CN104744554A - Method for cooperatively producing tea polyphenol, tea polysaccharide and tea saponin from oil-tea meal - Google Patents
Method for cooperatively producing tea polyphenol, tea polysaccharide and tea saponin from oil-tea meal Download PDFInfo
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- C07—ORGANIC CHEMISTRY
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- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
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Abstract
The invention relates to a method for cooperatively producing tea polyphenol, tea polysaccharide and tea saponin from an oil-tea meal. The method comprises the following steps: basically extracting, deslagging and performing microfiltration on the dried and smashed oil tea seed cake; and according to different molecular sizes of the tea polyphenol, tea polysaccharide and tea saponin, performing ultrafiltration and separation through different molar weight cut-offs to obtain the tea polyphenol, the tea polysaccharide and the tea saponin. The tea polyphenol, the tea polysaccharide and the tea saponin are obtained through the oil-tea meal co-production; the purity and yield of the product are not lower than those of the single-yield product, the production cost of the product is reduced and the sufficient development and utilization of the oil tea resource is realized. The environment pollution substance is not existed in the technical scheme provided by the invention, the environment pollution caused by the existing production method is reduced and the method has good developing prospect.
Description
Technical field
The present invention relates to food processing field, relate in particular to a kind of method of coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake.
Background technology
Extracted From Oil-tea-cake is resultant product after tea seed oil expression, about containing crude protein 15%, carbohydrate 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, tea seed polysaccharide, tea-polyphenol can be used as the important component of multiple industries such as food, fertilizer, agricultural chemicals, feed, chemical industry.Tea saponin is mainly used in wettable powder as the auxiliary agent of wetting agent, water soluble pesticide, botanical pesticide and the field such as sterilant, plant-growth regulator on pesticide industry, have nontoxic, can automatically degrade, to the feature such as pesticide synergistic is obvious.It is the extremely promising environmental protection type agricultural chemical auxiliary agent of one.Tea polysaccharide has hypoglycemic, reducing blood-fat, strengthening immunity, hypotensive, the effect such as reducing heart rate, increase coronary flow, anticoagulation, antithrombotic and hypoxia tolerance, is health care of food additive.Tea-polyphenol has anti-oxidation efficacy, can extend the food storage phase, prevents food from fading, and improve Mierocrystalline cellulose stability, the various nutrition of available protecting food is excellent foodstuff additive.Its discovered in recent years tea polysaccharide and tea-polyphenol have and improve animal physiological function, improve immunizing power, improve and produce growth performance, improve price of deed rate, reduce feeding cost, improve all many-sided functions such as meat quality on fodder industry, are high-quality feed additive.
The single production tea saponin of many employing Extracted From Oil-tea-cakes in current industrial production, tea polysaccharide or tea-polyphenol product, nearest report has employing Batteries by Organic Solvent Partition Process and resin isolation method to realize tea saponin and the tea polysaccharide coproduction (patent No.: 200710042332, the patent No. 201210401720, the patent No. 2010102591313 etc.), resin isolation method realizes tea saponin and tea-polyphenol coproduction (Lu Wenjing, " the comprehensive extraction of tea saponin and tea-polyphenol in Tea Flower, separation and purification and biocidal property research ", Agricultural University Of Anhui's Master's thesis, 2012), Subcritical Water Extraction tea polysaccharide and the tea-polyphenol coproduction (patent No.: production technique 201210263633.2), but also there is no tea saponin at present, tea polysaccharide, the technique report of tea-polyphenol coproduction, and the pollution problem had in existing technology environment more.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that can obtain tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake step by step, realizes the abundant exploitation of Extracted From Oil-tea-cake resource.
In order to solve the problems of the technologies described above, the invention provides a kind of method of coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprising the following steps:
(1) lixiviate: tea-seed pancake is carried out drying and crushing, 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) removal of impurities: add chitosan in filtrate 1, stirs, and the protein-based impurity in filtrate 1 is formed sedimentation and filtration removing, and reserved filtrate, obtains filtrate 2;
(3) micro-filtration: filtrate 2 is carried out micro-filtration, removes solid impurity further, reserved filtrate, obtain filtrate 3;
(4) ultrafiltration: adopt different molecular retention films to carry out substep ultrafiltration to filtrate 3, obtains tea saponin effluent liquid, tea-polyphenol solution stream fluid, tea polysaccharide effluent liquid respectively.
(5) purifying is with dry: tea polysaccharide effluent liquid, tea-polyphenol effluent liquid, tea saponin effluent liquid are carried out vacuum concentration by 3-5:1 concentration ratio respectively, obtains tea polysaccharide concentrated solution, tea-polyphenol concentrated solution and tea saponin concentrated solution;
Add according to the volume ratio of 1:1-2 in tea polysaccharide concentrated solution the ethanol that mass percent concentration is 80%-100%, stir, sedimentation tea polysaccharide 3-12h, filter, acquisition tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52%-64%;
By tea-polyphenol concentrated solution convection drying, the tea-polyphenol 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 micro-filtration, utilize tea-polyphenol, 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 obtained tea-polyphenol, tea polysaccharide and tea saponin, realize Extracted From Oil-tea-cake coproduction and obtain tea polysaccharide, tea polysaccharide and tea saponin, simultaneously the purity of product is all not less than current per unit area yield product on the market with yield, the production cost of product is declined and realizes the abundant exploitation of oil tea resource, do not have in technical solutions according to the invention to use material environment being had to pollution, decrease the pollution of existing production method to environment, there is good development prospect.
As preferably of the present invention, described ultrafiltration adopts poly (ether-sulfone) ultrafiltration membrane, adopt 10KDa, 20-30KDa respectively, 40-50Kda molecular retention amount film carries out substep ultrafiltration to filtrate 3, under temperature 25-30 DEG C, pressure 0.3-0.4MPa condition, employing molecular retention amount is obtain tea saponin effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 10KDa carries out ultrafiltration, employing molecular retention amount is obtain tea-polyphenol effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 20-30KDa carries out ultrafiltration, and employing molecular retention amount is obtain tea polysaccharide effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 40-50KDa carries out ultrafiltration.
Described tea-seed pancake is pulverized and is reached 40-60 orders.Tea-seed pancake being crushed to 40-60 orders can make the operations such as lixiviate below, filtration obtain better effect.
In order to the better effects if making micro-filtration be separated tea polysaccharide, tea polysaccharide and tea saponin, described micro-filtration adopts 0.1 μm of ceramic micro filter device, micro-filtration pressure 0.1-0.2MPa.
The add-on of described chitosan for add 1.5-2.0mg chitosan in every milliliter of filtrate 1.Protein-based impurity in filtrate 1 can be removed well.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
A method for coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is carried out drying and crushing, pulverizing order number is 40 orders, pulverize the add water ratio of 15ml of dried tea-seed pancake in every gram dried for pulverizing tea-seed pancake joined in 90 DEG C of water to process 30min, filter, carry out secondary lixiviate again, merge the filtrate obtained for twice, obtain filtrate 1;
(2) removal of impurities: add chitosan in filtrate 1, stirs, and the protein-based impurity in filtrate 1 is formed sedimentation and filtration removing, and reserved filtrate, obtains filtrate 2;
The add-on of chitosan is that every milliliter of filtrate 1 adds 1.5mg chitosan;
(3) micro-filtration: filtrate 2 adopted 0.1 μm of ceramic micro filter device to carry out micro-filtration, micro-filtration pressure 0.1MPa, removes solid impurity, reserved filtrate further, obtains filtrate 3;
(4) ultrafiltration: adopt 10KDa, 20-30KDa respectively, 40-50Kda molecular retention amount film carries out substep ultrafiltration to filtrate 3, under temperature 25 DEG C, pressure 0.3MPa condition, employing molecular retention amount is obtain tea saponin effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 10KDa carries out ultrafiltration, employing molecular retention amount is obtain tea-polyphenol effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 20-30KDa carries out ultrafiltration, and employing molecular retention amount is obtain tea polysaccharide effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 40-50KDa carries out ultrafiltration.
(5) purifying is with dry: tea polysaccharide effluent liquid, tea-polyphenol effluent liquid, tea saponin effluent liquid are carried out vacuum concentration by 3:1 concentration ratio respectively, obtains tea polysaccharide concentrated solution, tea-polyphenol concentrated solution and tea saponin concentrated solution;
Add the ethanol of 80% of 2 volumes according to the tea polysaccharide concentrated solution of every 1 volume in tea polysaccharide concentrated solution, stir, sedimentation tea polysaccharide 12h, filter, acquisition tea polysaccharide precipitates, can obtain 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-polyphenol concentrated solution convection drying, the tea-polyphenol 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 method for coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is carried out drying and crushing, pulverizing order number is 60 orders, by solid-to-liquid ratio 1:25(g/ml) join in 80 DEG C of water and process 20min, filter, 2 lixiviates, merge the filtrate obtained for 2 times, obtain filtrate 1;
(2) removal of impurities: add chitosan in filtrate 1, stirs, and the protein-based impurity in filtrate 1 is formed sedimentation and filtration removing, and reserved filtrate, obtains filtrate 2;
The add-on of chitosan is that every milliliter of filtrate 1 adds 2.0mg chitosan;
(3) micro-filtration: filtrate 2 is carried out micro-filtration, adopt 0.1 μm of ceramic micro filter device, micro-filtration pressure 0.2MPa, removes solid impurity, reserved filtrate further, obtains filtrate 3;
(4) ultrafiltration: adopt 10KDa, 20-30KDa respectively, 40-50Kda molecular retention amount film carries out substep ultrafiltration to filtrate 3, under temperature 30 DEG C, pressure 0.4MPa condition, employing molecular retention amount is obtain tea saponin effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 10KDa carries out ultrafiltration, employing molecular retention amount is obtain tea-polyphenol effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 20-30KDa carries out ultrafiltration, and employing molecular retention amount is obtain tea polysaccharide effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 40-50KDa carries out ultrafiltration.
(5) purifying is with dry: tea polysaccharide effluent liquid, tea-polyphenol effluent liquid, tea saponin effluent liquid are carried out vacuum concentration by 5:1 concentration ratio respectively, obtains tea polysaccharide concentrated solution, tea-polyphenol concentrated solution and tea saponin concentrated solution;
Add 99.9% ethanol according to the volume ratio of 1:1 in tea polysaccharide concentrated solution, stir, sedimentation tea polysaccharide 3h, filter, obtain tea polysaccharide precipitation, can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52%-64%;
By tea-polyphenol concentrated solution convection drying, the tea-polyphenol 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 method for coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is carried out drying and crushing, pulverizing order number is 50 orders, by solid-to-liquid ratio 1:20(g/ml) join in 85 DEG C of water and process 25min, filter, 2 lixiviates, merge the filtrate obtained for 2 times, obtain filtrate 1;
(2) removal of impurities: add chitosan in filtrate 1, stirs, and the protein-based impurity in filtrate 1 is formed sedimentation and filtration removing, and reserved filtrate, obtains filtrate 2;
The add-on of chitosan is that every milliliter of filtrate 1 adds 2.0mg chitosan;
(3) micro-filtration: filtrate 2 is carried out micro-filtration, adopt 0.1 μm of ceramic micro filter device, micro-filtration pressure 0.15MPa, removes solid impurity, reserved filtrate further, obtains filtrate 3;
(4) ultrafiltration: adopt 10KDa, 20-30KDa respectively, 40-50Kda molecular retention amount film carries out substep ultrafiltration to filtrate 3, under temperature 28 DEG C, pressure 0.35MPa condition, employing molecular retention amount is obtain tea saponin effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 10KDa carries out ultrafiltration, employing molecular retention amount is obtain tea-polyphenol effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 20-30KDa carries out ultrafiltration, and employing molecular retention amount is obtain tea polysaccharide effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 40-50KDa carries out ultrafiltration.
(5) purifying is with dry: tea polysaccharide effluent liquid, tea-polyphenol effluent liquid, tea saponin effluent liquid are carried out vacuum concentration by 4:1 concentration ratio respectively, obtains tea polysaccharide concentrated solution, tea-polyphenol concentrated solution and tea saponin concentrated solution;
Add 90% ethanol according to the volume ratio of 1:1.5 in tea polysaccharide concentrated solution, stir, sedimentation tea polysaccharide 8h, filter, obtain tea polysaccharide precipitation, can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52%-64%;
By tea-polyphenol concentrated solution convection drying, the tea-polyphenol 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 preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the method for coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake, comprises the following steps:
(1) lixiviate: tea-seed pancake is carried out drying and crushing, 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) removal of impurities: add chitosan in filtrate 1, stirs, and the protein-based impurity in filtrate 1 is formed sedimentation and filtration removing, and reserved filtrate, obtains filtrate 2;
(3) micro-filtration: filtrate 2 is carried out micro-filtration, removes solid impurity further, reserved filtrate, obtain filtrate 3;
(4) ultrafiltration: adopt different molecular retention films to carry out substep ultrafiltration to filtrate 3, obtains tea saponin effluent liquid, tea-polyphenol solution stream fluid, tea polysaccharide effluent liquid respectively;
(5) purifying is with dry: tea polysaccharide effluent liquid, tea-polyphenol effluent liquid, tea saponin effluent liquid are carried out vacuum concentration by 3-5:1 concentration ratio respectively, obtains tea polysaccharide concentrated solution, tea-polyphenol concentrated solution and tea saponin concentrated solution;
Add according to the volume ratio of 1:1-2 in tea polysaccharide concentrated solution the ethanol that mass percent concentration is 80%-100%, stir, sedimentation tea polysaccharide 3-12h, filter, acquisition tea polysaccharide precipitates, and can obtain tea polysaccharide product after drying, tea polysaccharide and glycoprotein total content reach 52%-64%;
By tea-polyphenol concentrated solution convection drying, the tea-polyphenol 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. one according to claim 1 coproduction tea-polyphenol from Extracted From Oil-tea-cake, the method of tea polysaccharide and tea saponin, it is characterized in that: described ultrafiltration adopts poly (ether-sulfone) ultrafiltration membrane, adopt 10KDa respectively, 20-30KDa, 40-50Kda molecular retention amount film carries out substep ultrafiltration to filtrate 3, temperature 25-30 DEG C, under pressure 0.3-0.4MPa condition, employing molecular retention amount is obtain tea saponin effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 10KDa carries out ultrafiltration, employing molecular retention amount is obtain tea-polyphenol effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 20-30KDa carries out ultrafiltration, employing molecular retention amount is obtain tea polysaccharide effluent liquid after the poly (ether-sulfone) ultrafiltration membrane of 40-50KDa carries out ultrafiltration.
3. the method for a kind of coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, is characterized in that: described tea-seed pancake is pulverized and reached 40-60 orders.
4. the method for a kind of coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, is characterized in that: described micro-filtration adopts 0.1 μm of ceramic micro filter device, micro-filtration pressure 0.1-0.2MPa.
5. the method for a kind of coproduction tea-polyphenol, tea polysaccharide and tea saponin from Extracted From Oil-tea-cake according to claim 1, is characterized in that: the add-on of described chitosan is that every milliliter of filtrate 1 adds 1.5-2.0mg chitosan.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106565813A (en) * | 2016-09-26 | 2017-04-19 | 中国林业科学研究院亚热带林业研究所 | Processing method for continuously purifying tea saponin |
| CN108003253A (en) * | 2017-12-11 | 2018-05-08 | 盛蓓蓓 | The effect that a kind of Extracted From Oil-tea-cake polysaccharide, preparation method and antagonism aftosa vaccine damage bull semen |
| CN108383891A (en) * | 2018-03-03 | 2018-08-10 | 广西师范大学 | A method of from the withered middle extraction saponin co-production Kaempferol of oil tea |
| CN110483591A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A method of combination embrane method refined theasapogenin |
| CN115448992A (en) * | 2022-10-10 | 2022-12-09 | 江西省科学院应用化学研究所 | Extraction method and application of camellia oleifera shell polysaccharide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106565813A (en) * | 2016-09-26 | 2017-04-19 | 中国林业科学研究院亚热带林业研究所 | Processing method for continuously purifying tea saponin |
| 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 |
| CN108003253A (en) * | 2017-12-11 | 2018-05-08 | 盛蓓蓓 | The effect that a kind of Extracted From Oil-tea-cake polysaccharide, preparation method and antagonism aftosa vaccine damage bull semen |
| 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 |
| CN108383891A (en) * | 2018-03-03 | 2018-08-10 | 广西师范大学 | A method of from the withered middle extraction saponin co-production Kaempferol of oil tea |
| 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 |
| CN110483591A (en) * | 2019-08-28 | 2019-11-22 | 中国科学院青岛生物能源与过程研究所 | A method of combination embrane method refined theasapogenin |
| 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 |
| CN115448992A (en) * | 2022-10-10 | 2022-12-09 | 江西省科学院应用化学研究所 | Extraction method and application of camellia oleifera shell polysaccharide |
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Denomination of invention: Method for cooperatively producing tea polyphenol, tea polysaccharide and tea saponin from oil-tea meal Effective date of registration: 20190426 Granted publication date: 20160706 Pledgee: Anhui Mount Holyoke rural commercial bank Limited by Share Ltd Pledgor: ANHUI ZHONGSHENG EDIBLE OIL TECHNOLOGY CO., LTD. Registration number: 2019340000215 |
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