CN107456458A - A kind of method for magnetizing destructive distillation extraction rhodioside health products - Google Patents
A kind of method for magnetizing destructive distillation extraction rhodioside health products Download PDFInfo
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- 241001165494 Rhodiola Species 0.000 claims abstract description 104
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 42
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- 238000000746 purification Methods 0.000 claims description 7
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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 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7032—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a polyol, i.e. compounds having two or more free or esterified hydroxy groups, including the hydroxy group involved in the glycosidic linkage, e.g. monoglucosyldiacylglycerides, lactobionic acid, gangliosides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- 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
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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
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
The present invention relates to the extracting method of rhodioside, more particularly to a kind of method for magnetizing destructive distillation extraction rhodioside health products, the method for the magnetization destructive distillation extraction rhodioside health products, comprises the following steps：（1）After rhodiola root is cleaned up, drying and crushing, 80 mesh sieves are crossed, obtain rhodiola root powder；（2）Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 150 ~ 280MHz, and magnetic field intensity is 6200 ~ 9500Gs；（3）Rhodiola root after magnetization is added into 5 ~ 15min of ultrasonic disperse in solvent, 30min is then stood at 5 ~ 15 DEG C, then destructive distillation purifies, that is, obtains rhodioside.The present invention is magnetized using high-frequency electric field, activates rhodiola root, further press filtration, is added ethanol solution and is precipitated, and further destructive distillation purifying, obtains high-purity rhodioside.This method is magnetized by high-frequency electric field, rhodioside is easy to activation and is leached, and not only yield is high, moreover, the red-spotted stonecrop glycosides purity obtained by destructive distillation is high, can be used as health products.
Description
Technical field
The present invention relates to the extracting method of rhodioside, more particularly to one kind magnetization destructive distillation extraction rhodioside health products
Method.
Background technology
Chinese Medicine Industry turns into the national new source of economic growth.Data show, 2015, the traditional Chinese medicine industry total yield in China
Value accounts for medicinal industry scale nearly 1/3 up to 786,600,000,000 yuan, has derived Chinese medicine industry, medicinal plant farming, Chinese medicine business, Chinese medicine guarantor
Strong product and food and daily chemical product etc..The big health industry scale of Chinese medicine breaks through trillion, and market development potential is huge.With people
Living material become better and better, people to diet more be particular about health and science, herbal cuisine have very big innovative space.With medical science
The progress of science and technology, traditional Chinese medicine will be accelerated development, and promote the well-being of mankind health, and further goes to the world.At present, traditional Chinese medicine standards system
Preliminarily form, for standard number up to 649, Development of Chinese Medicine average annual growth rate is about 29%, and traditional Chinese medicine has the irreplaceable spy of Western medicine
Point and effect.In particular with stepping up for people's health consciousness, herbal health care product are the emphasis of field of health care products development.
The national policy that country issues in recent years, Chinese herbal medicine development are tilting in terms of herbal health care.Policy vigorously support and
Under the background that Traditional Chinese medicine health-preserving knowledge is constantly popularized, enterprise and consumer deepen to the understanding of Chinese medicine, and increasing people is ready to use
Chinese medicine replaces Western medicine, and even during usually health control, Chinese medicine is also more by consumers, and Chinese medicine is to Western medicine
Substitution effect expanding.
Rhodiola is perennial herb or the wild plant of undershrub in Angiospermae Rosales Crassulaceae rhodiola
Thing, its aboundresources is various in style, and northeast, Gansu, Xinjiang, Sichuan, Tibet and Yunnan, Guizhou etc. are mainly distributed in China
Ground.Rhodiola root has very strong vitality and special adaptability, belongs to natural precious medicinal plant.Rhodioside is rhodiola root
In principle active component, and evaluation rhodiola root and its extract most important index.Modern pharmacology research confirmation, red scape
Its glycosides has extensive physiologically active, has adjustment effect to angiocarpy：There is protection to oxygen re supply damage cardiac muscle cell after anoxic
Effect, can make after anoxic that oxygen supply beating rate of myocardial cells remains normal again, reduce LDH releases, maintain myocardial cell membrane, myogen
The ultra microstructures such as fiber, mitochondria are normal.The effect of Central nervous system：Rhodioside can strengthen brain stem network
Excitability, the spontaneous potential activity of primary structure under cortical sensibility-motor area, visual area and cortex is excited, strengthens and photoelectricity is pierced
The current potential for swashing stress reaction changes.To the adjustment effect of immune system：Rhodioside can adjust normal human under cryogenic conditions
Specificity and non-specific immune function, strengthen cold tolerance, accelerate the foundation of acclimatization to cold.In addition, rhodioside also has
There is the effect such as antitumor, radioresistance, anti anoxia.Therefore, it is extremely important to the separating-purifying of rhodioside as health medicine.
At present, domestic and foreign scholars to the chemical composition of rhodiola root, pharmacological action, principle active component Structural Identification have compared with
For in-depth study, but the research to its extraction and purification process is also in the starting stage.Conventional extracting method mainly has immersion
Or heat reflow method, these method extraction times are long, solvent load is big, recovery rate is low and complex operation, it is difficult to reach medicinal and want.
The content of the invention
For current rhodioside extraction time is long, solvent load is big, recovery rate is low, purity is low and complex operation not
Foot, the present invention propose a kind of method for magnetizing destructive distillation extraction rhodioside health products, rhodioside is easy to activation and leach, not only
Yield is high, and the rhodioside purity obtained by destructive distillation is high, can be used as medicament.
To solve the above problems, the present invention uses following technical scheme：
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
（1）After rhodiola root is cleaned up, drying and crushing, 80 mesh sieves are crossed, obtain rhodiola root powder；
（2）Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 150 ~ 280MHz, and magnetic field intensity is
6200~9500Gs；
（3）Rhodiola root after magnetization is added into 5 ~ 15min of ultrasonic disperse in solvent, 30min is then stood at 5 ~ 15 DEG C, then
Destructive distillation purifies, that is, obtains rhodioside.
The present invention does not have special requirement to the source of rhodiola root raw material, and its species can be the art personnel institute
Know, such as can be at least one of wild sachalin rhodiola rhizome, bright red premium red-spotted stonecrop or spring onion rhodiola root.
Rhodiola root is dried first in the present invention, then magnetization treatment is carried out to it, it is preferred that in step（1）In, institute
Stating dry technique is：By rhodiola root temperature be 20 ~ 40 DEG C, pressure be -100 ~ -30KPa under conditions of, be dried to water content
For 5 ~ 15%.
Magnetic field processing can activate the rhodioside in rhodiola root in the present invention, depart from from rhodiola root matrix, therefore,
The intensity and frequency in magnetic field are that magnetic field intensity is too low, then can not play activation rhodiola root an important factor for influenceing rhodiola root activation
The effect of glycosides, and magnetic field intensity is too high, then can destroy rhodioside again, effectively rhodioside can not be extracted, preferably
, in step（2）In, the field frequency is 180 ~ 250MHz, and magnetic field intensity is 6900 ~ 8300Gs.
Another key factor for influenceing rhodioside activation is exactly the time handled in magnetic field, magnetization treatment time mistake
It is short, then it can not play a part of activating rhodioside, and magnetization treatment overlong time, then can destroy rhodioside again, can not
Effectively rhodioside is extracted, it is preferred that in step（2）In, processing time of the rhodiola root powder in high frequency magnetic field is 3
~ 10min, in order to improve the activation efficiency of rhodioside, reduce processing time, it is preferred that the magnetization treatment temperature is 15 ~ 40
℃。
Solvent is the medium for extracting rhodioside, and solvent is mixed in proportion with rhodioside, can be made red after activation
Red-spotted stonecrop glycosides dissolves in a solvent, therefore solvent is also an important factor for influenceing rhodioside extraction efficiency, it is preferred that the solvent
For at least one of ethanol, acetone, ethyl acetate, carbon tetrachloride, n-hexane and deionized water.Rhodioside is in a solvent
Solubility is bigger, can more improve its dissolved efficiency, and the solubility of rhodioside in organic solvent is substantially better than it in water
Solubility, therefore preferable organic solvent of the present invention, because the rhodioside prepared by the present invention is mainly used as medicament and health care
Product, therefore, the organic solvent should select the solvent nontoxic to human body, and such as ethanol, in order to reduce cost, solvent of the invention is excellent
Elect the mixed solvent of water and ethanol as.
The ratio of solvent and rhodiola root is to influence another key factor of extraction efficiency, if the too high levels of solvent,
It can then make that the purification time in later stage is elongated, and time-consuming, add time cost, and if the content of solvent is too low, then make red scape
The solubility of its glycosides in a solvent reaches capacity, part rhodioside can not the dissolution from rhodiola root, reduce rhodioside
Extraction efficiency, it is preferred that the weight ratio of the solvent and rhodiola root is（20~120）：1.
The present invention is separated solvent and rhodioside by destructive distillation, it is preferred that the technique of destructive distillation purifying is：It is first
First rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 30- is incubated when temperature reaches 86 DEG C~95 DEG C
50min, allows the abundant desolventizing of rhodiola root；Continue slowly heating after insulation, start to collect gas phase when temperature reaches 98 ~ 105 DEG C
Rhodioside extract solution, until temperature reaches 110~118 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, is obtained
To the rhodioside extract solution of liquid.By allowing vapor sufficiently to volatilize, the concentration of extract solution is improved, it is red fully extracting
While red-spotted stonecrop glycosides, because temperature reduces, the destruction of rhodioside is reduced, while shortens purification time, improves production
Efficiency, and because temperature control is more accurate, so as to get extract solution stable components, improve the quality of product.
In order to further improve the purity of rhodioside, it is preferred that carry out destructive distillation after purification to rhodiola root, also set
Fat adsorption and purification.
Preferably, the technique of the resin adsorption purifying is：The rhodioside extract solution that step (3) is obtained passes through macropore
Resin column, macroporous resin column filling nonpolar macroporous adsorption resin, with the washing decontamination of 1~2 times of column volume after absorption, then
With 50~70% ethanol elution rhodiosides of 2~3 times of column volumes, the eluent of rhodioside is collected, be concentrated under reduced pressure elution
Liquid obtains rhodioside crystal to doing.
In order to further improve the purity of rhodioside, it is preferred that after macroporous resin adsorption, with 2 times of column volumes
Wash decontamination, then the 70% ethanol elution rhodioside with 3 times of column volumes.
A kind of method for magnetizing destructive distillation extraction rhodioside health products of the present invention, compared with prior art, its spy protruded
Point and excellent effect are：
The present invention takes rhodiola root to crush, and is magnetized using high-frequency electric field, activates rhodiola root, departs from from rhodiola root matrix, passes through
The parameter of high frequency magnetic field is adjusted, rhodioside is easy to activation and leaches, then add ethanol solution and precipitated, further destructive distillation
Purifying, obtains high-purity rhodioside, further carries out resin adsorption purifying, obtains the rhodiola root that purity is 98.2 ~ 99.9%
Glycosides, the present invention magnetize rhodiola root by high-frequency electric field, and not only yield is high for obtained rhodioside, and purity is high, extraction time
It is short, it is with a wide range of applications in medicament and health products.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 20 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -80KPa, it is 5% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 150MHz, magnetic field intensity 6200Gs,
Magnetizing time is 3min, and magnetization temperature is 15 DEG C；
Rhodiola root after magnetization is added into ultrasonic disperse 5min in ethanol, wherein（The weight of rhodiola root and ethanol ratio is 20：1）,
Then 30min is stood at 5 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 30min is incubated when temperature reaches 86 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, the rhodioside for starting to collect gas phase when temperature reaches 98 DEG C carries
Liquid is taken, until temperature reaches 110 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the rhodioside of liquid
Extract solution；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 1~2 times of column volume, then the 50 ethanol elution rhodiosides with 2 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain high-purity salidroside crystal to doing.Whole extraction process, extraction process are easy
Control, extraction time is short, and extraction efficiency is high, and yield is more than 92% so that rhodioside is fully extracted.As shown in table 1.
Embodiment 2
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 25 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -100KPa, it is 6% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 160MHz, magnetic field intensity 6500Gs,
Magnetizing time is 4min, and magnetization temperature is 16 DEG C；
Rhodiola root after magnetization is added into ultrasonic disperse 6min in acetone, wherein（The weight of rhodiola root and acetone ratio is 30：1）,
Then 30min is stood at 6 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 40min is incubated when temperature reaches 87 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, start to collect the rhodiola root of gas phase when temperature reaches 98 ~ 105 DEG C
Glycosides extract solution, until temperature reaches 112 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the red scape of liquid
Its glycosides extract solution；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 1 times of column volume, then the 52% ethanol elution rhodioside with 3 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain rhodioside crystal to doing.Whole extraction process, extraction process is easily-controllable, extraction
Time is short, and extraction efficiency is high, and yield is high so that rhodioside is fully extracted.As shown in table 1.
Embodiment 3
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 24 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -50KPa, it is 8% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 200MHz, magnetic field intensity 7200Gs,
Magnetizing time is 5min, and magnetization temperature is 20 DEG C；
Rhodiola root after magnetization is added into ultrasonic disperse 7min in ethyl acetate, wherein（The weight of rhodiola root and ethyl acetate ratio
For 100：1）, then stand 30min at 8 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 50min is incubated when temperature reaches 90 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, start to collect the rhodiola root of gas phase when temperature reaches 98 ~ 105 DEG C
Glycosides extract solution, until temperature reaches 115 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the red scape of liquid
Its glycosides extract solution；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 2 times of column volumes, then the 58% ethanol elution rhodioside with 2 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain rhodioside crystal to doing.Whole extraction process, extraction process is easily-controllable, extraction
Time is short, and extraction efficiency is high, and yield is high so that rhodioside is fully extracted.As shown in table 1.
Embodiment 4
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 40 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -30KPa, it is 12% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 280MHz, magnetic field intensity 9500Gs,
Magnetizing time is 10min, and magnetization temperature is 40 DEG C；
Rhodiola root after magnetization is added into ultrasonic disperse 5min in carbon tetrachloride, wherein（The weight of rhodiola root and carbon tetrachloride ratio
For（120：1）, then stand 30min at 15 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 30min is incubated when temperature reaches 95 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, the rhodioside for starting to collect gas phase when temperature reaches 105 DEG C carries
Liquid is taken, until temperature reaches 118 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the rhodioside of liquid
Extract solution；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 2 times of column volumes, then the 70% ethanol elution rhodioside with 2 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain rhodioside crystal to doing.Whole extraction process, extraction process is easily-controllable, extraction
Time is short, and extraction efficiency is high, and yield is high so that rhodioside is fully extracted.As shown in table 1.
Embodiment 5
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 35 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -58KPa, it is 13% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 250MHz, magnetic field intensity 8500Gs,
Magnetizing time is 9min, and magnetization temperature is 36 DEG C；
Rhodiola root after magnetization is added into ultrasonic disperse 12min in deionized water, wherein（The weight of rhodiola root and deionized water ratio
For 58：1）, then stand 30min at 7 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 45min is incubated when temperature reaches 95 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, the rhodioside for starting to collect gas phase when temperature reaches 102 DEG C carries
Liquid is taken, until temperature reaches 116 DEG C, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the rhodioside of liquid
Extract solution；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 2 times of column volumes, then the 65% ethanol elution rhodioside with 3 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain rhodioside crystal to doing.Whole extraction process, extraction process is easily-controllable, extraction
Time is short, and extraction efficiency is high, and yield is high so that rhodioside is fully extracted.As shown in table 1.
Comparative example 1：
A kind of method for magnetizing destructive distillation extraction rhodioside health products, comprises the following steps：
It it is 20 DEG C in temperature after rhodiola root is cleaned up, under conditions of pressure is -80KPa, it is 5% to be dried to water content, so
After grind, cross 80 mesh sieves, obtain rhodiola root powder；
Rhodiola root powder is added into ultrasonic disperse 5min in ethanol, wherein（The weight of rhodiola root and ethanol ratio is 20：1）, then
30min is stood at 5 DEG C；
Rhodiola root is put into gas retort under atmospheric pressure state and carries out heat temperature raising, 50min is incubated when temperature reaches 86 DEG C, allows
The abundant desolventizing of rhodiola root；Continue slowly heating after insulation, start to collect the rhodioside extraction of gas phase when temperature reaches 98
Liquid, until temperature reaches 110, the rhodioside extract solution of gas phase is cooled down by condenser, obtains the rhodioside extraction of liquid
Liquid；
Above-mentioned rhodioside extract solution is passed through into macroporous resin column, macroporous resin column filling nonpolar macroporous adsorption resin, absorption
Afterwards with the washing decontamination of 1~2 times of column volume, then the 50 ethanol elution rhodiosides with 2 times of column volumes, rhodiola root is collected
The eluent of glycosides, the eluent that is concentrated under reduced pressure obtain rhodioside crystal to doing.Whole extraction process, not only purity is low, and
Rate substantially reduces height, as shown in table 1.
Comparative example 2：
According to Chinese patent CN201610688870.1《A kind of technique of ultrasonic assistant extraction rhodioside》Method,
A kind of technique of ultrasonic assistant extraction rhodioside, is comprised the following steps that：
A, dry rhodiola is handled, shredded, crossed 300 mesh sieves, obtain rhodiola powder；
B, rhodiola is weighed, rhodiola powder is handled using subpackage, it is pressed into 500g- with medical non-woven fabrics
1000g is wrapped up, and medical non-woven fabrics at least wraps up 3 layers；
C, the rhodiola bandaged is put into closed container, the ethanol solution for adding 65-75% is soaked, immersion at least 4
Hour；
D, the rhodiola of immersion is placed in ultrosonic extractor, ultrasonic power 700W-1100W, temperature 70-85
DEG C, extract at least four times；Add 60-80% petroleum ether for the first time, extract 20-40min；Second plus 50-80% n-butanol, are carried
Take 20-40min；The methanol of third time plus 65-80%, extract 30-40min；The chloroform of the 4th time plus 60-80%, extract 20-
60min；
E, merge after No. four extract solutions being cooled into room temperature, obtain extract solution；
F, citrate synthase will be added in extract solution, is 10MPa in pressure, temperature is distilled under conditions of being 110-160 DEG C；
Distillation time is 20-40min；
G, after distilling, add adjuvant and concentrated, then dried, produce rhodioside；Include activity in the adjuvant
Charcoal and atlapulgite.
Whole extraction process complex process, extraction time length, yield are low.As shown in table 1.
Table 1：
| Test event | Rhodioside purity | Rhodioside yield | Extraction time（h） |
| Embodiment 1 | 99.9% | 92.3% | <1.5 |
| Embodiment 2 | 99.5% | 93.6% | <1.5 |
| Embodiment 3 | 99.3% | 91.5% | <2 |
| Embodiment 4 | 98.8% | 93.4% | <2 |
| Embodiment 5 | 98.2% | 92.8% | <2.5 |
| Comparative example 1 | 71.3% | 67.5% | <3 |
| Comparative example 2 | 98% | 82.2% | >10 |
Claims (10)
- A kind of 1. method for magnetizing destructive distillation extraction rhodioside health products, it is characterised in that comprise the following steps：（1）After rhodiola root is cleaned up, drying and crushing, 80 mesh sieves are crossed, obtain rhodiola root powder；（2）Rhodiola root powder is put into high frequency magnetic field and handled, wherein field frequency is 150 ~ 280MHz, and magnetic field intensity is 6200~9500Gs；（3）Rhodiola root after magnetization is added into 5 ~ 15min of ultrasonic disperse in solvent, 30min is then stood at 5 ~ 15 DEG C, then Destructive distillation purifies, that is, obtains rhodioside.
- 2. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that in step （1）In, the technique of the drying is：By rhodiola root temperature be 20 ~ 40 DEG C, pressure be -100 ~ -30KPa under conditions of, drying It is 5 ~ 15% to water content.
- 3. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that in step （2）In, the field frequency is 180 ~ 250MHz, and magnetic field intensity is 6900 ~ 8300Gs.
- 4. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that in step （2）In, processing time of the rhodiola root powder in high frequency magnetic field is 3 ~ 10min, and treatment temperature is 15 ~ 40 DEG C.
- 5. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that the solvent For at least one of ethanol, acetone, ethyl acetate, carbon tetrachloride, n-hexane and deionized water.
- 6. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that the solvent Weight ratio with rhodiola root is（20~120）：1.
- 7. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that the destructive distillation The technique of purifying is：Rhodiola root is put into gas retort under atmospheric pressure state first and carries out heat temperature raising, when temperature reaches 86 DEG C 30-50min is incubated at~95 DEG C, allows the abundant desolventizing of rhodiola root；Continue slowly heating after insulation, when temperature reaches 98 ~ 105 DEG C When start collect gas phase rhodioside extract solution, until temperature reaches 110~118 DEG C, the rhodioside extract solution of gas phase leads to Condenser cooling is crossed, obtains the rhodioside extract solution of liquid.
- 8. the method for magnetization destructive distillation extraction rhodioside health products according to claim 1, it is characterised in that to rhodiola root Carry out destructive distillation after purification, also carry out resin adsorption purifying.
- 9. the method for magnetization destructive distillation extraction rhodioside health products according to claim 8, it is characterised in that the resin The technique of adsorption and purification is：The rhodioside extract solution that step (3) is obtained passes through macroporous resin column, and macroporous resin column filling is non- Polar macroporous adsorption resin, with the washing decontamination of 1~2 times of column volume after absorption, then with the 50 of 2~3 times of column volumes~ 70% ethanol elution rhodioside, the eluent of rhodioside is collected, the eluent that is concentrated under reduced pressure obtains rhodioside to doing.
- 10. the method for magnetization destructive distillation extraction rhodioside health products according to claim 9, it is characterised in that through macropore After resin adsorption, with the washing decontamination of 2 times of column volumes, then the 70% ethanol elution rhodioside with 3 times of column volumes.
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