CN106398539A - Extraction method of camellia seed shell tannin extract - Google Patents
Extraction method of camellia seed shell tannin extract Download PDFInfo
- Publication number
- CN106398539A CN106398539A CN201610699672.5A CN201610699672A CN106398539A CN 106398539 A CN106398539 A CN 106398539A CN 201610699672 A CN201610699672 A CN 201610699672A CN 106398539 A CN106398539 A CN 106398539A
- Authority
- CN
- China
- Prior art keywords
- oil tea
- extract
- tea shell
- standby
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000284 extract Substances 0.000 title claims abstract description 61
- 235000018553 tannin Nutrition 0.000 title claims abstract description 37
- 229920001864 tannin Polymers 0.000 title claims abstract description 37
- 239000001648 tannin Substances 0.000 title claims abstract description 37
- 238000000605 extraction Methods 0.000 title claims abstract description 25
- 235000018597 common camellia Nutrition 0.000 title abstract description 7
- 240000001548 Camellia japonica Species 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000741 silica gel Substances 0.000 claims abstract description 25
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 25
- 238000011282 treatment Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000005352 clarification Methods 0.000 claims abstract description 4
- 241001122767 Theaceae Species 0.000 claims description 56
- 239000003921 oil Substances 0.000 claims description 47
- 239000007788 liquid Substances 0.000 claims description 31
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 11
- 235000002639 sodium chloride Nutrition 0.000 claims description 10
- 239000010779 crude oil Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000003480 eluent Substances 0.000 claims description 6
- 239000010420 shell particle Substances 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 239000003495 polar organic solvent Substances 0.000 claims description 5
- 159000000000 sodium salts Chemical class 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 229920005654 Sephadex Polymers 0.000 claims description 3
- 239000012507 Sephadex™ Substances 0.000 claims description 3
- 241000607479 Yersinia pestis Species 0.000 claims description 3
- 201000010099 disease Diseases 0.000 claims description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 2
- 229910052710 silicon Inorganic materials 0.000 claims 2
- 239000010703 silicon Substances 0.000 claims 2
- 239000003960 organic solvent Substances 0.000 claims 1
- 241000196324 Embryophyta Species 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 241000209507 Camellia Species 0.000 abstract 3
- 238000004440 column chromatography Methods 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 238000011221 initial treatment Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000010903 husk Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000011344 liquid material Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 241000526900 Camellia oleifera Species 0.000 description 1
- 244000025797 Castanea pumila Species 0.000 description 1
- 235000007763 Castanea pumila Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000238370 Sepia Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses an extraction method of camellia seed shell tannin extract and relates to the technical field of biological medicines. The method comprises the following steps: (1) preparing raw materials, (2) carrying out primary treatment, (3) carrying out ultrasonic treatment, (4) carrying out crushing, (5) carrying out extraction, (6) carrying out primary silica gel-based treatment, (7) carrying out primary concentration, (8) carrying out dissolution, (9) carrying out column chromatography, (10) carrying out secondary concentration, (11) carrying out clarification, (12) carrying out secondary silica gel-based treatment and (13) carrying out tertiary condensation. The extraction method has the characteristics of wide raw material source, low production cost and high product purity. The extraction method is suitable for extracting camellia seed shell tannin extract from camellia seed shells and can also be used to extract tannin extract from other plants.
Description
Technical field
The present invention relates to biomedicine technical field, particularly a kind of extracting method of oil tea shell tannin extract.
Background technology
Tannin extract (tannin extract) is to process system by the plant material rich in tannin through steps such as floodings and concentration
The chemical products obtaining.It is usually brown color to sepia, powdery or bulk.It is mainly used in tanning, curriery is referred to as vegetable tanning
Agent.Because the molecular weight of tannin extract is between 500-3000, complex structure, chemical property is active, has high biologically active, except being used for
Outside process hides, also serve as beneficiation inhibitor, water treating agent for boilers, drilling mud diluent and metal surface corrosion inhibitor, condensing class evergreen chinquapin
Timber work glue also made by glue.
In the world contain tannin is more, can be used for produce tannin extract plant have kind more than 600.The higher plant of Chinese amount containing tannin
There is kind more than 70.First raw material is crushed during production, so that most cells wall is ruptured, be beneficial to the diffusion of tannin and dissolving during extraction.
Leaching liquor, through vacuum evaporation and drying, obtains final product tannin extract product.
Oil tea shell is the epidermis shell that camellia oleifera fruit separates after drying, and contains abundant tannin compositions, China in oil tea shell
Adopt oil tea shell as raw material in 20 century 70s, carry out oil tea shell tannin extract and produce.
A kind of Chinese patent (number of patent application is 201510203982.9) disclosed " preparation of refined oil-tea camellia husks tannin extract
Method ", comprises the following steps:Be dried after oil-tea camellia husks natural air drying, removal of impurities, cool down, pulverize, sieve after obtain material A；Will
Material A and prepare the leaching liquor that obtains and put in the second process equipment, included countercurrent leaching, air stirring, concentration step
Dynamic extraction obtains liquid material B；Again material B, saturation copper chloride solution are put into the 3rd process equipment, stir, place
Afterwards, vacuum filtration is precipitated thing；Sediment is put in deionized water, is then passed through sulphur to containing in sedimentary deionized water
After change hydrogen no longer reduces up to sediment, vacuum filtration obtains liquid material C；Again liquid material C is concentrated, be dried, powder
Broken obtain refined oil-tea camellia husks tannin extract.
Content of the invention
It is an object of the invention to provide a kind of extraction of the tannin extract that raw material sources are wide, low production cost, product purity are high
Method.
For achieving the above object, the technical measures that the present invention is taken are to invent a kind of extracting method of oil tea shell tannin extract,
Its extraction process is as follows：
(1), get the raw materials ready：Selection is no rotted, no goes mouldy, the fresh oil tea shell of no disease and pests harm, standby；
(2), just process：Oil tea shell drying to moisture is less than 5%, reprocesses into the oil tea shell in 0.15-0.35cm for the particle diameter
Coarse granule, standby；
(3), ultrasonically treated：Oil tea shell coarse granule is put in supersonic extractors, is simultaneously introduced the ultrasonic molten of 2-4 times of weight
Agent, under the normal temperature condition for 100-200Hz for the frequency, processes 1.5-3.0h, filters, obtain ultrasonically treated oil tea shell particle；
(4), pulverize：Ultrasonically treated oil tea shell particle weight concentration is the common salt aqueous solution of 15.5-22.5% in normal temperature
Lower washing 1-3 time, transfers to shady place and dries in the shade to moisture less than 10%, the oil tea shell being then processed into 40-60 mesh is thin
Material, standby；
(5), extract：Oil tea shell fines is put in the Extraction solvent of 1-3 times of weight, soak extraction 5- at 45-60 DEG C
10h, meanwhile, stirs 5-8min in the direction of the clock every 30min, filters, and collects first time extract and extracts slag for the first time；
Extract the Extraction solvent of addition equivalent weight in slag, soak extraction 1-2.5h again to first time, meanwhile, press up time every 15min
5-8min is stirred in pin direction, filters, and collects second extract；Again by first time extract and second extract mixing, obtain
Total extract, standby；
(6) a, silica gel treatment：First add, in total extract, the salt accounting for crude oil tea shell fines weight 1.5-5%, stir
Even, place 2-4h at normal temperatures；Add in total extract again and account in crude oil tea shell fines weight 10-20%, 100-200 purpose
Property silica gel, stir process 30-45min at normal temperatures, filter, obtain a silica gel treatment liquid, standby；
(7), once concentration：Silica gel treatment liquid is concentrated into original volume at pressure 5-10KPa, temperature 45-60 DEG C
15-25%, obtains once concentration liquid, standby；
(8), dissolve：The once concentration liquid warm water of 2-4 times of weight, temperature 45-60 DEG C is dissolved, filters, collect clarification
Water-soluble liquid, standby；
(9), cross post：Water-soluble liquid is crossed at 40-50 DEG C sephadex column, flow velocity is 15-20L/h；Then use quality
Fraction is that the sodium-salt aqueous solution of 5-15% elutes at 30-38 DEG C, and flow velocity is 10-18L/h, collects eluent, standby；
(10), secondary concentration：Eluent is concentrated at pressure 5-10KPa, temperature 45-60 DEG C the 20-30% of original volume,
Obtain secondary concentration liquid；
(11), clarify：Add polar organic solvent in secondary concentration liquid, so that the volumetric concentration of polar organic solvent is reached
More than 70%, then quiet put 10-20h, filter, obtain settled solution, standby；
(12), secondary silica gel treatment：Add in settled solution account for crude oil tea shell fines weight 5-8%, more than 300 mesh in
Property silica gel, stir process 10-25min at 30-38 DEG C, filter, obtain secondary silica gel treatment liquid, standby；
(13), concentrate：Will be concentrated for secondary silica gel treatment liquid, dry, obtain final product oil tea shell tannin extract.
Described step (3) in ultrasonic solvent be ethyl acetate or petroleum ether or by water：Ethyl acetate：Petroleum ether
Press (0.1-0.3):0.2:(1.5-4) part by weight mixes.
Described step (5) in Extraction solvent be ethyl acetate or by ethyl acetate：Water presses (6-10):(0.2-
0.35) part by weight mixes.
Described step (9) in sodium salt be sodium chloride or sodium acetate or by sodium chloride：Sodium acetate presses 1:(0.3-
0.5) part by weight mixes.
Described step (11) in polar organic solvent be one or more of methyl alcohol, ethanol, acetone, when for two kinds or three
Kind when, the ratio of each component is wait weight portion or other ratio.
The extracting method of the oil tea shell tannin extract of the present invention, is as raw material using discarded oil tea shell, thus, its raw material comes
Source is wide.Meanwhile, devise in addition ultrasonically treated, solvent extraction, concentrate for three times, secondary silica gel treatment and cross the operations such as post so that
Extract more thorough, more efficient, product goes out rate and purity is higher, and production cost is relatively low.
Table 1 below is the effective ingredient detection data of the oil tea shell tannin extract that the application method of the present invention is extracted：
Table 1 (content of 100g)
| Composition | Content (g) |
| Tannin extract | 96.25 |
| Tea polysaccharide | 1.12 |
| Tea Saponin | 0.54 |
| Moisture | 1.65 |
Can be seen that the oil tea shell tannin extract that the application method of the present invention is extracted from upper table data, content is high, quality better,
It is suitable for the application in each field.
Specific embodiment
With reference to embodiments, the present invention is further illustrated.Description below is in the way of enumerating, but this
Bright protection domain is not limited thereto.
The extracting method of the oil tea shell tannin extract of the present embodiment, its extraction process is as follows：
(1), get the raw materials ready：Selection is no rotted, no goes mouldy, the fresh oil tea shell of no disease and pests harm, standby；
(2), just process：Oil tea shell drying to moisture is less than 5%, reprocesses into thick of the oil tea shell in 0.25cm for the particle diameter
Grain, standby；
(3), ultrasonically treated：Oil tea shell coarse granule is put in supersonic extractors, is simultaneously introduced 3 times of weight, by water：Acetic acid
Ethyl ester：Petroleum ether presses 0.2:0.2:The ultrasonic solvent that 2.5 part by weight mixes, in the normal temperature condition for 150Hz for the frequency
Under, process 2.5h, filter, obtain ultrasonically treated oil tea shell particle；
(4), pulverize：The common salt aqueous solution that ultrasonically treated oil tea shell particle weight concentration is 18% is washed 2 at normal temperatures
Secondary, transfer to shady place and dry in the shade to moisture less than 10%, be then processed into the oil tea shell fines of 50 mesh, standby；
(5), extract：By oil tea shell fines 2 times of weight of input, by ethyl acetate：Water presses 8:0.3 part by weight mixing and
In the Extraction solvent becoming, soak extraction 8h at 55 DEG C, meanwhile, stirs 6min in the direction of the clock every 30min, filters, receive
Collection first time extract and for the first time extraction slag；Extract the Extraction solvent of addition equivalent weight in slag again to first time, immersion carries
Take 2h, meanwhile, stir 7min in the direction of the clock every 15min, filter, collect second extract；Again first time is extracted
Liquid and second extract mixing, obtain total extract, standby；
(6) a, silica gel treatment：First add, in total extract, the salt accounting for crude oil tea shell fines weight 3.5%, stir evenly,
Place 3h at normal temperatures；Add in total extract again and account for crude oil tea shell fines weight 15%, the neutral silica gel of 150 mesh, normal
Lower stir process 40min of temperature, filters, obtains a silica gel treatment liquid, standby；
(7), once concentration：Silica gel treatment liquid is concentrated into the 20% of original volume at pressure 8KPa, 55 DEG C of temperature,
Obtain once concentration liquid, standby；
(8), dissolve：The once concentration liquid warm water of 3 times of weight, 55 DEG C of temperature is dissolved, filters, collect the water-soluble of clarification
Solution liquid, standby；
(9), cross post：Water-soluble liquid is crossed at 45 DEG C sephadex column (G-150), flow velocity is 18L/h；Then use matter
Amount fraction be 10%, by sodium chloride：Sodium acetate presses 1:The sodium-salt aqueous solution that 0.4 part by weight mixes is washed at 35 DEG C
De-, flow velocity is 15L/h, collects eluent, standby；
(10), secondary concentration：Eluent is concentrated into the 25% of original volume at pressure 8KPa, 55 DEG C of temperature, obtains secondary dense
Contracting liquid；
(11), clarify：Add methyl alcohol in secondary concentration liquid, make the volumetric concentration of methyl alcohol reach more than 70%, then quiet put
10-20h, filters, obtains settled solution, standby；
(12), secondary silica gel treatment：Add in settled solution and account for crude oil tea shell fines weight 6%, neutrality more than 300 mesh
Silica gel, stir process 20min at 35 DEG C, filter, obtain secondary silica gel treatment liquid, standby；
(13), concentrate：Will be concentrated for secondary silica gel treatment liquid, dry, obtain final product oil tea shell tannin extract.
The extracting method of the oil tea shell tannin extract of the present invention, is suitable for extracting oil tea shell tannin extract with oil tea shell it can also be used to use
Other plant extract tannin extracts.
Claims (5)
1. a kind of extracting method of oil tea shell tannin extract is it is characterised in that extraction process is as follows：
(1), get the raw materials ready：Selection is no rotted, no goes mouldy, the fresh oil tea shell of no disease and pests harm, standby；
(2), just process：Oil tea shell drying to moisture is less than 5%, reprocesses into thick of the oil tea shell in 0.15-0.35cm for the particle diameter
Grain, standby；
(3), ultrasonically treated：Oil tea shell coarse granule is put in supersonic extractors, is simultaneously introduced the ultrasonic solvent of 2-4 times of weight,
Frequency is under the normal temperature condition of 100-200Hz, processes 1.5-3.0h, filters, obtains ultrasonically treated oil tea shell particle；
(4), pulverize：The common salt aqueous solution that ultrasonically treated oil tea shell particle weight concentration is 15.5-22.5% is washed at normal temperatures
Wash 1-3 time, transfer to shady place and dry in the shade to moisture less than 10%, be then processed into the oil tea shell fines of 40-60 mesh, standby
With；
(5), extract：Oil tea shell fines is put in the Extraction solvent of 1-3 times of weight, soak extraction 5-10h at 45-60 DEG C, with
When, stir 5-8min in the direction of the clock every 30min, filter, collect first time extract and extract slag for the first time；Again to
Once extract slag in add equivalent weight Extraction solvent, soak extraction 1-2.5h, meanwhile, every 15min in the direction of the clock
Stirring 5-8min, filters, and collects second extract；Again by first time extract and second extract mixing, obtain and always extract
Liquid, standby；
(6) a, silica gel treatment：First add, in total extract, the salt accounting for crude oil tea shell fines weight 1.5-5%, stir evenly,
2-4h is placed under normal temperature；The neutral silicon accounting for crude oil tea shell fines weight 10-20%, 100-200 mesh is added again in total extract
Glue, stir process 30-45min at normal temperatures, filter, obtain a silica gel treatment liquid, standby；
(7), once concentration：Silica gel treatment liquid is concentrated at pressure 5-10KPa, temperature 45-60 DEG C the 15- of original volume
25%, obtain once concentration liquid, standby；
(8), dissolve：The once concentration liquid warm water of 2-4 times of weight, temperature 45-60 DEG C is dissolved, filters, collect the water-soluble of clarification
Solution liquid, standby；
(9), cross post：Water-soluble liquid is crossed at 40-50 DEG C sephadex column, flow velocity is 15-20L/h；Then use mass fraction
Sodium-salt aqueous solution for 5-15% elutes at 30-38 DEG C, and flow velocity is 10-18L/h, collects eluent, standby；
(10), secondary concentration：Eluent is concentrated at pressure 5-10KPa, temperature 45-60 DEG C the 20-30% of original volume, obtains two
Secondary concentrate；
(11), clarify：To in secondary concentration liquid add polar organic solvent, make the volumetric concentration of polar organic solvent reach 70% with
On, then quiet put 10-20h, filter, obtain settled solution, standby；
(12), secondary silica gel treatment：Add in settled solution and account for crude oil tea shell fines weight 5-8%, neutral silicon more than 300 mesh
Glue, stir process 10-25min at 30-38 DEG C, filter, obtain secondary silica gel treatment liquid, standby；
(13), three concentrations：Will be concentrated for secondary silica gel treatment liquid, dry, obtain final product oil tea shell tannin extract.
2. according to claim 1 oil tea shell tannin extract extracting method it is characterised in that：Described step (3) in ultrasonic solvent
It is by water：Ethyl acetate：Petroleum ether presses (0.1-0.3):0.2:(1.5-4) part by weight mixes.
3. according to claim 1 oil tea shell tannin extract extracting method it is characterised in that：Described step (5) in Extraction solvent
It is by ethyl acetate：Water presses (6-10):(0.2-0.35) part by weight mixes.
4. according to claim 1 oil tea shell tannin extract extracting method it is characterised in that：Described step (9) in sodium salt be by
Sodium chloride：Sodium acetate presses 1:(0.3-0.5) part by weight mixes.
5. according to claim 1 oil tea shell tannin extract extracting method it is characterised in that：Described step (11) in polarity organic
Solvent is one or more of methyl alcohol, ethanol, acetone, when for two or three, the ratio of each component is etc. weight portion or
Other ratios.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610699672.5A CN106398539A (en) | 2016-08-19 | 2016-08-19 | Extraction method of camellia seed shell tannin extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610699672.5A CN106398539A (en) | 2016-08-19 | 2016-08-19 | Extraction method of camellia seed shell tannin extract |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106398539A true CN106398539A (en) | 2017-02-15 |
Family
ID=58005154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610699672.5A Pending CN106398539A (en) | 2016-08-19 | 2016-08-19 | Extraction method of camellia seed shell tannin extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106398539A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029415A (en) * | 2020-08-28 | 2020-12-04 | 广西灵水林化有限公司 | Method for extracting acacia melanoxylon tannin extract by ultrasonic-assisted biological enzyme method |
-
2016
- 2016-08-19 CN CN201610699672.5A patent/CN106398539A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 戴甜甜: "油茶蒲鞣质提取及其降血糖活性研究", 《中国优秀硕士学位论文 医药卫生科技辑》 * |
| 戴甜甜等: "油茶果壳鞣质提取工艺及降血糖功能研究", 《食品工业科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029415A (en) * | 2020-08-28 | 2020-12-04 | 广西灵水林化有限公司 | Method for extracting acacia melanoxylon tannin extract by ultrasonic-assisted biological enzyme method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103463123B (en) | Method for extracting effective constituents from maca | |
| CN105193863B (en) | A kind of preparation method of high-purity seeweed polyphenol | |
| CN101463027B (en) | Method for extracting and separating flavone and anthocyanidin from elder fruit | |
| CN110201012B (en) | Preparation method and application of purslane extract | |
| CN104311676B (en) | A kind of extraction food starch method of by-product tannic acid from rubber seed core | |
| CN102432582A (en) | Preparation method of proanthocyanidin | |
| CN106349133A (en) | Extraction method of sulforaphane | |
| CN108997471A (en) | A kind of environment-friendly preparation method thereof of high-purity tea saponin | |
| CN104876824A (en) | Technology for separation and purification of chlorogenic acid from coffee beans | |
| CN101856427B (en) | Method for extracting solanine from potato peels | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN107857792A (en) | A kind of extracting method of gleditschiasaponin | |
| CN106832051A (en) | A kind of preparation method of Chinese fiber crops pectin and the new Chinese fiber crops jelly powder prepared according to the method | |
| CN108948124A (en) | A kind of preparation method of Tea Saponin | |
| WO2019080571A1 (en) | Method for extracting toosendanin | |
| CN106398539A (en) | Extraction method of camellia seed shell tannin extract | |
| CN107793492A (en) | A kind of extracting method of fructus cannabis polysaccharide | |
| CN108546589A (en) | A kind of preparation method of the tea oil rich in tea polyphenols | |
| CN105154485A (en) | Method for extracting compound amino acid from polygonatum odoratum through enzymolysis and ultrasonic treatment | |
| CN115569158A (en) | Method for extracting total flavonoids from guava leaves by using ultrasonic-assisted eutectic solvent extraction technology | |
| CN100415697C (en) | Agent of extracting polyphenol from rape seed cakes or husks and its preparation | |
| CN107488413A (en) | The extracting method of tannin extract in a kind of granatum | |
| CN105193880A (en) | Extraction method for actinidia arguta flavones | |
| CN109467580B (en) | Extraction process of naringin | |
| CN102952002A (en) | Method for refining magnolol through supersonic extraction separating technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170215 |
|
| RJ01 | Rejection of invention patent application after publication |