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CN104744554B - A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake - Google Patents

A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake Download PDF

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CN104744554B
CN104744554B CN201510139637.3A CN201510139637A CN104744554B CN 104744554 B CN104744554 B CN 104744554B CN 201510139637 A CN201510139637 A CN 201510139637A CN 104744554 B CN104744554 B CN 104744554B
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tea
polysaccharide
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saponin
polyphenols
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CN104744554A (en
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王庆彬
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ANHUI ZHONGSHENG EDIBLE OIL TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J63/00Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
    • C07J63/008Expansion of ring D by one atom, e.g. D homo steroids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G99/00Subject matter not provided for in other groups of this subclass
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof

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  • Health & Medical Sciences (AREA)
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  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

The present invention relates to a kind of coproduction tea polyphenols from Extracted From Oil-tea-cake, the method of tea polysaccharide and tea saponin, tea-seed pancake after drying and crushing is carried out the lixiviate on basis, slagging-off, after microfiltration, utilize tea polyphenols, the difference of the molecular size of tea polysaccharide and tea saponin, ultra-filtration and separation is carried out by different molecular retention amounts, final prepared tea polyphenols, tea polysaccharide and tea saponin, realize Extracted From Oil-tea-cake coproduction and obtain tea polysaccharide, tea polysaccharide and tea saponin, the purity of product and yield are all not less than at present per unit area yield product on the market simultaneously, the production cost making product declines and realizes the abundant exploitation of oil tea resource, technical solutions according to the invention do not have use the material that environment has pollution, decrease the pollution to environment of the existing production method, there is good development prospect.

Description

A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake
Technical field
The present invention relates to food processing field, relate in particular to a kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake.
Background technology
Extracted From Oil-tea-cake is resultant product after Semen Camelliae oil expression, containing about crude protein 15%, saccharide 40%, Saponin 10%-15% and organic 74.4% etc. in Extracted From Oil-tea-cake, and the many kinds of substances such as the tea saponin wherein contained, Camellia Oleifera polysaccharide, tea polyphenols can be used as the important component of multiple industries such as food, fertilizer, pesticide, feedstuff, chemical industry.Tea saponin is mainly used in wettable powder as wetting agent, the auxiliary agent of water soluble pesticide, botanical pesticide and the field such as antibacterial, plant growth regulator on pesticide industry, have nontoxic, can automatically degrade, to the feature such as pesticide synergistic is obvious.It it is the extremely promising environmental protection type agricultural chemical auxiliary agent of one.Tea polysaccharide has the effects such as blood sugar lowering, blood fat reducing, enhancing immunity, blood pressure lowering, decreased heart rate, increase coronary flow, anticoagulation, antithrombotic and anoxia enduring, is health care of food additive.Tea polyphenols has anti-oxidation efficacy, it is possible to extend the food storage phase, it is prevented that food fades, and improves cellulose stability, and effectively the protection various nutrition of food, is excellent food additive.Its discovered in recent years tea polysaccharide and tea polyphenols have on feed industry improve animal physiological function, improve immunity, improve produce growth performance, improve price of deed rate, reduce feeding cost, all many-sided functions of improving meat quality etc., for high-quality feed additive.
nullMany employing single production tea saponins of Extracted From Oil-tea-cake in current commercial production、Tea polysaccharide or tea polyphenols product,Report has employing Batteries by Organic Solvent Partition Process to realize tea saponin and the tea polysaccharide coproduction (patent No.: 200710042332 with resin partition method recently、The patent No. 201210401720、The patent No. 2010102591313 etc.)、Resin partition method realizes tea saponin and tea polyphenols coproduction (Lu Wenjing," the comprehensive extraction of tea saponin and tea polyphenols in Flos Camelliae sinensis、Separate purification and biocidal property research ",Agricultural University Of Anhui's Master's thesis,2012)、The production technology of Subcritical Water Extraction tea polysaccharide and tea polyphenols coproduction (patent No.: 201210263633.2),But there is presently no tea saponin、Tea polysaccharide、The technique report of tea polyphenols coproduction,And existing technology has the pollution problem to environment more.
Summary of the invention
The technical problem to be solved is to provide a kind of method that can obtain tea polyphenols, tea polysaccharide and tea saponin step by step from Extracted From Oil-tea-cake, it is achieved the abundant exploitation of Extracted From Oil-tea-cake resource.
In order to solve above-mentioned technical problem, the present invention provides a kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is dried pulverizing, by solid-to-liquid ratio 1:15 25(g/ml) join lixiviate 20 30min in 80 DEG C of 90 DEG C of water, filter, then carry out secondary lixiviate, merge the filtrate obtained for twice, obtain filtrate 1;
(2) remove impurity: add chitosan in filtrate 1, stirring, the protein-based impurity in filtrate 1 is formed precipitation and is filtered to remove, reserved filtrate, obtain filtrate 2;
(3) microfiltration: filtrate 2 is carried out microfiltration, removes solid impurity, reserved filtrate further, obtain filtrate 3;
(4) ultrafiltration: filtrate 3 adopts different molecular retention films carry out substep ultrafiltration, respectively obtains tea saponin effluent, tea polyphenols solution effluent, tea polysaccharide effluent.
(5) purification is with dry: by 3 5:1 cocnentration factors, tea polysaccharide effluent, tea polyphenols effluent, tea saponin effluent are carried out vacuum concentration respectively, obtains tea polysaccharide concentrated solution, tea polyphenols concentrated solution and tea saponin concentrated solution;
Tea polysaccharide concentrated solution adds the ethanol that mass percent concentration is 80% 100%, stirring according to the volume ratio of 1:1 2, settles tea polysaccharide 3-12h, filter, acquisition tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, and tea polysaccharide and glycoprotein total content reach 52% 64%;
By tea polyphenols concentrated solution convection drying, the tea polyphenols product that purity is 72% 85% can be obtained;
By tea saponin concentrated solution convection drying, the tea saponin product that purity is 75% 84% can be obtained.
Tea-seed pancake after drying and crushing is carried out the lixiviate on basis by the present invention, slagging-off, after microfiltration, utilize tea polyphenols, the difference of the molecular size of tea polysaccharide and tea saponin, ultra-filtration and separation is carried out by different molecular retention amounts, final prepared tea polyphenols, tea polysaccharide and tea saponin, realize Extracted From Oil-tea-cake coproduction and obtain tea polysaccharide, tea polysaccharide and tea saponin, the purity of product and yield are all not less than at present per unit area yield product on the market simultaneously, the production cost making product declines and realizes the abundant exploitation of oil tea resource, technical solutions according to the invention do not have use the material that environment has pollution, decrease the pollution to environment of the existing production method, there is good development prospect.
Preferred as the present invention, described ultrafiltration adopts poly (ether-sulfone) ultrafiltration membrane, be respectively adopted 10KDa, filtrate 3 is carried out substep ultrafiltration by 20 30KDa, 40 50Kda molecular retention amount films, when temperature 25 30 DEG C, pressure 0.3 0.4MPa, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 10KDa obtains tea saponin effluent after carrying out ultrafiltration, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 20 30KDa obtains tea polyphenols effluent after carrying out ultrafiltration, and the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 40 50KDa obtains tea polysaccharide effluent after carrying out ultrafiltration.
Described tea-seed pancake is pulverized and is reached 40 60 orders.Tea-seed pancake is crushed to 40 60 orders can so that the operations such as lixiviate below, filtration obtain better effect.
So that the better effects if of microfiltration separation tea polysaccharide, tea polysaccharide and tea saponin, described microfiltration adopts 0.1 μm of ceramic micro filter device, microfiltration pressure 0.1 0.2MPa.
The addition of described chitosan for add 1.5 2.0mg chitosans in every milliliter of filtrate 1.Protein-based impurity in filtrate 1 can be removed well.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is dried pulverizing, pulverizing order number is 40 orders, pulverize the add water ratio of 15ml of dried tea-seed pancake in every gram to be joined by dried for pulverizings tea-seed pancake 90 DEG C of water process 30min, filter, carry out secondary lixiviate again, merge the filtrate obtained for twice, obtain filtrate 1;
(2) remove impurity: add chitosan in filtrate 1, stirring, the protein-based impurity in filtrate 1 is formed precipitation and is filtered to remove, reserved filtrate, obtain filtrate 2;
The addition of chitosan is that every milliliter of filtrate 1 adds 1.5mg chitosan;
(3) microfiltration: filtrate 2 adopts 0.1 μm of ceramic micro filter device carry out microfiltration, microfiltration pressure 0.1MPa, removes solid impurity, reserved filtrate further, obtain filtrate 3;
(4) ultrafiltration: be respectively adopted 10KDa, filtrate 3 is carried out substep ultrafiltration by 20 30KDa, 40 50Kda molecular retention amount films, when temperature 25 DEG C, pressure 0.3MPa, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 10KDa obtains tea saponin effluent after carrying out ultrafiltration, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 20 30KDa obtains tea polyphenols effluent after carrying out ultrafiltration, and the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 40 50KDa obtains tea polysaccharide effluent after carrying out ultrafiltration.
(5) purification is with dry: by 3:1 cocnentration factor, tea polysaccharide effluent, tea polyphenols effluent, tea saponin effluent are carried out vacuum concentration respectively, obtains tea polysaccharide concentrated solution, tea polyphenols concentrated solution and tea saponin concentrated solution;
Tea polysaccharide concentrated solution adds according to the tea polysaccharide concentrated solution of every 1 volume 2 volumes 80% ethanol, stirring, sedimentation tea polysaccharide 12h, filter, acquisition tea polysaccharide precipitates, can obtaining tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content (containing protein in the molecular structure of part sugar, the tea polysaccharide therefore obtained is actually the mixture of polysaccharide and glycoprotein) reach 52% 64%;
By tea polyphenols concentrated solution convection drying, the tea polyphenols product that purity is 72% 85% can be obtained;
By tea saponin concentrated solution convection drying, the tea saponin product that purity is 75% 84% can be obtained.
Embodiment 2
A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is dried pulverizing, pulverizing order number is 60 orders, by solid-to-liquid ratio 1:25(g/ml) join process 20min in 80 DEG C of water, filter, 2 lixiviates, merge the filtrate obtained for 2 times, obtain filtrate 1;
(2) remove impurity: add chitosan in filtrate 1, stirring, the protein-based impurity in filtrate 1 is formed precipitation and is filtered to remove, reserved filtrate, obtain filtrate 2;
The addition of chitosan is that every milliliter of filtrate 1 adds 2.0mg chitosan;
(3) microfiltration: filtrate 2 carries out microfiltration, adopts 0.1 μm of ceramic micro filter device, microfiltration pressure 0.2MPa, removes solid impurity, reserved filtrate further, obtain filtrate 3;
(4) ultrafiltration: be respectively adopted 10KDa, filtrate 3 is carried out substep ultrafiltration by 20 30KDa, 40 50Kda molecular retention amount films, when temperature 30 DEG C, pressure 0.4MPa, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 10KDa obtains tea saponin effluent after carrying out ultrafiltration, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 20 30KDa obtains tea polyphenols effluent after carrying out ultrafiltration, and the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 40 50KDa obtains tea polysaccharide effluent after carrying out ultrafiltration.
(5) purification is with dry: by 5:1 cocnentration factor, tea polysaccharide effluent, tea polyphenols effluent, tea saponin effluent are carried out vacuum concentration respectively, obtains tea polysaccharide concentrated solution, tea polyphenols concentrated solution and tea saponin concentrated solution;
According to addition 99.9% ethanol of the volume ratio of 1:1 in tea polysaccharide concentrated solution, stirring, settle tea polysaccharide 3h, filter, it is thus achieved that tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52% 64%;
By tea polyphenols concentrated solution convection drying, the tea polyphenols product that purity is 72% 85% can be obtained;
By tea saponin concentrated solution convection drying, the tea saponin product that purity is 75% 84% can be obtained.
Embodiment 3
A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is dried pulverizing, pulverizing order number is 50 orders, by solid-to-liquid ratio 1:20(g/ml) join process 25min in 85 DEG C of water, filter, 2 lixiviates, merge the filtrate obtained for 2 times, obtain filtrate 1;
(2) remove impurity: add chitosan in filtrate 1, stirring, the protein-based impurity in filtrate 1 is formed precipitation and is filtered to remove, reserved filtrate, obtain filtrate 2;
The addition of chitosan is that every milliliter of filtrate 1 adds 2.0mg chitosan;
(3) microfiltration: filtrate 2 carries out microfiltration, adopts 0.1 μm of ceramic micro filter device, microfiltration pressure 0.15MPa, removes solid impurity, reserved filtrate further, obtain filtrate 3;
(4) ultrafiltration: be respectively adopted 10KDa, filtrate 3 is carried out substep ultrafiltration by 20 30KDa, 40 50Kda molecular retention amount films, when temperature 28 DEG C, pressure 0.35MPa, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 10KDa obtains tea saponin effluent after carrying out ultrafiltration, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 20 30KDa obtains tea polyphenols effluent after carrying out ultrafiltration, and the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 40 50KDa obtains tea polysaccharide effluent after carrying out ultrafiltration.
(5) purification is with dry: by 4:1 cocnentration factor, tea polysaccharide effluent, tea polyphenols effluent, tea saponin effluent are carried out vacuum concentration respectively, obtains tea polysaccharide concentrated solution, tea polyphenols concentrated solution and tea saponin concentrated solution;
According to addition 90% ethanol of the volume ratio of 1:1.5 in tea polysaccharide concentrated solution, stirring, settle tea polysaccharide 8h, filter, it is thus achieved that tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52% 64%;
By tea polyphenols concentrated solution convection drying, the tea polyphenols product that purity is 72% 85% can be obtained;
By tea saponin concentrated solution convection drying, the tea saponin product that purity is 75% 84% can be obtained.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention.

Claims (4)

1. a method for coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is dried pulverizing, joins lixiviate 20 30min in 80 DEG C of 90 DEG C of water by solid-to-liquid ratio 1:15 25g/ml, filters, then carries out secondary lixiviate, merges the filtrate obtained for twice, obtain filtrate 1;
(2) remove impurity: add chitosan in filtrate 1, stirring, the protein-based impurity in filtrate 1 is formed precipitation and is filtered to remove, reserved filtrate, obtain filtrate 2;
(3) microfiltration: filtrate 2 is carried out microfiltration, removes solid impurity, reserved filtrate further, obtain filtrate 3;
(4) ultrafiltration: filtrate 3 adopts different molecular retention films carry out substep ultrafiltration, respectively obtains tea saponin effluent, tea polyphenols solution effluent, tea polysaccharide effluent;
Described ultrafiltration adopts poly (ether-sulfone) ultrafiltration membrane, be respectively adopted 10kDa, filtrate 3 is carried out substep ultrafiltration by 20 30kDa, 40 50kDa molecular retention amount films, when temperature 25 30 DEG C, pressure 0.3 0.4MPa, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 10kDa obtains tea saponin effluent after carrying out ultrafiltration, the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 20 30kDa obtains tea polyphenols effluent after carrying out ultrafiltration, and the poly (ether-sulfone) ultrafiltration membrane adopting molecular retention amount to be 40 50kDa obtains tea polysaccharide effluent after carrying out ultrafiltration;
(5) purification is with dry: by 3 5:1 cocnentration factors, tea polysaccharide effluent, tea polyphenols effluent, tea saponin effluent are carried out vacuum concentration respectively, obtains tea polysaccharide concentrated solution, tea polyphenols concentrated solution and tea saponin concentrated solution;
Tea polysaccharide concentrated solution adds the ethanol that mass percent concentration is 80% 100%, stirring according to the volume ratio of 1:1 2, settles tea polysaccharide 3-12h, filter, acquisition tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, and tea polysaccharide and glycoprotein total content reach 52% 64%;
By tea polyphenols concentrated solution convection drying, the tea polyphenols product that purity is 72% 85% can be obtained;
By tea saponin concentrated solution convection drying, the tea saponin product that purity is 75% 84% can be obtained.
2. a kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, it is characterised in that: described tea-seed pancake is pulverized and is reached 40 60 orders.
3. a kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, it is characterised in that: described microfiltration adopts 0.1 μm of ceramic micro filter device, microfiltration pressure 0.1 0.2MPa.
4. a kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, it is characterised in that: the addition of described chitosan is that every milliliter of filtrate 1 adds 1.5 2.0mg chitosans.
CN201510139637.3A 2015-03-29 2015-03-29 A kind of method of coproduction tea polyphenols, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake Active CN104744554B (en)

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CN105461778A (en) * 2015-10-29 2016-04-06 广东星汇生物科技有限公司 Method for extracting tea saponin from sasangua cake
CN106565813B (en) * 2016-09-26 2018-06-19 中国林业科学研究院亚热带林业研究所 The processing method that a kind of Tea Saponin continuously purifies
CN108003253B (en) * 2017-12-11 2019-05-03 盛蓓蓓 The effect that a kind of Extracted From Oil-tea-cake polysaccharide, preparation method and antagonism aftosa vaccine damage bull semen
CN108383891B (en) * 2018-03-03 2020-10-20 广西师范大学 Method for extracting saponin and co-producing kaempferol from camellia oleifera abel cake
CN110483591B (en) * 2019-08-28 2022-02-15 中国科学院青岛生物能源与过程研究所 Method for refining tea saponin by combined membrane method
CN115448992B (en) * 2022-10-10 2024-07-16 江西省科学院应用化学研究所 Oil tea fruit chitin extraction method and application thereof

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CN101863950A (en) * 2010-06-07 2010-10-20 邓培红 Method for extracting tea saponin from oil tea cakes
CN102993329A (en) * 2012-12-31 2013-03-27 广西师范大学 Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes
CN103012544A (en) * 2012-12-31 2013-04-03 广西师范大学 Method for extracting saponin and polysaccharide from tea-seed pancake

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CN101863950A (en) * 2010-06-07 2010-10-20 邓培红 Method for extracting tea saponin from oil tea cakes
CN102993329A (en) * 2012-12-31 2013-03-27 广西师范大学 Method for comprehensively extracting saponin, polysaccharides and polyphenol from camellia oleifera abel defatted cakes
CN103012544A (en) * 2012-12-31 2013-04-03 广西师范大学 Method for extracting saponin and polysaccharide from tea-seed pancake

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Inventor after: Yuan Huaibo

Inventor after: Wang Qingbin

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Denomination of invention: Method for cooperatively producing tea polyphenol, tea polysaccharide and tea saponin from oil-tea meal

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Pledgee: Anhui Mount Holyoke rural commercial bank Limited by Share Ltd

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Pledgor: ANHUI ZHONGSHENG EDIBLE OIL TECHNOLOGY Co.,Ltd.

Registration number: 2019340000215