CN109929002A - Preparation method of salidroside - Google Patents
Preparation method of salidroside Download PDFInfo
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- CN109929002A CN109929002A CN201910168702.3A CN201910168702A CN109929002A CN 109929002 A CN109929002 A CN 109929002A CN 201910168702 A CN201910168702 A CN 201910168702A CN 109929002 A CN109929002 A CN 109929002A
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- rhodioside
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- salidroside
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- ILRCGYURZSFMEG-UHFFFAOYSA-N Salidroside Natural products OC1C(O)C(O)C(CO)OC1OCCC1=CC=C(O)C=C1 ILRCGYURZSFMEG-UHFFFAOYSA-N 0.000 title abstract 7
- ILRCGYURZSFMEG-RQICVUQASA-N salidroside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)OC1OCCC1=CC=C(O)C=C1 ILRCGYURZSFMEG-RQICVUQASA-N 0.000 title abstract 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 41
- 238000000605 extraction Methods 0.000 claims abstract description 26
- 108090000790 Enzymes Proteins 0.000 claims abstract description 14
- 102000004190 Enzymes Human genes 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000000287 crude extract Substances 0.000 claims abstract description 8
- 239000007853 buffer solution Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 238000001694 spray drying Methods 0.000 claims abstract 2
- 235000019441 ethanol Nutrition 0.000 claims description 24
- 241001165494 Rhodiola Species 0.000 claims description 19
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000284 extract Substances 0.000 claims description 14
- 229940088598 enzyme Drugs 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000012046 mixed solvent Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 108010059892 Cellulase Proteins 0.000 claims description 3
- 108090001060 Lipase Proteins 0.000 claims description 3
- 102000004882 Lipase Human genes 0.000 claims description 3
- 239000004367 Lipase Substances 0.000 claims description 3
- 108090000526 Papain Proteins 0.000 claims description 3
- 108010029182 Pectin lyase Proteins 0.000 claims description 3
- 239000004365 Protease Substances 0.000 claims description 3
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 229940106157 cellulase Drugs 0.000 claims description 3
- 230000009849 deactivation Effects 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000002706 hydrostatic effect Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 235000019421 lipase Nutrition 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229940055729 papain Drugs 0.000 claims description 3
- 235000019834 papain Nutrition 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 244000042430 Rhodiola rosea Species 0.000 abstract description 4
- 235000003713 Rhodiola rosea Nutrition 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 108010009736 Protein Hydrolysates Proteins 0.000 abstract 1
- 230000001476 alcoholic effect Effects 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 230000002255 enzymatic effect Effects 0.000 abstract 1
- 230000000415 inactivating effect Effects 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 description 4
- 230000002745 absorbent Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229920005654 Sephadex Polymers 0.000 description 1
- 239000012507 Sephadex™ Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000004237 preparative chromatography Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method of salidroside, which comprises the following steps: removing mud from the root and stem of rhodiola rosea, cleaning and drying; pulverizing radix Rhodiolae, adding buffer solution, and performing enzymolysis with biological enzyme to obtain enzymolysis solution; inactivating enzyme of the enzymatic hydrolysate, filtering, collecting filtrate, and spray drying to obtain crude extract of salidroside; adding ethanol into the crude extract of salidroside to obtain ethanol extractive solution; adding hydrochloric acid into the alcoholic extractive solution, stirring, and heating to obtain primary extractive solution; centrifuging the primary extraction solution, removing precipitate, collecting supernatant, and performing static pressure at room temperature to obtain high-pressure extraction solution; back-extracting the high-pressure extraction solution, adding a macroporous adsorption resin material, and eluting with ethanol to obtain a purified solution; concentrating the purified solution, evaporating for crystallization, and pulverizing to obtain salidroside powder product. The invention uses the compound enzyme to carry out enzymolysis on the rhodiola rosea, so that the salidroside is dissolved out to the maximum extent, the extraction rate is ensured, and the purity of the salidroside is improved.
Description
Technical field
The present invention relates to medicine extractive technique fields, more particularly to a kind of preparation method of rhodioside.
Background technique
Root of kirilow rhodiola (scientific name: Rhodiola rosea L.), alias: Rhodiola rosea sweeps sieve Ma boolean (hiding name) etc.；For
Herbaceos perennial, it is 10-20 centimetres high.Root thickness are strong, and cone, meat is isabelline, and rootstock has most fibrous roots, and rhizome is short,
Thick shape, cylindrical, the squamaceous leaf arranged by most imbricates.1800-2500 meters of height above sea level high and cold contamination-freely bands are grown in,
Its growing environment is severe, thus has very strong vitality and special adaptability.Can make it is medicinal, can tonifying Qi clearing lung-heat, intelligence development
Nourishing heart is to act on extensive Chinese medicine simply.Also there is very big cosmetic result, skin care item can be made, it is also edible.
Natural plant raw material is especially pulverized by crushing, and partial size is obviously reduced, and specific surface area dramatically increases, and makes
Obtaining product has polymolecularity and highly dissoluble.Raw material, which are ground into Ultramicro-powder, facilitates medical and edible dual purpose plant effective component
It extracts, facilitates the dissolution rate etc. for increasing effective component.The fast development of superfine communication technique, field of food also obtain compared with
Big concern.
The method for extracting rhodioside from root of kirilow rhodiola at present is more, such as: with solvent extraction combination macroporous absorbent resin point
From then with silicagel column purification extraction；Preparation is separated with high performance liquid preparative chromatography method with chemistry.There are also by polyamide, anti-
Four kinds of phase macroreticular resin, silica gel and sephadex column chromatographies are applied in combination and prepare rhodioside.However, existing method exists
Extracted from root of kirilow rhodiola rhodioside recovery rate is low and the low defect of rhodioside purity extracted.
Summary of the invention
One technical problem to be solved by the embodiment of the invention is that: a kind of preparation method of rhodioside is provided, with solution
Certainly problems of the prior art.
According to an aspect of an embodiment of the present invention, a kind of preparation method of the rhodioside provided, comprising:
S1: root of kirilow rhodiola rhizome soil being removed, is cleaned up root of kirilow rhodiola rhizome using medicine washing machine, is dried after cleaning；
S2: root of kirilow rhodiola rhizome is crushed, and 10-20 times of buffer solution of its weight is added, and adjusting pH is 4- 5, temperature 45-
55 DEG C, the biological enzyme of root of kirilow rhodiola weight 0.05-0.1% is added, digests 1.5-3 hours, obtains enzymolysis liquid；
S3: by enzymolysis liquid enzyme deactivation, filtrate is collected in filtering, and the 1/4- 1/2 of concentration filtrate to filtrate original volume is spraying dry
It is dry, obtain rhodioside crude extract；
S4: 15-20 times of weight of enzymolysis and extraction powder of 80% ethyl alcohol is added into rhodioside crude extract, at 70 DEG C
Under the conditions of carry out 2 hours water-bath refluxing extractions, be repeated extract three times later, alcohol extract is made in each 1.5h；
S5: will be added hydrochloric acid, after stirring evenly, be heated to 170 DEG C inside alcohol extract, so that internal alcohol is decomposed into
Alkene and water are discharged after gas, and preliminary extraction solution is made；
S6: will tentatively extract solution and be centrifuged 18 minutes under the conditions of 5000 revs/min, remove precipitating, supernatant be taken, in room
The lower pressure of temperature acts on supernatant with the hydrostatic pressure of 275.5Mpa, obtains high pressure extraction solution；
S7: being saturated with water n-butanol back extraction for high pressure extraction solution, then that the coarse extraction of acquirement also internal addition is big
Macroporous adsorbent resin material, impregnate 2-3 hours it is to be absorbed after, be first eluted with water to no color, then with 10% ethanol elution, obtain
To purification solution；
S8: by purification solution concentration, crystallization operation is evaporated by organic mixed solvent later, after crystallization
Crystalline solid pulverization process, then grinding obtains rhodioside powder-product.
In another embodiment of preparation method based on above-mentioned rhodioside, in the step S1, dried after cleaning
Environmental condition are as follows: root of kirilow rhodiola medicinal material is irradiated using infrared baking lamp, drying temperature controls the irradiation at 70 DEG C -80 DEG C
Time is 18-24 hours.
It,, will after hydrochloric acid is added in the step S5 in another embodiment of preparation method based on above-mentioned rhodioside
The pH value of solution is deployed to 1.5-2.3.
In another embodiment of preparation method based on above-mentioned rhodioside, the biological enzyme in the step S2 is quality
Than the mixture for the cellulase of 20:8:15:2, papain, pectin lyase and lipase.
In another embodiment of preparation method based on above-mentioned rhodioside, the buffer solution in the step S1 is lemon
Lemon acid sodium or citric acid solution.
Organic mixed solvent in another embodiment of preparation method based on above-mentioned rhodioside, in the step S8
For the mixed solvent of ethyl alcohol and ethyl acetate.
In another embodiment of preparation method based on above-mentioned rhodioside, the volume ratio of the ethyl alcohol and ethyl acetate
For 4-8:1, preferably 5-7:1.
In another embodiment of preparation method based on above-mentioned rhodioside, extracted in advance to preliminary in the step S6
The acetic acid lead solution that quality grading is 10% is added dropwise in solution, until precipitating occurs, further removes internal impurity.
Macroporous absorbent resin in another embodiment of preparation method based on above-mentioned rhodioside, in the step S7
Material uses AB-8 resin material, and elution speed is 5 ml/mins.
Evaporative crystallization temperature in another embodiment of preparation method based on above-mentioned rhodioside, in the step S8
Control is at 70 DEG C -80 DEG C, evaporative crystallization 2-3 times repeatedly, and 45 minutes every time.
Compared with prior art, the invention has the following advantages that
Preparation method based on the rhodioside that the above embodiment of the present invention provides, it is maximum with complex enzyme zymohydrolysis root of kirilow rhodiola
Limit dissolves out rhodioside, guarantees that recovery rate further increases rhodioside purity in conjunction with Microwave Extraction, finally carries out
Washing guarantees rhodioside purity, while the operation of whole process to greatest extent, ensure that the bioactivity of rhodioside, have
Effect improves that rhodioside is antitumor and anti-fatigue effect, the alcohol matter of internal residual is eliminated by acidic environment heating, effectively
Remaining alcohol content after reducing alcohol extracting so that rhodioside have better purity, ensure that the doctor of rhodioside
Learn value；Adsorption and purification is carried out by macroporous absorbent resin material, the concentration of rhodioside finished product is improved, so that rhodioside
Practicability it is more outstanding, the fields such as medical treatment, health care and cosmetics can be effectively used for, be worthy to be popularized.
Below by embodiment, technical scheme of the present invention will be described in further detail.
Specific embodiment
Various exemplary embodiments of the invention will now be described in more detail.It should also be noted that unless specifically stated otherwise, otherwise existing
Component described in these embodiments and the positioned opposite of step, numerical expression and numerical value do not limit the scope of the invention.
Be to the description only actually of at least one exemplary embodiment below it is illustrative, never as to the present invention
And its application or any restrictions used.
Technology and equipment known to person of ordinary skill in the relevant may be not discussed in detail, but in appropriate situation
Under, the technology and equipment should be considered as part of specification.
The preparation method of rhodioside includes:
S1: root of kirilow rhodiola rhizome soil being removed, is cleaned up root of kirilow rhodiola rhizome using medicine washing machine, is dried after cleaning；
S2: root of kirilow rhodiola rhizome is crushed, and 10-20 times of buffer solution of its weight is added, and adjusting pH is 4- 5, temperature 45-
55 DEG C, the biological enzyme of root of kirilow rhodiola weight 0.05-0.1% is added, digests 1.5-3 hours, obtains enzymolysis liquid；
S3: by enzymolysis liquid enzyme deactivation, filtrate is collected in filtering, and the 1/4- 1/2 of concentration filtrate to filtrate original volume is spraying dry
It is dry, obtain rhodioside crude extract；
S4: 15-20 times of weight of enzymolysis and extraction powder of 80% ethyl alcohol is added into rhodioside crude extract, at 70 DEG C
Under the conditions of carry out 2 hours water-bath refluxing extractions, be repeated extract three times later, alcohol extract is made in each 1.5h；
S5: will be added hydrochloric acid, after stirring evenly, be heated to 170 DEG C inside alcohol extract, so that internal alcohol is decomposed into
Alkene and water are discharged after gas, and preliminary extraction solution is made；
S6: will tentatively extract solution and be centrifuged 18 minutes under the conditions of 5000 revs/min, remove precipitating, supernatant be taken, in room
The lower pressure of temperature acts on supernatant with the hydrostatic pressure of 275.5Mpa, obtains high pressure extraction solution；
S7: being saturated with water n-butanol back extraction for high pressure extraction solution, then that the coarse extraction of acquirement also internal addition is big
Macroporous adsorbent resin material, impregnate 2-3 hours it is to be absorbed after, be first eluted with water to no color, then with 10% ethanol elution, obtain
To purification solution；
S8: by purification solution concentration, crystallization operation is evaporated by organic mixed solvent later, after crystallization
Crystalline solid pulverization process, then grinding obtains rhodioside powder-product.
In the step S1, the environmental condition dried after cleaning are as follows: root of kirilow rhodiola medicinal material is carried out using infrared baking lamp
Irradiation, at 70 DEG C -80 DEG C, irradiation time is 18-24 hours for drying temperature control.
In the step S5, after hydrochloric acid is added, the pH value of solution is deployed to 1.5-2.3.
Biological enzyme in the step S2 be mass ratio be 20:8:15:2 cellulase, papain, pectin lyase
The mixture of enzyme and lipase.
Buffer solution in the step S1 is sodium citrate or citric acid solution.
Organic mixed solvent in the step S8 is the mixed solvent of ethyl alcohol and ethyl acetate, the ethyl alcohol and acetic acid second
The volume ratio of ester is 4-8:1, preferably 5-7:1.
The acetic acid lead solution that quality grading is 10% is added dropwise in solution to preliminary extract in advance in the step S6, until precipitating
Occur, further removes internal impurity.
Macroporous absorbent resin material in the step S7 uses AB-8 resin material, and elution speed is 5 ml/mins
Clock.
Evaporative crystallization temperature control in the step S8 is at 70 DEG C -80 DEG C, evaporative crystallization 2-3 times repeatedly, and 45 points every time
Clock.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with its
The difference of its embodiment, the same or similar part cross-reference between each embodiment.
Description of the invention is given for the purpose of illustration and description, and is not exhaustively or will be of the invention
It is limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.It selects and retouches
It states embodiment and is to more preferably illustrate the principle of the present invention and practical application, and those skilled in the art is enable to manage
The solution present invention is to design various embodiments suitable for specific applications with various modifications.
Claims (10)
1. a kind of preparation method of rhodioside characterized by comprising
S1: root of kirilow rhodiola rhizome soil being removed, is cleaned up root of kirilow rhodiola rhizome using medicine washing machine, is dried after cleaning；
S2: root of kirilow rhodiola rhizome is crushed, and 10-20 times of buffer solution of its weight is added, and adjusting pH is 4-5, and temperature is 45-55 DEG C,
The biological enzyme of root of kirilow rhodiola weight 0.05-0.1% is added, digests 1.5-3 hours, obtains enzymolysis liquid；
S3: by enzymolysis liquid enzyme deactivation, filtrate, the 1/4-1/2 of concentration filtrate to filtrate original volume are collected in filtering, and spray drying obtains
Rhodioside crude extract；
S4: 15-20 times of weight of enzymolysis and extraction powder of 80% ethyl alcohol is added into rhodioside crude extract, in 70 DEG C of condition
The lower water-bath refluxing extraction for carrying out 2 hours, is repeated extracts three times later, alcohol extract is made in each 1.5h；
S5: will be added hydrochloric acid, after stirring evenly, be heated to 170 DEG C inside alcohol extract, so that internal alcohol is decomposed into alkene
And water, it is discharged after gas, preliminary extraction solution is made；
S6: will tentatively extract solution and be centrifuged 18 minutes under the conditions of 5000 revs/min, remove precipitating, take supernatant, at room temperature
Pressure acts on supernatant with the hydrostatic pressure of 275.5Mpa, obtains high pressure extraction solution；
S7: being saturated with water n-butanol back extraction for high pressure extraction solution, then inhales the coarse extraction of the acquirement also internal macropore that is added
Attached resin material, impregnate 2-3 hours it is to be absorbed after, be first eluted with water to no color, then with 10% ethanol elution, obtain pure
Change solution；
S8: by purification solution concentration, being evaporated crystallization operation by organic mixed solvent later, by the crystallization after crystallization
Body pulverization process, then grinding obtains rhodioside powder-product.
2. the preparation method of rhodioside according to claim 1, which is characterized in that in the step S1, dried after cleaning
Dry environmental condition are as follows: root of kirilow rhodiola medicinal material is irradiated using infrared baking lamp, drying temperature is controlled at 70 DEG C -80 DEG C,
Irradiation time is 18-24 hours.
3. the preparation method of rhodioside according to claim 1, which is characterized in that in the step S5, hydrochloric acid is added
Afterwards, the pH value of solution is deployed to 1.5-2.3.
4. the preparation method of rhodioside according to claim 1, which is characterized in that the biological enzyme in the step S2 is
Mass ratio is the mixture of the cellulase of 20:8:15:2, papain, pectin lyase and lipase.
5. the preparation method of rhodioside according to claim 1, which is characterized in that the buffer solution in the step S1
For sodium citrate or citric acid solution.
6. the preparation method of rhodioside according to claim 1, which is characterized in that organic mixing in the step S8
Solvent is the mixed solvent of ethyl alcohol and ethyl acetate.
7. the preparation method of rhodioside according to claim 6, which is characterized in that the body of the ethyl alcohol and ethyl acetate
Product is than being 4-8:1, preferably 5-7:1.
8. the preparation method of rhodioside according to claim 6, which is characterized in that in advance to preliminary in the step S6
The acetic acid lead solution for being added dropwise that quality grading is 10% in solution is extracted, until precipitating occurs, further removes internal impurity.
9. the preparation method of rhodioside according to claim 6, which is characterized in that the macroporous absorption in the step S7
Resin material uses AB-8 resin material, and elution speed is 5 ml/mins.
10. the preparation method of rhodioside according to claim 6, which is characterized in that the evaporation knot in the step S8
The control of brilliant temperature is at 70 DEG C -80 DEG C, evaporative crystallization 2-3 times repeatedly, and 45 minutes every time.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825731A (en) * | 2020-07-02 | 2020-10-27 | 西藏天虹科技股份有限责任公司 | Extraction method of salidroside |
| CN113897406A (en) * | 2021-09-29 | 2022-01-07 | 山东恒鲁生物科技有限公司 | Method for extracting and purifying salidroside from rhodiola rosea powder |
-
2019
- 2019-03-06 CN CN201910168702.3A patent/CN109929002A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825731A (en) * | 2020-07-02 | 2020-10-27 | 西藏天虹科技股份有限责任公司 | Extraction method of salidroside |
| CN111825731B (en) * | 2020-07-02 | 2022-07-01 | 西藏天虹科技股份有限责任公司 | Extraction method of salidroside |
| CN113897406A (en) * | 2021-09-29 | 2022-01-07 | 山东恒鲁生物科技有限公司 | Method for extracting and purifying salidroside from rhodiola rosea powder |
| CN113897406B (en) * | 2021-09-29 | 2024-06-04 | 山东恒鲁生物科技有限公司 | Method for extracting and purifying salidroside from rhodiola rosea powder |
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