CN102180935A - Method for preparing high-purity sasanquasaponins - Google Patents
Method for preparing high-purity sasanquasaponins Download PDFInfo
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- 150000007949 saponins Chemical class 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 241001122767 Theaceae Species 0.000 claims description 52
- 239000003921 oil Substances 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 27
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- 238000001694 spray drying Methods 0.000 claims description 11
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- 230000002411 adverse Effects 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- HWKQNAWCHQMZHK-UHFFFAOYSA-N Trolnitrate Chemical compound [O-][N+](=O)OCCN(CCO[N+]([O-])=O)CCO[N+]([O-])=O HWKQNAWCHQMZHK-UHFFFAOYSA-N 0.000 claims description 4
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- 238000003795 desorption Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 4
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- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000007738 vacuum evaporation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N Silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229920001525 carrageenan Polymers 0.000 claims description 2
- 235000010418 carrageenan Nutrition 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N n-butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 239000010451 perlite Substances 0.000 claims description 2
- 235000019362 perlite Nutrition 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 125000003011 styrenyl group Chemical class [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 235000012222 talc Nutrition 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 238000000108 ultra-filtration Methods 0.000 claims description 2
- 241000209094 Oryza Species 0.000 claims 3
- 235000017709 saponins Nutrition 0.000 abstract description 27
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 235000013305 food Nutrition 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000007639 printing Methods 0.000 abstract description 3
- 235000012970 cakes Nutrition 0.000 abstract 1
- 238000004134 energy conservation Methods 0.000 abstract 1
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- 150000004804 polysaccharides Polymers 0.000 description 12
- 240000007594 Oryza sativa Species 0.000 description 11
- VXMKYRQZQXVKGB-CWWHNZPOSA-N Tannin Chemical compound O([C@H]1[C@H]([C@@H]2OC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)O[C@H]([C@H]2O)O1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 VXMKYRQZQXVKGB-CWWHNZPOSA-N 0.000 description 11
- 239000000049 pigment Substances 0.000 description 11
- 229920001864 tannin Polymers 0.000 description 11
- 235000018553 tannin Nutrition 0.000 description 11
- 239000001648 tannin Substances 0.000 description 11
- 229920002521 Macromolecule Polymers 0.000 description 9
- 239000002893 slag Substances 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 7
- 150000002016 disaccharides Chemical class 0.000 description 7
- 150000002402 hexoses Chemical class 0.000 description 7
- 235000014666 liquid concentrate Nutrition 0.000 description 7
- 150000001720 carbohydrates Chemical class 0.000 description 6
- 235000014633 carbohydrates Nutrition 0.000 description 6
- 235000008504 concentrate Nutrition 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 235000018102 proteins Nutrition 0.000 description 6
- 102000004169 proteins and genes Human genes 0.000 description 6
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- 229920002472 Starch Polymers 0.000 description 5
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- 238000003809 water extraction Methods 0.000 description 5
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- 239000011780 sodium chloride Substances 0.000 description 3
- 239000010495 camellia oil Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
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- 240000007049 Juglans regia Species 0.000 description 1
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- 244000057114 Sapium sebiferum Species 0.000 description 1
- 235000005128 Sapium sebiferum Nutrition 0.000 description 1
- BWPGKXYWPBQBPV-MWQJAWBESA-N Theasaponin Chemical compound O([C@H]1[C@H](O)[C@H](O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@@H](O)CO1)O[C@H]1[C@@H]([C@@H](O)[C@H](O)CO1)O)O[C@H]1CC[C@]2(C)[C@H]3CC=C4[C@@]([C@@]3(CC[C@H]2[C@@]1(CO)C)C)(C)C[C@@H](O)[C@@]1(CO)[C@@H](OC(C)=O)[C@@H](C(C[C@H]14)(C)C)OC(=O)C(\C)=C/C)C(O)=O)[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O BWPGKXYWPBQBPV-MWQJAWBESA-N 0.000 description 1
- BWPGKXYWPBQBPV-ZOADXXHESA-N Theasaponin Natural products O=C(O[C@@H]1[C@@H](OC(=O)C)[C@]2(CO)[C@@H](O)C[C@@]3(C)[C@@]4(C)[C@@H]([C@]5(C)[C@H]([C@@](CO)(C)[C@@H](O[C@@H]6[C@@H](O[C@@H]7[C@H](O[C@@H]8[C@@H](O)[C@H](O)[C@H](O)CO8)[C@H](O)[C@@H](O)CO7)[C@@H](O[C@H]7[C@H](O)[C@@H](O)[C@@H](O)[C@H](CO)O7)[C@H](O)[C@@H](C(=O)O)O6)CC5)CC4)CC=C3[C@@H]2CC1(C)C)/C(=C/C)/C BWPGKXYWPBQBPV-ZOADXXHESA-N 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
- 230000005712 crystallization Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
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Abstract
The invention discloses a method for preparing high-purity sasanquasaponins. The method comprises the following steps of: performing ultrasonic counter-current extraction of the sasanqua cakes serving as a raw material or dissolving raw sasanqua saponins serving as a raw material in a solvent, and performing filtration, ionic exchange, macro-porous adsorption, concentration and the like to obtain the high-purity white powdery sasanquasaponins of which the purity is over 95 percent. The high-purity sasanquasaponins can be applied to the high-end fields of foods, pharmacy, electronics, printing and the like. The method has the advantages of meeting national requirements of energy conservation, emission reduction and pollution-free production, realizing mass production, solving the problems of high cost, high energy consumption, difficulty in removing impurities and decolorizing and the like in an industrial sasanquasaponin-purifying method, along with low solvent consumption, low energy consumption and high extraction rate.
Description
Technical field
The present invention relates to field of fine chemical, specifically is a kind of preparation method of high purity sasanguasaponin.
Background technology
Oil tea (Camellia oleifera Abel), belong to Theaceae (Theaceae) Camellia (CamelliaL.) plant, be evergreen dungarunga or shrub, be the distinctive woody edible oil materials seeds of China, the cultivation in more than 2000 year is arranged and utilize historical, with Fructus oleae europaeae, oil palm, coconut and be called the world four big woody oleiferous plants plants, with Chinese tallow tree, tung oil tree and walnut and be called China four big woody oleiferous plants plants.At present, China's oil tea area has 4,500 ten thousand mu approximately, about 1,000,000 tons of tea seed annual production, produce about 260,000 tons of tea oil per year, about 11,000,000,000 yuan of the output value, mainly be distributed in the Yangtze valley and on the south 14 provinces (city, district), wherein Jiangxi, Hunan, Guangxi San Sheng (district) account for 76.2% of national total area.Tea seed utilizes degree near 100%, 14 the oil tea main products in the whole nation are economized (district, city) 659 families of existing oil tea processing enterprise, tea seed Design and Machining ability can reach 424.83 ten thousand tons, year can be processed 110.79 ten thousand tons of tea oil, working ability has 178 families in the enterprise more than 500 tons, enterprise with affinability reaches family more than 200, and oil tea processing took on a certain scale already, possessed certain basis.Oil tea byproduct comprehensive development and utilization technology is further ripe, can produce 68.39 ten thousand tons of the tea dregs of rice at present per year, can produce 70,000 tons of tea saponins.Sasanguasaponin claims theasaponin, tea saponin again, is the natural glycoside compound of a class that contains in the Theaceae oil tea fruit, and it is by seven kinds of aglucons (C30H5006), four kinds of glycosides and two kinds of a kind of pentacyclic triterpenoid saponins that organic carboxylic is formed.Tea saponin can extensively be used in fields such as food, pharmacy, daily-use chemical industry makeup, system are dyed, papermaking, printing, man-made fiber, weaving, plant pesticide.China at present can only the thick tea saponin of suitability for industrialized production, and saponin content is low, and the foreign matter content height only can only use in low-end market, and inapplicable modern science and technology is to this product volume requirement.Oil tea saponin extracts many methods, as extraction process, crystallization process, absorption method, polyamide column chromatography method, ion-exchange-resin process, flocculation agent method, ultrafiltrationmembrane process or the like, but also there are many problems in the suitability for industrialized production tea saponin: generally adopt water-containing solvents such as methyl alcohol or ethanol to extract, because organic solvent costs an arm and a leg, the production cost height, it is big that water extraction concentrates energy consumption; Membrane sepn filter membrane hole easily stop up, regenerate difficulty, production cost height.Oil tea saponin is easier to dissolving in water than in pure equal solvent, in industrial production to adopt water extraction for well, 1., how to remove impurity such as carbohydrate in the vat liquor, protein, starch, tannin, pigment effectively but also there is following subject matter in the present production of water extraction research:, in the time of water extraction leaching tea saponin, the impurity of a lot of solubilities such as carbohydrate, protein, tannin, pigment etc. also are dissolved in the water, enter filtrate with tea saponin during filtration, slag liquid separates very difficulty.2., how efficiently concentrate vat liquor, reduce production costs, with containing a large amount of moisture in the vat liquor behind the water extraction, it is big to concentrate energy consumption, time-consuming length.
Summary of the invention
Purpose of the present invention just provides and a kind ofly prepares the method for high purity sasanguasaponin from thick oil tea saponin, solves problems such as industrialization purification sasanguasaponin cost height, energy consumption are big, decon decolouring difficulty.
The present invention's technical scheme of being taked of dealing with problems is: preparing the method for high purity sasanguasaponin, can be raw material with the oil tea dregs of rice, can be raw material with thick oil tea saponin also.
When being raw material, may further comprise the steps with the oil tea dregs of rice:
1., the ultrasonic wave countercurrent extraction oil tea dregs of rice
The oil tea dregs of rice are joined in the ultrasonic wave counterflow extraction apparatus, add solvent and carry out the adverse current supersound extraction, the oil tea dregs of rice and solvent ratios are 1: 5 (weight ratio), and extraction time is 15-60 minute;
2., filter
Add 1-8ppm finings and 1-8ppm flocculating aids and clarify and filter, again with filter membrane coarse filtration, smart filter;
3., ion-exchange
Smart filtrate after the filtration is decoloured with basic anion exchange resin;
4., macroporous absorption
Adsorb with the macroporous absorption post;
5., concentrate
Organic solvent desorption liquid that contains through macroporous absorption post absorption concentrates through vacuum-evaporator, and the vacuum-evaporation thickening temperature is less than 50 ℃, drying machine with centrifugal spray drying again, through HPLC detect the Powdered sasanguasaponin of the above high purity white of content>95%.
With thick oil tea saponin is raw material, and thick oil tea saponin is that a kind of glycoside compound can be that liquid also can be powder, and its content is 50-60%.It may further comprise the steps:
1., with the thick oil tea saponin of dissolution with solvents
With thick oil tea saponin solvent, stir in the mixed precipitation jar in feed liquid 1: 20-40 (weight ratio) ratio adding belt stirrer, dissolution time normal temperature 7-10 hour, when heating for dissolving is temperature 40-50 ℃, 30-60 minute heat-up time;
2., filter
Add 1-8ppm finings and 1-8ppm flocculating aids and clarify and filter, again with filter membrane coarse filtration, smart filter;
3., ion-exchange
Smart filtrate after the filtration is decoloured with basic anion exchange resin;
4., macroporous absorption
Adsorb with the macroporous absorption post;
5., concentrate
Organic solvent desorption liquid that contains through macroporous absorption post absorption concentrates through vacuum-evaporator, and the vacuum-evaporation thickening temperature is less than 50 ℃, drying machine with centrifugal spray drying again, must through HPLC detect the Powdered sasanguasaponin of the above high purity white of content>95%.
Described solvent can be methyl alcohol, ethanol, propyl carbinol, propylene glycol, pure water.
Described finings can be higher derivative, ZTC 1+1 natural clarifying agent, carrageenin, bentonite (Bentonite), the polyvinylpolypyrrolidone (PVPP) of silicon dioxide gel (Silica sol), chitosan.
Described flocculating aids can be diatomite, silica powder, perlite, talcum powder
Described filtering membrane can be ceramic super-filtering film, organic membrane ultra-filtration membrane.
It is alkaline acrylic acid type anion exchange resin, macroreticular weakly base styrene series anion exchange resin that resin is adopted in described ion-exchange.
It is nonpolar macroporous adsorption resin basic anion exchange resin, macroporous adsorbent resin that described macroporous absorption adopts resin.
In the present invention: (1), employing ultrasonic continuous are extracted oil tea saponin in the oil tea dregs of rice; (2), adopt finings and flocculating aids macromolecular substance such as precipitate and separate carbohydrate, protein, starch, tannin, pigment for the first time; (3) adopt ceramic membrane coarse filtration, the smart small-molecule substances such as macromolecular substance such as separating carbohydrate, protein, starch, tannin, pigment for the second time and inorganic salt of filtering; (4) with the weakly basic exchange resin decolouring, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time; (5) stripping liquid concentrates in<50 ℃ of vacuum concentrators, and centrifugal spray drying gets the high purity sasanguasaponin.
The present invention's organic solvent, the thick oil tea saponin of water-containing organic solvent or water dissolution, adopt the carbohydrate in heavy clear agent and the thick oil tea saponin of the flocculating aids precipitate and separate first time, protein, starch, tannin, materials such as pigment, through the ceramic membrane coarse filtration, smart filter separates carbohydrate for the second time, protein, starch, tannin, small-molecule substances such as macromolecular substance such as pigment and inorganic salt, decolour with base exchange resin, macroporous adsorbent resin separates five-carbon sugar for the third time, hexose, monose, disaccharides, the polysaccharide glucide, stripping liquid concentrates through<50 ℃ of vacuum concentrators, and centrifugal spray drying gets>95% high purity sasanguasaponin.The present invention adopts several different methods in conjunction with small-molecule substances such as separating for several times macromolecular substance and inorganic salt; make glycoside compound obtain separating; easy obstruction and the easily saturated pressure of membrane sepn, absorption with macroporous adsorbent resin purifying have also been alleviated; obtain 95% high purity sasanguasaponin, the high purity sasanguasaponin can enter high-end fields such as food, pharmacy, electronics, printing, and this law solvent consumption is few; energy consumption is low; the extraction yield height meets national energy-saving and emission-reduction cleaner production requirement, and can carry out large-scale production.
Embodiment
The oil tea dregs of rice are joined in the ultrasonic wave counterflow extraction apparatus, adding organic solvent by the other end also can be that pure water carries out the adverse current supersound extraction, ultrasonic frequency is that 30-60KHz, ultrasonic time are 15-60 minute, ultrasonic power 12-76KW, extracting 20-60 ℃ of temperature, controlling solid-liquid ratio with liquid meter and input speed controller is 1: 5, extracting solution separates slag liquid, extracting solution feeding liquid treatment system through the slag liquid/gas separator; Adding the natural clarifying agent precipitation in setting tank goes part to remove macromolecular substance such as albumen, tannin, polysaccharide, add flocculating aids, leaching extracting solution after treatment, slough pigment with weakly basic exchange resin, must contain the oil tea saponin through two effect vacuum-evaporator evaporation recovery organic solvents and not have alcohol extract, be made into 5% aqueous solution with pure water, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time, stripping liquid concentrates in thickener, and centrifugal spray drying gets>95% high purity sasanguasaponin.
Specify below in conjunction with embodiment.
Embodiment 1
The 40-60 order oil tea dregs of rice are joined in the ultrasonic wave counterflow extraction apparatus for 1000 kilograms gradually, add 5000 kilogram of 80% (volumetric concentration) ethanol gradually by the other end and carry out the adverse current supersound extraction, ultrasonic frequency is that 30-60KHz, ultrasonic time are 15-60 minute, ultrasonic power 12-76KW, extracting 20-60 ℃ of temperature, controlling solid-liquid ratio with liquid meter and input speed controller is 1: 5, and extracting solution separates slag liquid through the slag liquid/gas separator; Extracting solution adds 60 kilograms of 5ppmZTC 1+1 natural clarifying agent precipitations and goes part to remove macromolecular substance such as albumen, tannin, polysaccharide in setting tank, add 60 kilograms of super-cells, again with filter membrane coarse filtration, smart filter; The leaching extracting solution, slough pigment with weakly basic exchange resin, must contain the oil tea saponin through two effect vacuum-evaporator evaporation recovery organic solvents and not have alcohol extract, be made into 5% aqueous solution with pure water, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time, and stripping liquid concentrates in thickener, and thickening temperature is 40-50 ℃, centrifugal spray drying gets 85.3 kilograms>95% high purity sasanguasaponin, and high purity sasanguasaponin extraction yield is 94.5%.
Embodiment 2
The 40-60 order oil tea dregs of rice 1000 are joined in the ultrasonic wave counterflow extraction apparatus gradually, add 5000 kilogram of 80% (volumetric concentration) methyl alcohol gradually by the other end and carry out the adverse current supersound extraction, ultrasonic frequency is that 30-60KHz, ultrasonic time are 15-60 minute, ultrasonic power 12-76KW, extracting 20-60 ℃ of temperature, controlling solid-liquid ratio with liquid meter and input speed controller is 1: 5, and extracting solution separates slag liquid through the slag liquid/gas separator; Extracting solution adds 60 kilograms of 5ppm ZTC 1+1 natural clarifying agent precipitations and goes part to remove macromolecular substance such as albumen, tannin, polysaccharide in setting tank, add 60 kilograms of super-cells, again with filter membrane coarse filtration, smart filter; Leaching extracting solution after treatment, slough pigment with weakly basic exchange resin, must contain the oil tea saponin through two effect vacuum-evaporator evaporation recovery organic solvents and not have alcohol extract, be made into 5% aqueous solution with pure water, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time, stripping liquid concentrates in thickener, and centrifugal spray drying gets 89.7 kilograms>95% high purity sasanguasaponin, and high purity sasanguasaponin extraction yield is 94.03%.
Embodiment 3
The 40-60 order oil tea dregs of rice 1000 are joined in the ultrasonic wave counterflow extraction apparatus gradually, add 5000 kilograms of pure water gradually by the other end and carry out the adverse current supersound extraction, ultrasonic frequency is that 30-60KHz, ultrasonic time are 15-60 minute, ultrasonic power 12-76KW, extracting 20-60 ℃ of temperature, controlling solid-liquid ratio with liquid meter and input speed controller is 1: 5, and extracting solution separates slag liquid through the slag liquid/gas separator; Extracting solution adds ZTC 1+1 natural clarifying agent precipitation and goes part to remove macromolecular substance such as albumen, tannin, polysaccharide in setting tank, add flocculating aids, again with filter membrane coarse filtration, smart filter; Leaching extracting solution after treatment, slough pigment with weakly basic exchange resin, imitate the vacuum-evaporator evaporation through two, add pure water and be made into 5% aqueous solution, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time, stripping liquid concentrates in thickener, and centrifugal spray drying gets 80.8 kilograms>91.1% high purity sasanguasaponin, and high purity sasanguasaponin extraction yield is 93.92%.
Embodiment 4
(oil tea saponin content is 50-60% to get 100 kilograms of thick oil tea saponins, weight ratio), 2000 kilogram of 80% (volume ratio) ethanol, with liquid meter and input speed controller control solid-liquid ratio is 1: 20, temperature 40-50 ℃, heating for dissolving is 1 hour in band stirring setting tank, adds 60 kilograms of 5ppmZTC 1+1 natural clarifying agents precipitations and go part to remove macromolecular substance such as albumen, tannin, polysaccharide in setting tank, add 60 kilograms of super-cells, again with filter membrane coarse filtration, smart filter; The leaching extracting solution, slough pigment with weakly basic exchange resin, must contain the oil tea saponin through two effect vacuum-evaporator evaporation recovery organic solvents and not have alcohol extract, be made into 5% aqueous solution with pure water, macroporous adsorbent resin separates glucides such as five-carbon sugar, hexose, monose, disaccharides, polysaccharide for the third time, stripping liquid concentrates in thickener, and thickening temperature is 40-50 ℃, and centrifugal spray drying gets 65 kilograms>95% high purity sasanguasaponin.
Claims (8)
1. a method for preparing the high purity sasanguasaponin is a raw material with the oil tea dregs of rice, and it may further comprise the steps:
1., ultrasonic wave countercurrent extraction
The oil tea dregs of rice are joined in the ultrasonic wave counterflow extraction apparatus, add solvent and carry out the adverse current supersound extraction, the oil tea dregs of rice and solvent ratios are 1: 5 (weight ratio), and extraction time is 15-60 minute;
2., filter
Add 1-8ppm finings and 1-8ppm flocculating aids and clarify and filter, again with filter membrane coarse filtration, smart filter;
3., ion-exchange
Smart filtrate after the filtration is decoloured with basic anion exchange resin;
4., macroporous absorption
Adsorb with the macroporous absorption post;
5., concentrate
Organic solvent desorption liquid that contains through macroporous absorption post absorption concentrates through vacuum-evaporator, and the vacuum-evaporation thickening temperature is less than 50 ℃, drying machine with centrifugal spray drying again, through HPLC detect content greater than the Powdered sasanguasaponin of 95% above high purity white.
2. a method for preparing the high purity sasanguasaponin is a raw material with thick oil tea saponin, and it may further comprise the steps:
1., with the thick oil tea saponin of dissolution with solvents
With thick oil tea saponin dissolution with solvents, stir in the mixed precipitation jar in feed liquid 1: 20-40 (weight ratio) ratio adding belt stirrer, dissolution time normal temperature 7-10 hour, when heating for dissolving is temperature 40-50 ℃, 30-60 minute heat-up time;
2., filter
Add 1-8ppm finings and 1-8ppm flocculating aids and clarify and filter, again with filter membrane coarse filtration, smart filter;
3., ion-exchange
Smart filtrate after the filtration is decoloured with basic anion exchange resin;
4., macroporous absorption
Adsorb with the macroporous absorption post;
5., concentrate
Organic solvent desorption liquid that contains through macroporous absorption post absorption concentrates through vacuum-evaporator, and the vacuum-evaporation thickening temperature is less than 50 ℃, drying machine with centrifugal spray drying again, through HPLC detect content greater than the Powdered sasanguasaponin of 95% above high purity white.
3. a kind of method for preparing the high purity sasanguasaponin according to claim 1 and 2 is characterized in that described solvent can be methyl alcohol, ethanol, propyl carbinol, propylene glycol, pure water.
4. a kind of method for preparing the high purity sasanguasaponin according to claim 1 and 2 is characterized in that described finings can be higher derivative, ZTC 1+1 natural clarifying agent, carrageenin, bentonite (Bentonite), the polyvinylpolypyrrolidone (PVPP) of silicon dioxide gel (Silica sol), chitosan.
5. a kind of method for preparing the high purity sasanguasaponin according to claim 1 and 2 is characterized in that described flocculating aids can be diatomite, silica powder, perlite, talcum powder
6. a kind of method for preparing the high purity sasanguasaponin according to claim 1 and 2 is characterized in that described filtering membrane can be ceramic super-filtering film, organic membrane, ultra-filtration membrane.
7. a kind of preparation high purity sasanguasaponin method according to claim 1 and 2 is characterized in that it is alkaline acrylic acid type anion exchange resin, macroreticular weakly base styrene series anion exchange resin that resin is adopted in described ion-exchange.
8. a kind of preparation high purity sasanguasaponin method according to claim 1 and 2 is characterized in that it is nonpolar macroporous adsorption resin basic anion exchange resin, macroporous adsorbent resin that described macroporous absorption adopts resin.
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CN102372761A (en) * | 2011-10-10 | 2012-03-14 | 安徽农业大学 | Method for extracting tea saponin from sasanglla cake |
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CN111994921A (en) * | 2020-08-04 | 2020-11-27 | 宁夏锦华化工有限公司 | Monocyanamide decoloring method |
CN112315838A (en) * | 2020-11-12 | 2021-02-05 | 东莞波顿香料有限公司 | Plant extract solution and preparation method and application thereof |
WO2022268235A1 (en) * | 2021-06-23 | 2022-12-29 | 广东菁萃生物科技有限公司 | Saponin composition having high stability and use thereof |
CN113801172A (en) * | 2021-09-14 | 2021-12-17 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
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