CN115558009A - A method for preparing extract containing salidroside - Google Patents
A method for preparing extract containing salidroside Download PDFInfo
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- CN115558009A CN115558009A CN202211304154.0A CN202211304154A CN115558009A CN 115558009 A CN115558009 A CN 115558009A CN 202211304154 A CN202211304154 A CN 202211304154A CN 115558009 A CN115558009 A CN 115558009A
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- ILRCGYURZSFMEG-UHFFFAOYSA-N Salidroside Natural products OC1C(O)C(O)C(CO)OC1OCCC1=CC=C(O)C=C1 ILRCGYURZSFMEG-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 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 claims abstract description 78
- 238000000034 method Methods 0.000 title claims description 12
- 238000003756 stirring Methods 0.000 claims abstract description 208
- 239000007788 liquid Substances 0.000 claims abstract description 107
- 238000010438 heat treatment Methods 0.000 claims abstract description 54
- 238000001816 cooling Methods 0.000 claims abstract description 40
- 239000000706 filtrate Substances 0.000 claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 244000042430 Rhodiola rosea Species 0.000 claims abstract description 18
- 235000003713 Rhodiola rosea Nutrition 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 15
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 13
- 229940088598 enzyme Drugs 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 230000009849 deactivation Effects 0.000 claims description 4
- 108010059892 Cellulase Proteins 0.000 claims description 3
- 108091005804 Peptidases Proteins 0.000 claims description 3
- 108010059820 Polygalacturonase Proteins 0.000 claims description 3
- 239000004365 Protease Substances 0.000 claims description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 3
- 229940106157 cellulase Drugs 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 21
- 238000000605 extraction Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 8
- 238000013461 design Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 241001165494 Rhodiola Species 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 241000220284 Crassulaceae Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241000997135 Rhodiola crenulata Species 0.000 description 1
- 210000001744 T-lymphocyte Anatomy 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000004064 dysfunction Effects 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000006996 mental state Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 208000037816 tissue injury Diseases 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/80—Mixers with rotating receptacles rotating about a substantially vertical axis
- B01F29/83—Mixers with rotating receptacles rotating about a substantially vertical axis with rotary paddles or arms, e.g. movable out of the receptacle
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/95—Heating or cooling systems using heated or cooled stirrers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/98—Cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/99—Heating
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
A preparation method of an extract containing salidroside comprises the steps of sequentially cleaning, drying and crushing rhodiola rosea to obtain crushed substances, mixing the crushed substances with pure water to obtain crushed liquid, putting the crushed liquid into a stirring tank, sequentially heating and cooling the crushed liquid, filtering after the operation is finished to obtain primary filtrate serving as treatment liquid, standing the treatment liquid at normal temperature until the temperature is consistent with the normal temperature, putting the treatment liquid into a reaction tank, adjusting the pH value of the treatment liquid in the reaction tank to 3-5, heating the treatment liquid, adding enzyme into the treatment liquid for enzymolysis, sequentially deactivating the enzyme after the enzymolysis, and filtering to obtain secondary filtrate serving as the extract containing salidroside. The design not only has good dissolving effect on the rhodiola rosea crushed material, but also can improve the extraction effect.
Description
Technical Field
The invention relates to a preparation process of salidroside, belongs to the field of rhodiola rosea application, and particularly relates to a preparation method of an extract containing salidroside.
Background
Rhodiola rosea (the scientific name: rhodiola rosea L.) is a perennial herb of Rhodiola of Crassulaceae, which is 10-20 cm high, thick in root, conical, fleshy, brownish yellow, has a plurality of fibrous roots at the root neck, short in root stock, thick, cylindrical and covered with a plurality of tile-shaped arranged scaly leaves. The rhodiola rosea grows in alpine and pollution-free areas with the altitude of 1800-2500 m, and the growth environment is severe, so that the rhodiola rosea has strong vitality and special adaptability. Can be used as a medicine, can tonify qi, clear away the lung-heat, benefit intelligence and nourish the heart, and is a traditional Chinese medicine with wide effect. It also has good skin caring effect, and can be used as skin care product or edible product.
Salidroside is the main component of rhodiola, also known as Salidroside or rhodiola extract, and has a sweet taste, is very soluble in water, easily soluble in methanol, soluble in ethanol and hardly soluble in ether. It can not only improve T-cell immunity to restore immune system, improve resistance of organism to toxic accumulated by infection development, and improve mental state of human body, but also alleviate cardiovascular tissue injury and dysfunction caused by pressure, prevent heart contractility decrease due to ambient environmental pressure in rapid freezing state, and help to stabilize contractility.
The Chinese patent with application number of 201210595582.3 and application date of 2012-12-13 discloses a production method for separating and purifying salidroside from rhodiola rosea, which comprises the following steps: the raw materials are crushed and then put into the extraction tank from the feeding hopper, the main machine of the extraction tank set rotates to slowly push the materials backwards from the front end of the unit, meanwhile, the extraction solvent enters the extraction tank from a liquid inlet pipe at the tail end of the unit, the materials which pass through the mobile tank from the rear end of the extraction tank flow to the front end, and the solid-liquid two-phase substances are fully contacted in the reverse movement, so that the active ingredients in the medicinal materials are extracted. Although the design can improve the utilization rate of raw materials by repeatedly using the decoction dregs, the design has the following defects:
the design is based on an extracting solution (the extracting solution is a mixture of a crushed rhodiola rosea and a solvent), the extracting solution is subjected to reflux extraction by using ethanol, so that a crude extracting solution is obtained, and then concentration, adsorption and washing are sequentially performed to obtain an extract containing salidroside.
The information disclosed in this background section is only for enhancement of understanding of the general background of the application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects and problems of poor dissolving effect on the rhodiola rosea crushed material and reduction of the extraction effect in the prior art, and provides a preparation method of an extract containing salidroside, which has good dissolving effect on the rhodiola rosea crushed material and improves the extraction effect.
In order to achieve the above purpose, the technical solution of the invention is as follows: a preparation method of a salidroside-containing extract is a salidroside-containing liquid, and comprises the following steps:
firstly, sequentially cleaning, drying and crushing rhodiola rosea to obtain crushed substances, mixing the crushed substances with pure water to obtain crushed liquid, wherein the mass of the pure water in the crushed liquid is 15-20 times of that of the crushed substances, then putting the crushed liquid into a stirring tank, sequentially heating and cooling the crushed liquid, and filtering after the operation is finished to obtain primary filter residue and primary filtrate, wherein the primary filtrate is the treatment liquid; the heating operation and the cooling operation comprise more than one heating operation;
and secondly, standing the treatment liquid at normal temperature until the temperature is consistent with the normal temperature, placing the treatment liquid in a reaction tank, adjusting the pH value of the treatment liquid in the reaction tank to 3-5, heating the treatment liquid until the temperature of the treatment liquid is 40-60 ℃, adding enzyme into the treatment liquid for enzymolysis, and sequentially performing enzyme deactivation and filtration after the enzymolysis to obtain secondary filter residue and secondary filtrate, wherein the secondary filtrate is the salidroside-containing extract.
The enzyme is any one or any mixture of cellulase, pectinase and protease.
In the first step, the sequentially performing the heating and cooling operations includes: firstly heating the crushed liquid to 40-50 ℃, carrying out primary stirring at the temperature, then cooling the crushed liquid to 5-10 ℃, carrying out secondary stirring at the temperature, then heating the crushed liquid to 60-70 ℃, carrying out tertiary stirring at the temperature, then cooling the crushed liquid to 10-15 ℃, carrying out four-time stirring at the temperature, then heating the crushed liquid to 70-80 ℃, carrying out five-time stirring at the temperature, then cooling the crushed liquid to 15-20 ℃, and carrying out six-time stirring at the temperature.
And the primary stirring, the tertiary stirring and the quintic stirring which correspond to the temperature rising operation are all external stirring carried out on the crushed liquid from outside to inside, and the secondary stirring, the quaternary stirring and the sextic stirring which correspond to the temperature lowering operation are all internal stirring carried out on the crushed liquid from inside to outside.
The stirring tank comprises a tank body, a tank inner cavity, a large cover plate, a small cover plate and a stirring unit, wherein the top of the tank body is in rotating fit with the outer periphery of the large cover plate through an outer bearing; the bottom of stirring unit extends to the inside of jar body, the top of stirring unit extends to directly over little apron.
The stirring unit comprises a left branch pipe, a left stirring part, a right stirring part and a right branch pipe which are sequentially communicated, the top ends of the left branch pipe and the right branch pipe penetrate through the small cover plate and extend to the position right above the small cover plate, the bottom end of the left branch pipe is connected with the top end of the left stirring part, the bottom end of the left stirring part is connected with the bottom end of the right stirring part, and the top end of the right stirring part is connected with the bottom end of the right branch pipe;
the left branch pipe and the right branch pipe are arranged in parallel, the left stirring part and the right stirring part are arranged oppositely, a stirring chamber is clamped between the left stirring part and the right stirring part, and the stirring chamber is positioned in the inner cavity of the tank and is communicated with the inner cavity of the tank; the width of the left stirring part and the right stirring part is larger than the diameter of the left branch pipe and the diameter of the right branch pipe.
The inside of jar body inserts and is connected with many heating rods, and all heating rods evenly set up along same circumference.
In the second step, after the extract containing the salidroside is obtained, the extract containing the salidroside is firstly adsorbed by macroporous adsorption resin, and then sequentially concentrated and dried to obtain a first preparation containing the salidroside, wherein the purity of the salidroside in the preparation is more than 92 percent.
In the second step, after the extract containing the salidroside is obtained, the extract containing the salidroside is firstly absorbed by macroporous absorption resin, and after the absorption is finished, the extract containing the salidroside is washed at least twice by ethanol and then dried in vacuum to obtain a first preparation containing the salidroside, wherein the purity of the salidroside in the preparation is more than 95 percent.
Mixing the primary filter residue and the secondary filter residue to obtain total filter residue, mixing the total filter residue with ethanol to obtain a residue-alcohol mixture, then preserving the temperature of the residue-alcohol mixture at 80-85 ℃ for 0.5-1 hour, filtering to obtain a tertiary filtrate, and then mixing the tertiary filtrate with the secondary filtrate to obtain the salidroside-containing extract.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of the extract containing salidroside firstly obtains the treatment solution, and then carries out acid adjustment, enzymolysis and filtration on the treatment solution to obtain the extract containing salidroside, wherein the key point of the design lies in the operation of temperature rise and temperature reduction in the process of obtaining the treatment solution. Known by whole operation process, the treatment fluid is the basis of follow-up enzymolysis process, just handling incompletely at the treatment fluid stage, will certainly lead to the reduction of extraction effect, for this reason, "intensification, cooling operation" just has been set for on purpose in this design, through the cold and hot switching of temperature lift to and the cold and hot switching of many gradients, not only can promote the dissolving effect of treatment fluid, the reinforcing mixes the degree of consistency, and more do benefit to the decomposition and the precipitation of useful component (the composition that contains salidroside) in the thing of smashing moreover, thereby do benefit to subsequent extraction. Therefore, the invention not only has better dissolving effect on the rhodiola root crushed material, but also can improve the extraction effect.
2. In the preparation method of the salidroside-containing extract, when a preferable scheme is adopted for the heating and cooling operation, namely the first step, the sequentially heating and cooling operation refers to the following steps: firstly heating the crushed liquid to 40-50 ℃, carrying out primary stirring at the temperature, then cooling the crushed liquid to 5-10 ℃, carrying out secondary stirring at the temperature, then heating the crushed liquid to 60-70 ℃, carrying out tertiary stirring at the temperature, then cooling the crushed liquid to 10-15 ℃, carrying out four-time stirring at the temperature, then heating the crushed liquid to 70-80 ℃, carrying out five-time stirring at the temperature, then cooling the crushed liquid to 15-20 ℃, and carrying out six-time stirring at the temperature, thus not only the temperature rise and the temperature fall are in gradient, but also the temperature has certain connectivity, and the operation of temperature rise and temperature fall is accompanied with the stirring, thereby further improving the dissolution effect on the whole effect, enhancing the precipitation of beneficial components and further being beneficial to the final extraction. Therefore, the invention has strong performability and good extraction effect.
3. In the preparation method of the salidroside-containing extract, the first stirring, the third stirring and the fifth stirring which correspond to the heating operation are preferably external stirring for the crushed liquid from outside to inside, and the second stirring, the fourth stirring and the sixth stirring which correspond to the cooling operation are internal stirring for the crushed liquid from inside to outside. Therefore, the invention has better mixing effect and extraction effect on the crushing liquid.
4. In the preparation method of the salidroside-containing extract, the preferable stirring tank comprises a tank body, a tank inner cavity, a large cover plate, a small cover plate and a stirring unit, wherein the top of the tank body is in running fit with the outer periphery of the large cover plate through an outer bearing, the inner periphery of the large cover plate is in running fit with the outer periphery of the small cover plate through an inner bearing, and the middle part of the small cover plate is fixedly connected with the middle part of the stirring unit; the bottom of stirring unit extends to the inside of jar body, the top of stirring unit extends to directly over little apron. The stirring unit comprises a left branch pipe, a left stirring part, a right stirring part and a right branch pipe which are sequentially communicated, the top ends of the left branch pipe and the right branch pipe penetrate through the small cover plate and extend to the position right above the small cover plate, the bottom end of the left branch pipe is connected with the top end of the left stirring part, the bottom end of the left stirring part is connected with the bottom end of the right stirring part, and the top end of the right stirring part is connected with the bottom end of the right branch pipe; the left branch pipe and the right branch pipe are arranged in parallel, the left stirring part and the right stirring part are arranged oppositely, a stirring chamber is clamped between the left stirring part and the right stirring part, and the stirring chambers are positioned in the inner cavity of the tank and are communicated with each other; the width of left side stirring portion, right stirring portion all is greater than the diameter of left branch pipe, right branch pipe, and during the application, drive stirring unit rotates in order to carry out the interior stirring around inner bearing, and drive jar body rotates in order to carry out outer stirring around outer bearing, and interior stirring, outer stirring interval go on to along with corresponding cooling, intensification operation, not only the operation is simple and easy, stirs moreover, mixes the effect better. Therefore, the invention has better mixing effect and convenient operation.
5. In the preparation method of the salidroside-containing extract, a stirring unit comprises a left branch pipe, a left stirring part, a right stirring part and a right branch pipe which are sequentially communicated, and when the preparation method is applied, cold air is sequentially communicated in the left branch pipe, the left stirring part, the right stirring part and the right branch pipe so as to realize cooling; in addition, the inside of jar body inserts and is connected with many heating rods, and all heating rods evenly set up along same circumference, during the application, heat jar body through the heating rod, pass to its inside crushing liquid with the heat again from jar body in, realize the intensification to crushing liquid, and it is thus obvious that intensification, cooling operation are easily realized not only, can not introduce outside impurity moreover, lead to the reduction of mixed effect. Therefore, the invention is not only easy to operate, but also has better mixing effect.
Drawings
FIG. 1 is a schematic view of the construction of a stirring tank in the present invention.
Fig. 2 is a schematic structural view of the stirring unit in fig. 1.
Fig. 3 is a top view of fig. 1.
In the figure: the stirring tank comprises a stirring tank 1, a tank body 2, a tank inner cavity 3, a large cover plate 4, an outer bearing 41, a small cover plate 5, an inner bearing 51, a stirring unit 6, a left branch pipe 61, a left stirring part 62, a right stirring part 63, a right branch pipe 64, a stirring chamber 65 and a heating rod 7.
Detailed Description
The present invention will be described in further detail with reference to the following description and embodiments in conjunction with the accompanying drawings.
Referring to fig. 1 to 3, a method for preparing a salidroside-containing extract, which is a salidroside-containing liquid, comprises the following steps:
firstly, sequentially cleaning, drying and crushing rhodiola rosea to obtain crushed substances, mixing the crushed substances with pure water to obtain crushed liquid, wherein the mass of the pure water in the crushed liquid is 15-20 times of that of the crushed substances, then putting the crushed liquid into a stirring tank 1, sequentially heating and cooling the crushed liquid, and filtering after the operation is finished to obtain primary filter residue and primary filtrate, wherein the primary filtrate is treatment liquid; the heating operation and the cooling operation comprise more than one heating operation;
and secondly, standing the treatment liquid at normal temperature until the temperature is consistent with the normal temperature, placing the treatment liquid in a reaction tank, adjusting the pH value of the treatment liquid in the reaction tank to 3-5, heating the treatment liquid until the temperature of the treatment liquid is 40-60 ℃, adding enzyme into the treatment liquid for enzymolysis, and sequentially performing enzyme deactivation and filtration after the enzymolysis to obtain secondary filter residue and secondary filtrate, wherein the secondary filtrate is the salidroside-containing extract.
The enzyme is any one or any mixture of cellulase, pectinase and protease.
In the first step, the sequentially performing the heating and cooling operations includes: firstly heating the crushed liquid to 40-50 ℃, carrying out primary stirring at the temperature, then cooling the crushed liquid to 5-10 ℃, carrying out secondary stirring at the temperature, then heating the crushed liquid to 60-70 ℃, carrying out tertiary stirring at the temperature, then cooling the crushed liquid to 10-15 ℃, carrying out four-time stirring at the temperature, then heating the crushed liquid to 70-80 ℃, carrying out five-time stirring at the temperature, then cooling the crushed liquid to 15-20 ℃, and carrying out six-time stirring at the temperature.
And the primary stirring, the third stirring and the fifth stirring which correspond to the temperature increasing operation are all external stirring for stirring the crushed liquid from outside to inside, and the secondary stirring, the fourth stirring and the sixth stirring which correspond to the temperature decreasing operation are all internal stirring for stirring the crushed liquid from inside to outside.
The stirring tank 1 comprises a tank body 2, a tank inner cavity 3, a large cover plate 4, a small cover plate 5 and a stirring unit 6, wherein the top of the tank body 2 is in rotating fit with the outer periphery of the large cover plate 4 through an outer bearing 41, the inner periphery of the large cover plate 4 is in rotating fit with the outer periphery of the small cover plate 5 through an inner bearing 51, and the middle part of the small cover plate 5 is fixedly connected with the middle part of the stirring unit 6; the bottom end of the stirring unit 6 extends to the inside of the tank body 2, and the top end of the stirring unit 6 extends to the position right above the small cover plate 5.
The stirring unit 6 comprises a left branch pipe 61, a left stirring part 62, a right stirring part 63 and a right branch pipe 64 which are sequentially communicated, the top ends of the left branch pipe 61 and the right branch pipe 64 penetrate through the small cover plate 5 and then extend to the position right above the small cover plate 5, the bottom end of the left branch pipe 61 is connected with the top end of the left stirring part 62, the bottom end of the left stirring part 62 is connected with the bottom end of the right stirring part 63, and the top end of the right stirring part 63 is connected with the bottom end of the right branch pipe 64;
the left branch pipe 61 and the right branch pipe 64 are arranged in parallel, the left stirring part 62 and the right stirring part 63 are arranged oppositely, a stirring chamber 65 is clamped between the left stirring part 62 and the right stirring part 63, and the stirring chamber 65 is positioned in the inner cavity 3 of the tank and communicated with each other; the widths of the left stirring part 62 and the right stirring part 63 are larger than the diameters of the left branch pipe 61 and the right branch pipe 64.
The inside of jar body 2 inserts and is connected with many heating rods 7, and all heating rods 7 evenly set up along same circumference.
In the second step, after the extract containing salidroside is obtained, the extract containing salidroside is firstly adsorbed by macroporous adsorption resin, and then sequentially concentrated and dried to obtain a first preparation containing salidroside, wherein the purity of the salidroside in the preparation is more than 92 percent.
In the second step, after the extract containing salidroside is obtained, the extract containing salidroside is firstly absorbed by macroporous absorption resin, after the absorption is finished, ethanol is used for washing at least twice, and then vacuum drying is carried out to obtain a first preparation containing salidroside, wherein the purity of the salidroside in the preparation is more than 95%.
Mixing the primary filter residue and the secondary filter residue to obtain total filter residue, mixing the total filter residue with ethanol to obtain a residue-alcohol mixture, then preserving the temperature of the residue-alcohol mixture at 80-85 ℃ for 0.5-1 hour, filtering to obtain a third filtrate, and then mixing the third filtrate with the secondary filtrate to obtain the salidroside-containing extract.
The principle of the invention is illustrated as follows:
the rhodiola rosea used in the present invention refers to the dried root and rhizome of rhodiola crenulata belonging to the family Crassulaceae.
The reason for carrying out the heating and cooling operations on the crushing liquid in sequence is two aspects, one is that the physical structure of the crushing liquid is changed by multiple switching of cold and heat, particularly the physical structure of the crushed material is changed, so that the crushing liquid is further refined in stirring, beneficial components are more favorably decomposed or separated out, and the mixed crushing liquid is more favorably uniform; on the other hand, the growing environment of the rhodiola rosea is mostly in a high and cold non-pollution zone with the altitude of 1800-2500 m, so that the cooling operation is more suitable for the growing temperature of the rhodiola rosea, and the beneficial components are more favorably separated out.
Example 1:
referring to fig. 1 to 3, a method for preparing a salidroside-containing extract, which is a salidroside-containing liquid, comprises the following steps:
firstly, sequentially cleaning, drying and crushing rhodiola rosea to obtain crushed substances, mixing the crushed substances with pure water to obtain crushed liquid, wherein the mass of the pure water in the crushed liquid is 15-20 times of that of the crushed substances, then putting the crushed liquid into a stirring tank 1, sequentially heating and cooling the crushed liquid, and filtering after the operation is finished to obtain primary filter residue and primary filtrate, wherein the primary filtrate is treatment liquid; the heating and cooling operation comprises more than one heating operation;
and secondly, standing the treatment liquid at normal temperature until the temperature is consistent with the normal temperature, placing the treatment liquid in a reaction tank, adjusting the pH value of the treatment liquid in the reaction tank to 3-5, heating the treatment liquid until the temperature of the treatment liquid is 40-60 ℃, adding enzyme into the treatment liquid for enzymolysis, and sequentially performing enzyme deactivation and filtration after the enzymolysis to obtain secondary filter residue and secondary filtrate, wherein the secondary filtrate is the extract containing the salidroside.
Example 2:
the basic contents are the same as example 1, except that:
in the first step, the sequentially heating and cooling operations include: firstly heating the crushed liquid to 40-50 ℃, carrying out primary stirring at the temperature, then cooling the crushed liquid to 5-10 ℃, carrying out secondary stirring at the temperature, then heating the crushed liquid to 60-70 ℃, carrying out tertiary stirring at the temperature, then cooling the crushed liquid to 10-15 ℃, carrying out four-time stirring at the temperature, then heating the crushed liquid to 70-80 ℃, carrying out five-time stirring at the temperature, then cooling the crushed liquid to 15-20 ℃, and carrying out six-time stirring at the temperature. And the primary stirring, the third stirring and the fifth stirring which correspond to the temperature increasing operation are all external stirring for stirring the crushed liquid from outside to inside, and the secondary stirring, the fourth stirring and the sixth stirring which correspond to the temperature decreasing operation are all internal stirring for stirring the crushed liquid from inside to outside.
Example 3:
the basic content is the same as that of the embodiment 2, except that:
structurally: preferably, the stirring tank 1 comprises a tank body 2, a tank inner cavity 3, a large cover plate 4, a small cover plate 5 and a stirring unit 6, wherein the top of the tank body 2 is in running fit with the outer periphery of the large cover plate 4 through an outer bearing 41, the inner periphery of the large cover plate 4 is in running fit with the outer periphery of the small cover plate 5 through an inner bearing 51, and the middle part of the small cover plate 5 is fixedly connected with the middle part of the stirring unit 6; the bottom end of the stirring unit 6 extends to the inside of the tank body 2, and the top end of the stirring unit 6 extends to the position right above the small cover plate 5. The stirring unit 6 comprises a left branch pipe 61, a left stirring part 62, a right stirring part 63 and a right branch pipe 64 which are sequentially communicated, the top ends of the left branch pipe 61 and the right branch pipe 64 penetrate through the small cover plate 5 and then extend to the position right above the small cover plate 5, the bottom end of the left branch pipe 61 is connected with the top end of the left stirring part 62, the bottom end of the left stirring part 62 is connected with the bottom end of the right stirring part 63, and the top end of the right stirring part 63 is connected with the bottom end of the right branch pipe 64; the left branch pipe 61 and the right branch pipe 64 are arranged in parallel, the left stirring part 62 is arranged opposite to the right stirring part 63, a stirring chamber 65 is clamped between the left stirring part 62 and the right stirring part 63, and the stirring chamber 65 is positioned in the inner cavity 3 of the tank and communicated with each other; the widths of the left stirring part 62 and the right stirring part 63 are larger than the diameters of the left branch pipe 61 and the right branch pipe 64. The inside of jar body 2 inserts and is connected with many heating rods 7, and all heating rods 7 evenly set up along same circumference.
The operation method comprises the following steps: tank body 2 rotates around outer bearing 41 in order to realize outer stirring, and stirring unit 6 stirs in order to realize around inner bearing 51, and simultaneously, outer stirring cooperatees with the operation of rising the temperature, and interior stirring cooperatees with the operation of cooling down. The cooling operation is performed by passing cold air through the left branch pipe 61, the left stirring part 62, the right stirring part 63 and the right branch pipe 64 in sequence, so as to maintain the fluidity of the cold air until the temperature is reduced to a required value, and simultaneously, the cooling rate can be controlled. The temperature raising operation is realized by heat transfer of the heating rod 7 to the crushing liquid through the tank body 2.
Example 4:
the basic contents are the same as example 1, except that:
in the second step, after the extract containing the salidroside is obtained, the extract containing the salidroside is firstly adsorbed by macroporous adsorption resin, and then sequentially concentrated and dried to obtain a first preparation containing the salidroside, wherein the purity of the salidroside in the preparation is more than 92 percent.
Or,
in the second step, after the extract containing the salidroside is obtained, the extract containing the salidroside is firstly absorbed by macroporous absorption resin, and after the absorption is finished, the extract containing the salidroside is washed at least twice by ethanol and then dried in vacuum to obtain a first preparation containing the salidroside, wherein the purity of the salidroside in the preparation is more than 95 percent.
Example 5:
the basic contents are the same as example 1, except that:
mixing the primary filter residue and the secondary filter residue to obtain total filter residue, mixing the total filter residue with ethanol to obtain a residue-alcohol mixture, then preserving the temperature of the residue-alcohol mixture at 80-85 ℃ for 0.5-1 hour, filtering to obtain a third filtrate, and then mixing the third filtrate with the secondary filtrate to obtain the salidroside-containing extract.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention as set forth in the appended claims.
Claims (10)
1. A preparation method of an extract containing salidroside, wherein the extract containing salidroside is a liquid containing salidroside, and is characterized in that the preparation method comprises the following steps:
firstly, sequentially cleaning, drying and crushing rhodiola rosea to obtain crushed substances, mixing the crushed substances with pure water to obtain crushed liquid, wherein the mass of the pure water in the crushed liquid is 15-20 times of that of the crushed substances, then putting the crushed liquid into a stirring tank (1), sequentially heating and cooling the crushed liquid, and filtering after the operation is finished to obtain primary filter residue and primary filtrate, wherein the primary filtrate is treatment liquid; the heating operation and the cooling operation comprise more than one heating operation;
and secondly, standing the treatment liquid at normal temperature until the temperature is consistent with the normal temperature, placing the treatment liquid in a reaction tank, adjusting the pH value of the treatment liquid in the reaction tank to 3-5, heating the treatment liquid until the temperature of the treatment liquid is 40-60 ℃, adding enzyme into the treatment liquid for enzymolysis, and sequentially performing enzyme deactivation and filtration after the enzymolysis to obtain secondary filter residue and secondary filtrate, wherein the secondary filtrate is the extract containing the salidroside.
2. The method for preparing a salidroside-containing extract according to claim 1, wherein: the enzyme is any one or any mixture of cellulase, pectinase and protease.
3. The method for producing a salidroside-containing extract according to claim 1 or 2, wherein: in the first step, the sequentially heating and cooling operations include: firstly heating the crushed liquid to 40-50 ℃, carrying out primary stirring at the temperature, then cooling the crushed liquid to 5-10 ℃, carrying out secondary stirring at the temperature, then heating the crushed liquid to 60-70 ℃, carrying out tertiary stirring at the temperature, then cooling the crushed liquid to 10-15 ℃, carrying out four-time stirring at the temperature, then heating the crushed liquid to 70-80 ℃, carrying out five-time stirring at the temperature, then cooling the crushed liquid to 15-20 ℃, and carrying out six-time stirring at the temperature.
4. The method for preparing a salidroside-containing extract according to claim 3, wherein: and the primary stirring, the third stirring and the fifth stirring which correspond to the temperature increasing operation are all external stirring for stirring the crushed liquid from outside to inside, and the secondary stirring, the fourth stirring and the sixth stirring which correspond to the temperature decreasing operation are all internal stirring for stirring the crushed liquid from inside to outside.
5. The method for producing a salidroside-containing extract according to claim 1 or 2, wherein: the stirring tank (1) comprises a tank body (2), a tank inner cavity (3), a large cover plate (4), a small cover plate (5) and a stirring unit (6), wherein the top of the tank body (2) is in running fit with the outer periphery of the large cover plate (4) through an outer bearing (41), the inner periphery of the large cover plate (4) is in running fit with the outer periphery of the small cover plate (5) through an inner bearing (51), and the middle part of the small cover plate (5) is fixedly connected with the middle part of the stirring unit (6); the bottom of stirring unit (6) extends to the inside of jar body (2), the top of stirring unit (6) extends to directly over little apron (5).
6. The method for preparing a salidroside-containing extract according to claim 5, wherein: the stirring unit (6) comprises a left branch pipe (61), a left stirring part (62), a right stirring part (63) and a right branch pipe (64) which are sequentially communicated, the top ends of the left branch pipe (61) and the right branch pipe (64) penetrate through the small cover plate (5) and then extend to the position right above the small cover plate (5), the bottom end of the left branch pipe (61) is connected with the top end of the left stirring part (62), the bottom end of the left stirring part (62) is connected with the bottom end of the right stirring part (63), and the top end of the right stirring part (63) is connected with the bottom end of the right branch pipe (64);
the left branch pipe (61) and the right branch pipe (64) are arranged in parallel, the left stirring part (62) and the right stirring part (63) are arranged oppositely, a stirring chamber (65) is clamped between the left stirring part (62) and the right stirring part (63), and the stirring chamber (65) is positioned in the inner cavity (3) of the tank and communicated with each other; the widths of the left stirring part (62) and the right stirring part (63) are larger than the diameters of the left branch pipe (61) and the right branch pipe (64).
7. The method for preparing a salidroside-containing extract according to claim 6, wherein: the inside of jar body (2) inserts and is connected with many heating rod (7), and all heating rod (7) evenly set up along same circumference.
8. The method for producing a salidroside-containing extract according to claim 1 or 2, wherein: in the second step, after the extract containing salidroside is obtained, the extract containing salidroside is firstly adsorbed by macroporous adsorption resin, and then sequentially concentrated and dried to obtain a first preparation containing salidroside, wherein the purity of the salidroside in the preparation is more than 92 percent.
9. The method for producing a salidroside-containing extract according to claim 1 or 2, wherein: in the second step, after the extract containing salidroside is obtained, the extract containing salidroside is firstly absorbed by macroporous absorption resin, after the absorption is finished, ethanol is used for washing at least twice, and then vacuum drying is carried out to obtain a first preparation containing salidroside, wherein the purity of the salidroside in the preparation is more than 95%.
10. The method for producing a salidroside-containing extract according to claim 1 or 2, wherein: mixing the primary filter residue and the secondary filter residue to obtain total filter residue, mixing the total filter residue with ethanol to obtain a residue-alcohol mixture, then preserving the temperature of the residue-alcohol mixture at 80-85 ℃ for 0.5-1 hour, filtering to obtain a third filtrate, and then mixing the third filtrate with the secondary filtrate to obtain the salidroside-containing extract.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392011A (en) * | 2008-11-05 | 2009-03-25 | 江南大学 | Isolation and purification method of natural salidroside |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| 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 |
| CN114225730A (en) * | 2021-12-24 | 2022-03-25 | 湖北省吉美化妆品有限公司 | Emulsifying device and emulsifying process for emulsion skin care products |
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- 2022-10-24 CN CN202211304154.0A patent/CN115558009A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392011A (en) * | 2008-11-05 | 2009-03-25 | 江南大学 | Isolation and purification method of natural salidroside |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| 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 |
| CN114225730A (en) * | 2021-12-24 | 2022-03-25 | 湖北省吉美化妆品有限公司 | Emulsifying device and emulsifying process for emulsion skin care products |
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