of glutinous rehmannia is extracted the method for Dihuang polysaccharide, and it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. filtrate is separated by 50000D (dalton) ultra-filtration membrane and obtain on the film liquid under the liquid and film;
D. getting under the film that above-mentioned steps c obtains liquid separates by the 10000D ultra-filtration membrane and obtains on the film liquid under the liquid and film;
E. get that liquid is concentrated into sugar degree 10～50% with the vacuum-evaporator heating on the film that above-mentioned steps d obtains, add 1～9 times of ethanol after the cooling and stirred 0.1～1 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product.
Glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, Dihuang polysaccharide, or glutinous rehmannia is extracted the method for rehmannia root oligose, or glutinous rehmannia is extracted the method for Dihuang polysaccharide, can also further be utilized by the slag that produces in each process of its technology, liquid, such as being used to produce Catalpol, amino acid, fodder additives etc.
Glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, Dihuang polysaccharide, or glutinous rehmannia is extracted the method for rehmannia root oligose, or glutinous rehmannia is extracted the method for Dihuang polysaccharide, be with the glutinous rehmannia raw material, glutinous rehmannia is the fresh or dried root of scrophulariaceae rehmannia glutinosa plant Rehmannia glutinosa Libosch, has the Yin-nourishing and body fluid promoting effect, modern pharmacological research is found, glutinous rehmannia has the adjusting immunologic function, influence cardiovascular systems, hemopoietic system, endocrine system, each side activity such as central nervous system, and have many-sided effects such as antitumor, anti-ageing and hypoglycemic.The Dihuang polysaccharide that extracts from glutinous rehmannia has the effect that improves immunity function, suppresses tumour; The rehmannia root oligose that extracts from glutinous rehmannia can strengthen hemopoietic function promotion immunity, the effect of lowering blood glucose, can promote the hyperplasia of bifidus bacillus in the human intestinal, can be used for treating acute and chronic diarrhoea, hepatogenic encephalopathy, particularly rehmannia root oligose can and regulate intestinal microecology and constipation is produced the comprehensive therapy effect by its hypertonicity.
Glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, Dihuang polysaccharide, or glutinous rehmannia is extracted the method for rehmannia root oligose, or glutinous rehmannia is extracted the method for Dihuang polysaccharide, be to have adopted membrane separation technique to realize from glutinous rehmannia, extracting rehmannia root oligose, Dihuang polysaccharide, the existing separation of membrane separation technique, concentrate, purifying and purified function, efficient, energy-saving and environmental protection are arranged again, molecular level filters and filtration procedure is simple, be easy to feature such as control.Adopt membrane separation technique to extract rehmannia root oligose, Dihuang polysaccharide, can realize sepn process efficiently and less energy-consumption; The working temperature near room temperature of sepn process makes extraction process be convenient to operate and be convenient to serialization production; Because adopting membrane sepn is pure physical process, any chemical transformation can not take place, and does not more need to add any material, as flocculating aids, chemical reagent etc., thereby extraction process is oversimplified, cost of manufacture is cheap; Because the equipment of membrane separation technique itself does not have moving parts, about room temperature, reliability is very high, thereby the quality stability of product is good again in work; Because the equipment making material of membrane separation technique cleaning, environmental protection, thereby make and the job site sanitation and hygiene meet the requirement that environmental protection is produced.
The invention has the beneficial effects as follows, owing to adopted membrane separation technique to realize from glutinous rehmannia, extracting rehmannia root oligose, Dihuang polysaccharide, clean with clear water by the Rehmannia Root of will gather in the crops in the ground, grind or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation, then filtrate is passed through 50000D (dalton) ultra-filtration membrane, the 10000D ultra-filtration membrane, 1000D sodium filter membrane, the stage trapping of 500D sodium filter membrane, liquid on the film after the separation of 10000D ultra-filtration membrane is concentrated into sugar degree 10～50% with the vacuum-evaporator heating, adding 1～9 times of ethanol after the cooling stirred 0.1～1 hour, liquid is abandoned in filtration, filter residue can get the Dihuang polysaccharide finished product in oven dry below 100 ℃, liquid on the film after the separation of 500D sodium filter membrane is concentrated into sugar degree 10～50% with vacuum-evaporator, spraying drying can contain stachyose 〉=80% rehmannia root oligose finished product, and it is simple to have extraction process, rationally, the advantage that cost of manufacture is cheap.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail; But the method that a kind of glutinous rehmannia of the present invention is extracted rehmannia root oligose, Dihuang polysaccharide is not limited to embodiment.
Embodiment one, and a kind of glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, Dihuang polysaccharide, and it comprises the steps:
Step a. cleans the Rehmannia Root of gathering in the crops in the ground, grind with clear water, gets ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
Step b. with the ground speiss add water logging 8 hours again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
Step c with filtrate by 50000D (dalton) ultra-filtration membrane be separated into 〉=the A liquid of 50000D and≤the B liquid of 50000D;
Steps d. with B liquid by the 10000D ultra-filtration membrane be separated into 10000～50000D C liquid and≤the D liquid of 10000D;
Step e. with D liquid by 1000D sodium filter membrane be separated into 1000～10000D E liquid and≤the F liquid of 1000D;
Step f. with F liquid by 500D sodium filter membrane be separated into 500～1000D G liquid and≤the H liquid of 500D;
Step g. C liquid is concentrated into sugar degree 45% with vacuum-evaporator heating, adds 7 times of ethanol after the cooling and stirred 0.6 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product;
Step h. is concentrated into sugar degree 40% with G liquid with vacuum-evaporator, and spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
Embodiment two, and a kind of glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, Dihuang polysaccharide, and it comprises the steps:
Step a. grinds the Radix Rehmanniae water logging after 9 hours, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
Step b. with the ground speiss add water logging 9 hours again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
Step c with filtrate by 50000D (dalton) ultra-filtration membrane be separated into 〉=the A liquid of 50000D and≤the B liquid of 50000D;
Steps d. with B liquid by the 10000D ultra-filtration membrane be separated into 10000～50000D C liquid and≤the D liquid of 10000D;
Step e. with D liquid by 1000D sodium filter membrane be separated into 1000～10000D E liquid and≤the F liquid of 1000D;
Step f. with F liquid by 500D sodium filter membrane be separated into 500～1000D G liquid and≤the H liquid of 500D;
Step g. C liquid is concentrated into sugar degree 40% with vacuum-evaporator heating, adds 8 times of ethanol after the cooling and stirred 0.8 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product;
Step h. is concentrated into sugar degree 45% with G liquid with vacuum-evaporator, and spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
Embodiment three, and a kind of glutinous rehmannia of the present invention is extracted the method for rehmannia root oligose, and it comprises the steps:
Step a. is cleaned, grinds with clear water by the Rehmannia Root of gathering in the crops in the ground or the Radix Rehmanniae water logging ground after 7 hours, gets ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
Step b. with the ground speiss add water logging 6 hours again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
Step c is separated filtrate and is obtained on the film liquid under the liquid and film by 50000D (dalton) ultra-filtration membrane;
Steps d. get under the film that above-mentioned steps c obtains liquid and separate by the 10000D ultra-filtration membrane again and obtain on the film liquid under the liquid and film;
Step e. gets under the film that above-mentioned steps d obtains liquid and separates by 1000D sodium filter membrane and obtain on the film liquid under the liquid and film;
Step f. gets under the film that above-mentioned steps e obtains liquid and separates by 500D sodium filter membrane and obtain on the film liquid under the liquid and film;
Step g. get that liquid is concentrated into sugar degree 35% with vacuum-evaporator on the film that above-mentioned steps f obtains, spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
Embodiment four, and a kind of glutinous rehmannia of the present invention is extracted the method for Dihuang polysaccharide, and it comprises the steps:
Step a. is cleaned, grinds with clear water by the Rehmannia Root of gathering in the crops in the ground or the Radix Rehmanniae water logging ground after 6 hours, gets ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
Step b. with the ground speiss add water logging 5 hours again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
Step c is separated filtrate and is obtained on the film liquid under the liquid and film by 50000D (dalton) ultra-filtration membrane;
Steps d. get under the film that above-mentioned steps c obtains liquid and separate by the 10000D ultra-filtration membrane again and obtain on the film liquid under the liquid and film;
Step e. gets that liquid is concentrated into sugar degree 30% with the vacuum-evaporator heating on the film that above-mentioned steps d obtains, and adds 5 times of ethanol after the cooling and stirs 0.9 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product.
Claims (3)
1. a glutinous rehmannia is extracted the method for rehmannia root oligose, Dihuang polysaccharide, and it is characterized in that: it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. with filtrate by the 50000D ultra-filtration membrane be separated into 〉=the A liquid of 50000D and≤the B liquid of 50000D;
D. with B liquid by the 10000D ultra-filtration membrane be separated into 10000～50000D C liquid and≤the D liquid of 10000D;
E. with D liquid by 1000D sodium filter membrane be separated into 1000～10000D E liquid and≤the F liquid of 1000D;
F. with F liquid by 500D sodium filter membrane be separated into 500～1000D G liquid and≤the H liquid of 500D;
G. C liquid is concentrated into sugar degree 10～50% with vacuum-evaporator heating, adds 1～9 times of ethanol after the cooling and stirred 0.1～1 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product;
H. G liquid is concentrated into sugar degree 10～50% with vacuum-evaporator, spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
2. a glutinous rehmannia is extracted the method for rehmannia root oligose, and it is characterized in that: it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. filtrate is separated by the 50000D ultra-filtration membrane and obtain on the film liquid under the liquid and film;
D. getting under the film that above-mentioned steps c obtains liquid separates by the 10000D ultra-filtration membrane and obtains on the film liquid under the liquid and film;
E. getting under the film that above-mentioned steps d obtains liquid separates by 1000D sodium filter membrane and obtains on the film liquid under the liquid and film;
F. getting under the film that above-mentioned steps e obtains liquid separates by 500D sodium filter membrane and obtains on the film liquid under the liquid and film;
G. get that liquid is concentrated into sugar degree 10～50% with vacuum-evaporator on the film that above-mentioned steps f obtains, spraying drying promptly gets and contains stachyose 〉=80% rehmannia root oligose finished product.
3. a glutinous rehmannia is extracted the method for Dihuang polysaccharide, and it is characterized in that: it comprises the steps:
A. the Rehmannia Root of gathering in the crops in the ground is cleaned, grinds with clear water or the Radix Rehmanniae water logging ground after 1～10 hour, get ground yellow filtrate and ground speiss with the whizzer high speed centrifugation;
B. the ground speiss is added water logging 1～10 hour again centrifugation once, waste merges secondary filtrate, removes mechanical impurity with the pressure filter press filtration;
C. filtrate is separated by the 50000D ultra-filtration membrane and obtain on the film liquid under the liquid and film;
D. getting under the film that above-mentioned steps c obtains liquid separates by the 10000D ultra-filtration membrane and obtains on the film liquid under the liquid and film;
E. get that liquid is concentrated into sugar degree 10～50% with the vacuum-evaporator heating on the film that above-mentioned steps d obtains, add 1～9 times of ethanol after the cooling and stirred 0.1～1 hour, filter and abandon liquid, filter residue dry below 100 ℃ the Dihuang polysaccharide finished product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610043391A CN100575357C (en) | 2006-03-24 | 2006-03-24 | A kind of method of from glutinous rehmannia, extracting rehmannia root oligose and Dihuang polysaccharide simultaneously |
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| CN200610043391A CN100575357C (en) | 2006-03-24 | 2006-03-24 | A kind of method of from glutinous rehmannia, extracting rehmannia root oligose and Dihuang polysaccharide simultaneously |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018819B (en) * | 2009-09-18 | 2012-01-04 | 劲牌有限公司 | Radix rehmanniae extract membrane treatment process |
| CN102028801B (en) * | 2009-09-30 | 2013-03-20 | 上海中医药大学附属曙光医院 | Radix Rehmanniae oligosaccharide pulmonary delivery traditional Chinese medicinal preparation as well as preparation method and application thereof |
| CN103319546A (en) * | 2013-06-18 | 2013-09-25 | 陕西新药技术开发中心 | Method for separating high-purity stachyose from rehmannia |
| CN104546988A (en) * | 2014-12-31 | 2015-04-29 | 贵州省科晖制药厂 | Preparation method of trichosanthes kirilowii Maxim polysaccharide immunopotentiator |
| CN106632712A (en) * | 2016-11-01 | 2017-05-10 | 福建海兴保健食品有限公司 | Process for extracting oligosaccharide by utilizing polysaccharide extracted green algae waste liquor |
| CN106820141A (en) * | 2017-01-06 | 2017-06-13 | 河南中医药大学 | A kind of adhesive rehmannia flower polysaccharide buccal tablets and preparation method thereof |
| CN113476525A (en) * | 2021-08-11 | 2021-10-08 | 江苏省中医药研究院 | Traditional Chinese medicine glucoside composition with lipid-lowering and weight-losing effects and preparation method and application thereof |
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- 2006-03-24 CN CN200610043391A patent/CN100575357C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018819B (en) * | 2009-09-18 | 2012-01-04 | 劲牌有限公司 | Radix rehmanniae extract membrane treatment process |
| CN102028801B (en) * | 2009-09-30 | 2013-03-20 | 上海中医药大学附属曙光医院 | Radix Rehmanniae oligosaccharide pulmonary delivery traditional Chinese medicinal preparation as well as preparation method and application thereof |
| CN103319546A (en) * | 2013-06-18 | 2013-09-25 | 陕西新药技术开发中心 | Method for separating high-purity stachyose from rehmannia |
| CN103319546B (en) * | 2013-06-18 | 2016-05-04 | 陕西新药技术开发中心 | A kind of from glutinous rehmannia the method for Separation of Water threose |
| CN104546988A (en) * | 2014-12-31 | 2015-04-29 | 贵州省科晖制药厂 | Preparation method of trichosanthes kirilowii Maxim polysaccharide immunopotentiator |
| CN104546988B (en) * | 2014-12-31 | 2019-03-19 | 贵州省科晖制药厂 | A kind of preparation method of Snakegourd Fruit polysaccharide immunopotentiator |
| CN106632712A (en) * | 2016-11-01 | 2017-05-10 | 福建海兴保健食品有限公司 | Process for extracting oligosaccharide by utilizing polysaccharide extracted green algae waste liquor |
| CN106820141A (en) * | 2017-01-06 | 2017-06-13 | 河南中医药大学 | A kind of adhesive rehmannia flower polysaccharide buccal tablets and preparation method thereof |
| CN113476525A (en) * | 2021-08-11 | 2021-10-08 | 江苏省中医药研究院 | Traditional Chinese medicine glucoside composition with lipid-lowering and weight-losing effects and preparation method and application thereof |
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| CN100575357C (en) | 2009-12-30 |
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