CN107441763B - A kind of raising immunity, anti-inflammatory, radiation protection saussurea involucrata Herba Epimedii rhodiola root composition - Google Patents
A kind of raising immunity, anti-inflammatory, radiation protection saussurea involucrata Herba Epimedii rhodiola root composition Download PDFInfo
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- CN107441763B CN107441763B CN201710873871.8A CN201710873871A CN107441763B CN 107441763 B CN107441763 B CN 107441763B CN 201710873871 A CN201710873871 A CN 201710873871A CN 107441763 B CN107441763 B CN 107441763B
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- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/38—Other non-alcoholic beverages
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Abstract
A kind of saussurea involucrata means of supercritical extraction device is disclosed, the extraction element is efficient, and can reduce the generation of by-product in extraction process to the maximum extent, and the extract to make has higher pharmacological activity.
Description
Technical field
The present invention relates to a kind of saussurea involucrata means of supercritical extraction devices, and the Saussurea involucrata extract obtained using the device.
Background technology
Saussurea involucrata is the rare rare Chinese medicine in China, have it is remote with history and abundant civil medication basis,
The flavones and its glycosides that contain in saussurea involucrata, Phenylpropanoid Glycosides class, sesquiterpene lactone, cumarin, lignanoid, organic acid, amino acid, steroidal,
The ingredients such as polysaccharide have antirheumatic, analgesia, adjust the bioactivity such as cardiovascular system, anticancer, anti-aging, radiation protection, have
Prodigious medicinal Development volue.
In the exploitation of saussurea involucrata Chinese medicine, quality control is particularly critical, in particular how controls saussurea involucrata active constituent and carries
It is a problem to take the content of middle impurity.The ingredients such as rutin, chlorogenic acid, Syringin and dehydro-α-curcumene are non-lanatechead saussurea herb with flower
Peculiar desired constituents, how they effectively to be detached with pharmacological component to extraction process improve it is very high requirement and
Challenge.
CN101041653B discloses a kind of method of extraction and enriching saussurea involucrate total flavone, and this method first surpasses saussurea involucrata
Critical CO2Extraction obtains therein volatile and hot unstable ingredient, is then extracted again with Conventional solvents.By overcritical extraction
Xuelianhuangtong ingredient after taking is easier to release out of plant.
CN102106890B discloses application and preparation method and the saussurea involucrata total sesquiterpene lactone of saussurea involucrata total sesquiterpene lactone
Application in preparing anti-anoxic medicine can pass through solvent method, carbon dioxide supercritical extraction, total times of petroleum ether refluxing extraction
Sesquiterpene lactone, experiment find and demonstrate drug of the saussurea involucrata total sesquiterpene lactone for preparing gained in the preparation of anti-anoxic medicine
With apparent oxygen lack resistant function.
The extracting method of CN104397683A saussurea medusa flower essence substances, includes the following steps：(1) saussurea medusa flower
Pretreatment；(2) saussurea medusa flower and deionized water and bean curd obtained pretreatment mixes, and with boiling 2-10 hours, bean curd is removed in drift,
Filtering, obtains filtrate i, and the residue of gained after filtering is dried in the shade；(3) by the residue after drying in the shade with rice vinegar to mix thoroughly, bored profit 6-10 point
Clock, after rice vinegar is absorbed to the greatest extent, until in frying container, with slow boiling fried dry, taking-up is dried in the air cool；(4) cooling residue is pulverized, mistake
20-40 mesh sieves, and places and is extracted in supercritical extraction reactor, and the temperature of extraction is 50-70 DEG C, and the pressure of extraction is 20-40Mpa, with
Ethyl alcohol is entrainer, uses CO2Follow bad extraction 2-5 hours, after extraction in separating still discharge hole for discharge, obtain filtrate II；(5)
Filtrate I and filtrate II are mixed, the filtering with microporous membrane for being 0.22 μm with aperture obtains filtrate III；(6) by filtrate III 60 DEG C with
Lower rotary evaporation is concentrated under reduced pressure, until being concentrated to solid content as 60-80%；(7) concentrate is dried to get jellyfish
Herba Saussureae Involueratae extract.
CN106511213A discloses a kind of cosmetics having plant extraction liquid, is mixed by the ingredient of following weight percents
It is combined into：Aloe 20-50%, yellow chamomile 5-20%, lanatechead saussurea herb with flower 5-15%, Jasmine 10-30%, tealeaves 10-20%；It will be above-mentioned
After ingredient is mixed according to weight percent, drying and crushing, medicinal powder carries out carbon dioxide supercritical extraction, using absolute ethyl alcohol as solvent
Extraction is concentrated under reduced pressure recycling ethyl alcohol, obtains alcohol extracting concentrate；By the dregs of a decoction after carbon dioxide supercritical extraction with concentration 10%-
70% ethanol solution is Extraction solvent, and after heating extraction and concentration, concentrate is crossed macroporous resin column and is enriched with, and use is dense
Degree is that 30%-90% alcohol repeatedly elutes, and eluent is dissolved after reduced pressure with 1.3 butanediols, filtering, finally with two
Carbonoxide supercritical extract is worth solution mixing to get plant extraction liquid.
CN102106889A discloses the application and its snow of a kind of saussurea involucrata and Saussurea involucrata extract in preparing anti-anoxic medicine
The preparation method of lotus extract, the one kind of the saussurea involucrata in snow lotus of big bud, Saussurea medusa or Saus-surea obvallata (DC.) Edgew, the saussurea involucrata carry
It is one kind in snow lotus of big bud extract, Saussurea medusa extract or Saus-surea obvallata (DC.) Edgew extract to take object；The Saussurea involucrata extract is
The water extract of saussurea involucrata or the ethanol extract of saussurea involucrata and its through systematic solvent extraction extraction and Flavonoids by Macroporous Adsorption Resin extraction gained
Anti anoxia active component.
A kind of Saussurea involucrata extracts of CN101209274A, it is characterised in that by weight percentage containing 0.5% to 1.2% purple
Syringin, 7% to 17% chlorogenic acid and 8% to 25% rutin.
" research of saussurea involucrata water-soluble polysaccharide extraction process ", Liu Chunlan etc., food and biotechnology journal, 2007,26
(3):37-40 compares the factors such as solid-liquid ratio, temperature, extraction time to saussurea involucrata Polyose extraction in Xinjiang Saussurea involucrate tissue culture
The influence of rate, and provide the optimum extraction process of saussurea involucrata water-soluble polysaccharide.
In summary, number of drawbacks is still had in the prior art, and especially the extracting method of saussurea involucrata is still in the prior art
What is continued to use is traditional extraction process, although the existing report for extracting saussurea involucrata pharmacological active substance using supercritical process, still
It is the conventional supercritical extracting equipment and technique continued to use, pharmacology active component content is relatively low and undesirable in extract
Impurity content is higher.In addition, there is not yet Saussurea involucrata extract, Shorthorned Epimedium P.E and gadol extract compounding are prepared compound
The report of preparation, or be usually all that the extract i.e. crude extract that three is contained complicated ingredient mixes, not only effect is poor, and
And synergistic effect is also poor.This field needs extraction equipment and the side of a kind of Saussurea involucrata extract efficiently obtaining high pharmacological activity
Method.
Invention content
To solve the above-mentioned technical problems in the prior art simultaneously, the present invention provides a kind of saussurea involucrata means of supercritical extraction
Device, using can effectively extract acquisition pharmacological component when the device, pharmacological component content is high and undesirable miscellaneous
Matter content is low.Above-mentioned Saussurea involucrata extract and there is high anti-inflammatory efficacy comprising its compound preparation, improve efficacy of immunity etc.,
And the synthesis pharmacological activity improved.For this purpose, the present invention provides following technical schemes.
In one aspect of the invention, a kind of saussurea involucrata means of supercritical extraction device is provided, which includes：Intake section carries
Take part and exit portion.
For the present invention, the intake section may include：Carbon dioxide supply tank (1), is connected to pressure meter
(5) valve (2,4,7), compressor (3), carbon dioxide storage reservoir (6), high-pressure pump (8), coil pipe (9) and towards extraction pond
(11) CO2Inlet valve (10).
For the present invention, the extraction part may include：It extracts pond (11), the pressure gauge (12) being connect with extraction pond,
The heating system being made of emitting bulb (13), the fan (14) for making equalizing temperature and microthermometer, the precision
Thermometer is connect with temperature controller (15) is used for measuring temperature.
For the present invention, the exit portion may include：The outlet valve (16) in extraction pond, extract collector (17),
Heating bath (18) and flowmeter (19).
Preferably, the extraction pond is made of stainless steel alloy.
It is highly preferred that the composition of the stainless steel alloy is by weight percentage：0.3%≤Mn≤0.8%；3.0%
≤ Cr≤6.0%；4.0%≤Ni≤10.0%；1.0%≤Al≤2%；1.0%≤Ti≤1.5%, 0.001%≤P≤
0.02%, 0.1%≤W≤0.2%；0.001%≤S≤0.005%；0.0001%≤N≤0.0060%；0.0001%≤C
≤ 0.025%；0.0001%≤Si≤0.25；0.0001%≤O≤0.0050%, surplus Fe.
The present inventor is the study found that in the alloy, the addition of Ti is remarkably improved the intensity of alloy, makes alloy through height
Its fracture toughness can be improved after carrying out timeliness crystal grain thinning again in warm deformation, and the addition of Ni can improve the toughness of alloy.Al and
Ni and Al and it is W-shaped at intermetallic compound, dispersion-strengthened action and antioxidation can be played in the alloy, to carry
The intensity and impact flexibility of high alloy, such as the alloy than being not added with Ni, W are compared, and intensity improves 30-50%.
The extraction pond of the present invention can be by the following method made by the alloy：
(1) half is first made into product by raw material ingot casting；
(2) and then at 850-920 DEG C described half is made to carry out Isothermal treatment at product, isothermal time is 3-6 hours, so
It is quickly cooled to the temperature less than or equal to -80 DEG C afterwards to carry out depth cooling treatment；
(3) aging anneal processing is carried out at 400-480 DEG C, aging time is 10-20 hours.
The extraction pond that the present invention is obtained by the above method still has particularly preferred resistance to fracture and tough under extremely high pressure
Property, and be not easy to generate by CO under high pressure2Surface erosion caused by sour gas so that can in elevated pressures and
Means of supercritical extraction is carried out under lower temperature.
In another aspect of this invention, the method for extracting saussurea involucrata active ingredient using said extracted device, the party are provided
Method includes：(1) device is made to reach the pressure condition needed for extraction in intake section；(2) in extraction part in selected temperature and
It is extracted under pressure condition；(3) extract is taken out in exit portion.
In another aspect of this invention, the saussurea involucrata for providing using above-mentioned apparatus or being obtained using the above method is extracted
Object.
Preferably, the content of volatile oil is less than 1.2wt% in the Saussurea involucrata extract.It is highly preferred that the saussurea involucrata extraction
Rutin in object, chlorogenic acid, Syringin and dehydro-α-curcumene total content be less than 2.5wt%.Most preferably, the saussurea involucrata carries
The lactone compound total content with parent nucleus shown in following formula (a) in object is taken to be more than 65.0wt%：
The present inventor the study found that when the said components in Saussurea involucrata extract simultaneously meet the content requirement when, can
Particularly effectively ensure the pharmacological activity of Saussurea involucrata extract, especially antiphlogistic effects.
In the present invention, it is preferred to extraction a diameter of 6.1 centimetres of pond (11), be highly 18 centimetres, available capacity is
0.50L；The emitting bulb power is 200-300W；The temperature is calculated as ASQ F200 microthermometers, the temperature control
Device is SCM Based temperature controller.In the present invention, due to made of aforementioned alloy extract pond can bear it is higher
Pressure, thus extraction can carry out at a lower temperature, required temperature can be obtained by using lamp heated, so as to gram
It takes and heats uneven and relatively low (such as temperature runaway of heating control precision existing for existing conventional heating means such as oil bath or heating water bath
Phenomenon) the problem of, so as to effectively prevent the fluctuation of supercritical extract condition, effectively reduce the generation of extraction by-product.
The present inventor has found that the optimum process condition of saussurea involucrata extraction is by many experiments：By drying and crushing (such as grain size
400 ± 25 μm) lanatechead saussurea herb with flower (such as 25 grams) be put into ultrasonic extraction pond, extract and carry at 40 DEG C and pressure 10.34MPa
Object, every batch of extraction is taken to carry out 120-180 minutes, carbon dioxide drainage speed is 125.25 ± 15.00m L/min, will be used to collect
The pond of extract is immersed in ice-water bath (8 ± 0.5 DEG C).
In another aspect of this invention, a kind of composition including said extracted object is provided.The composition also includes
Shorthorned Epimedium P.E and gadol extract.The weight ratio of Saussurea involucrata extract, Shorthorned Epimedium P.E and gadol extract is
(10-5):(1-3):(1-3)。
In another aspect of this invention, the purposes for providing above-mentioned composition, human immunity work(can be enhanced by being used to prepare
Drug, health products or the drink of energy.
Preferably, the purity of the glucosides substance in Herba Epimedii composition is more than 99.0wt%.It is highly preferred that the glucosides
The purity of substance is more than 99.2wt%.Most preferably, the purity of the glucosides substance is more than 99.7wt%.
The glucosides substance is preferably or includes the mixture of compound shown in lower formula (I) and (II)：
The weight ratio of formula (I) and formula (II) compound is preferably 1:5-5:1.
Studies have shown that described two compounds are glucoside compound, with general flavone compound such as icariine A
It is compared with B, there is especially extensive and relatively high bioactivity, such as anti-osteoporosis disease, anti-inflammatory and antitumaous effect.
The formula (I) and formula (II) compound preferably are extracted to obtain by following method：
(1) MeOH (preferably 3 × 6L, each soaking time are about 20h) extraction Herba Epimedii herbal medicine powder is used at room temperature (preferably
1.18kg), combined extract is evaporated under reduced pressure to obtain brown residue (162.5g) i.e. methanol extract liquid；
(2) reverse phase silica gel column (such as RP-18 silicagel columns) is utilized, uses MeOH-H first2O mixed solutions are to the remnants
Object carries out gradient elution, and to carry out pillar layer separation, preferred elution step is 0:1 (1L), 1:9 (1L), 2:8 (1L), 3:7
(1L), 4:6 (1L), 5:5 (2L), 6:4 (2L), 7:3 (1L), 1:0 (2L) then uses acetone (2L), obtains 10 successively and wash
De- component is denoted as elution component A-J；
(3) elution fraction B (such as 6.5g) is subjected to chromatographic isolation on silicagel column (preferably 60cm × 5cm), uses use
CHCl3-MeOH-H2O mixed solutions carry out gradient elution, and (gradient is preferably 20:1:0 (1L), 10:1:0 (2L), 30:8:1
(2L) and 15:6:1 (2.5L)), 4 elution components are obtained, elution fraction B1-B4 is denoted as；
(4) elution fraction B2 (such as 300.2mg) is used into MeOH-H2O(1:1) in Sephadex LH-20 (preferably 100cm
× 3cm) on detach, obtain 7 time elution fractions, be denoted as elution fraction B2.1-B2.7；
(5) by the mixture (such as total weight 210.5mg) of elution fraction B2.5 and B2.6 by silica gel CC columns (preferably
80cm × 2.5cm), eluent EtOAc-CHCl3-MeOH-H2O(12:6:3:1), eluent is concentrated to dryness, is obtained
The mixture of compound shown in pale yellow powder (such as 11.2mg), as formula (I) and formula (II).
The method can effectively exclude the interference of albumen and other impurity, and other low liter polysaccharide can also be had
The separation of effect.The applicant is obtained by above-mentioned 5 grades of column chromatography for separation shown in formula (I) and the formula (II) of extreme high purity for the first time
Compound, has close level and matching relationship between 5 grades of piece-rate systems, for example, sequence selection with regard to extremely important.
For the present invention, the gadol extract is preferably rhodioside.Rhodioside can take this field
Conventional method extracts.It is further preferred that the gadol extract is modified gadol extract, it is most preferably, described red
Red-spotted stonecrop extract is by being modified the lower formula (II) obtained or (III) compound represented to rhodioside：
Compared with general natural nucleoside substance, the immunological regulation of formula (II) or (III) compound represented to normal mouse
Effect becomes apparent from, and due to the introducing of electron-withdrawing group Cl and F, enhances its ability for removing free radical, can dramatically increase mouse
Special antibody secreting cell number can enhance delayed allergy intensity in 50mg/ (kgd) dosage, in addition also show
Go out the phagocytic function of the mixed lymphocyte reaction (MLP) to special-shaped mouse and macrophage, and can reduce to a certain extent white
The activity of cytokine shows that the two is a kind of up-and-coming immunomodulator.
Substance with structure formula (II)-(III) can synthesize by the following method：MCM-22 is added in the reaction vessel
Molecular sieve alternatively property catalyst, is then added chloroform solvent, then by the chloroacetic chloride of natural salidroside and chloro or fluoro
With 1:The molar ratio of 1-1.3 is added in reaction dissolvent that (chloroacetic chloride of natural salidroside and chloro or fluoro is preferably with chlorine
Imitative solution form is added), reaction temperature is 20-30 DEG C, reaction time 10-30min, and separation and drying can be obtained describedization
Close object.This method has the advantages that high income, impurity are few.It is particularly due to the shape-selective effect of MCM-22 molecular sieves, can significantly be dropped
The generation of low side reaction.
In another aspect of this invention, the purposes for providing the composition, human immunity work(can be enhanced by being used to prepare
Energy, the drug with antiphlogistic effects or radiation-proof effect, health products or drink.
Preferably, the drug is Chinese traditional compound medicine.Preferably, the composition is used to prepare oral capsule, electuary
Deng.The health products include oral-cavity article such as chewable tablets or lozenge.
Description of the drawings
Fig. 1 is the schematic diagram of extraction element according to the present invention.
Specific implementation mode
Embodiment 1
Saussurea involucrata for extracting is Herba Saussureae Involueratae (managing Co., Ltd purchased from Urumchi Bei Yuan spring agricultural and sideline products).
The extraction element of use includes：Intake section, extracts part and exit portion, the intake section may include：Carbon dioxide supplies
Storage tank (1) is given, the valve (2,4,7) of pressure meter (5), compressor (3), carbon dioxide storage reservoir (6), high pressure are connected to
It pumps (8), coil pipe (9) and the CO towards extraction pond (11)2Inlet valve (10)；The extraction part may include：It extracts pond (11), with
The pressure gauge (12) for extracting pond connection, by emitting bulb (13), fan (14) and microthermometer for making equalizing temperature
The heating system of composition, the microthermometer is connect with temperature controller (15) is used for measuring temperature, and the exit portion can
Including：Extract the outlet valve (16) in pond, extract collector (17), heating bath (18) and flowmeter (19)；The extraction Chi Youshang
The text stainless steel alloy is made；Process conditions are：The lanatechead saussurea herb with flower of 25 grams of drying and crushings (400 ± 25 μm) is put into ultrasonic wave extraction
It takes in pond, extract is extracted under 40 DEG C and 10.34MPa pressure, every batch of extraction carries out 180 minutes, carbon dioxide drainage speed
For 125.25 ± 17.22m L/min, will be immersed in ice-water bath (8 ± 0.5 DEG C) for collecting the pond of extract.After testing, saussurea involucrata
The content of volatile oil is 1.0wt% in extract, rutin, chlorogenic acid, Syringin and dehydro-α-curcumene total content be
1.1wt%.Most preferably, the lactone compound total content with parent nucleus shown in formula (a) in the Saussurea involucrata extract is
81.1wt%.
Comparative example 1
Means of supercritical extraction is carried out according to the method that embodiment in CN102106890B is recorded.After testing, in Saussurea involucrata extract
The content of volatile oil is 2.3wt%, rutin, chlorogenic acid, Syringin and dehydro-α-curcumene total content be 4.3wt%.Most
Preferably, the lactone compound total content with parent nucleus shown in formula (a) in the Saussurea involucrata extract is 77.3wt%.
It can be seen from above-described embodiment and comparative example the present invention extraction element can lactone compound total content slightly
In the case of being improved, the content of undesirable component can be significantly reduced.
Embodiment 2
Inhibiting effect of the Saussurea involucrata extract of testing example 1 to adjuvant-induced arthritis secondary lesion.
Wistar rats 60 are taken, half male and half female, 150~200g of weight, half male and half female is randomly divided into 3 groups, i.e., normal right
According to group, conventional extract group (0.05gkg-1, control group, wherein Saussurea involucrata extract are according to the side described in CN101041653B
Method obtains), 1 extract group (0.05gkg of embodiment-1)；It first uses toes capacity measurer to measure the left back vola pedis of every group of rat to hold
It is worth based on product.In addition to Normal group, remaining each group is in right metapedes plantar subcutaneous injection Freund ' s Freund's complete adjuvants
0.1mL, cause it is scorching after each administration groups of 12d start gastric infusion, the distilled water of Normal group and model group gavage equivalent, continuously
8d.Each group measures left back vola pedis (non-injection toes) volume to 20d with toes volumetric type meter every other day after administration.It is dynamic to calculate each group
The toes swelling of object.
Compared with model group and control group, the Saussurea involucrata extract of embodiment 1 inhibits adjuvant-induced arthritis secondary lesion
Significant difference is acted on, shows that the FUFANG XUELIAN JIAONANG of the present invention can effectively mitigate adjuvant-induced arthritis secondary lesion, has
Apparent anti-inflammatory effect has obvious inhibiting effect if even if extending with administration time in the case of low dosage, see the table below 1：
Table 1：Saussurea involucrata extract is to adjuvant-induced arthritis secondary lesion inhibiting effect
| Group | Dosage/gkg-1 | 3rd day toes swelling/ml after cause is scorching |
| Normal group | - | 0.14±0.05 |
| Embodiment 1 group (according to present invention) | 0.05 | 0.95±0.12 |
| Conventional extract group | 0.05 | 1.15±0.18 |
By above example clearly it can be seen from the present invention Saussurea involucrata extract obtained relative to conventional Supercritical extraction method
The extract arrived has good inhibiting effect, especially has apparent better antiphlogistic effects.
Embodiment 3
Include the preparation of the capsule of Saussurea involucrata extract, Shorthorned Epimedium P.E and gadol extract, wherein 1 institute of Example
Saussurea involucrata extract, previously described Shorthorned Epimedium P.E and the gadol extract stated, Saussurea involucrata extract, Shorthorned Epimedium P.E and
The weight ratio of gadol extract is 8:1:1, each capsule contains 0.1g contents.By the capsule according to the method for embodiment 2
The inhibiting effect test to adjuvant-induced arthritis secondary lesion is carried out to cause after inflammation the 3rd day under same dose and experiment condition
Toes swelling (ml) be 0.86 ± 0.11.
By embodiment 2 and 3 again it can be seen that the addition of Shorthorned Epimedium P.E and gadol extract, enhances saussurea involucrata
The antiphlogistic effects of extract.Its reason is speculated, in addition to Shorthorned Epimedium P.E and gadol extract itself have centainly anti-inflammatory
Certain mutually collaboration facilitation may be also created outside effect, between three.
This written description discloses the present invention, including optimal mode using example, and also enables those skilled in the art
It manufactures and using the present invention.The present invention can patentable scope be defined by the claims, and may include this field skill
Other examples that art personnel expect.If this other examples have not different from the structural elements of the literal language of claims
Element, or if this other examples include with equivalent structure element of the literal language of claims without substantial differences,
Then this other examples are intended within the scope of claims.In the case where inconsistent degree will not be caused, by reference to
It will be incorporated herein in place of all references referred to herein.
Claims (2)
1. a kind of raising immunity, anti-inflammatory, radiation protection saussurea involucrata Herba Epimedii rhodiola root composition, the composition are also carried comprising Herba Epimedii
Object and gadol extract are taken, the weight ratio of Saussurea involucrata extract, Shorthorned Epimedium P.E and gadol extract is (10-5):(1-
3):(1-3)；
The content of volatile oil is less than 1.2wt% in the Saussurea involucrata extract, rutin, chlorogenic acid, purple fourth in the Saussurea involucrata extract
The total content of fragrant glycosides and dehydro-α-curcumene is less than 2.5wt%, has the interior of parent nucleus shown in following formula (a) in the Saussurea involucrata extract
Ester compounds total content is more than 65.0wt%：
The purity of glucosides substance in the Shorthorned Epimedium P.E is more than 99.0wt%；
The glucosides substance is the mixture of compound shown in lower formula (I) and (II)：
The weight ratio of formula (I) and formula (II) compound is 1:5-5:1；
The gadol extract is by being modified the lower formula (III) compound represented obtained to rhodioside：
Formula (III) compound represented synthesizes by the following method：MCM-22 molecular sieve conducts are added in the reaction vessel
Then chloroform solvent is added in catalysts selective, then by the chloroacetic chloride of natural salidroside and chloro with 1:The molar ratio of 1-1.3
It is added in reaction dissolvent, reaction temperature is 20-30 DEG C, reaction time 10-30min, and separation and drying obtain the formula
(III) compound represented.
2. composition according to claim 1, wherein the formula (I) and formula (II) compound are extracted by following method
It arrives：
(1) Herba Epimedii herbal medicine powder is extracted with MeOH at room temperature, combined extract is evaporated under reduced pressure to obtain brown residue i.e.
Methanol extract liquid；
(2) reverse phase silica gel column is utilized, uses MeOH-H first2O mixed solutions carry out gradient elution to the residue, to carry out
Pillar layer separation, elution step 0:1 total 1L, 1:9 total 1L, 2:8 total 1L, 3:7 total 1L, 4:6 total 1L, 5:5 total 2L, 6:4 total 2L,
7:3 total 1L, 1:Then 0 total 2L uses acetone 2L, obtains 10 elution fractions successively, be denoted as elution component A-J；
(3) elution fraction B is subjected to chromatographic isolation on a silica gel column, uses CHCl3-MeOH-H2O mixed solutions carry out gradient and wash
It is de-, gradient 20:1:0 total 1L, 10:1:0 total 2L, 30:8:1 total 2L and 15:6:1 total 2.5L obtains 4 elution components,
It is denoted as elution fraction B1-B4；
(4) by elution fraction B2 with 1:1 MeOH-H2O is detached on Sephadex LH-20, obtains 7 elution fractions, note
For elution fraction B2.1-B2.7；
(5) mixture of elution fraction B2.5 and B2.6 are passed through into silica gel CC columns, eluent 12:6:3:1 EtOAc-CHCl3-
MeOH-H2Eluent is concentrated to dryness by O, obtains pale yellow powder, and as compound shown in formula (I) and formula (II) is mixed
Close object.
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| CN201710873871.8A CN107441763B (en) | 2017-09-25 | 2017-09-25 | A kind of raising immunity, anti-inflammatory, radiation protection saussurea involucrata Herba Epimedii rhodiola root composition |
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| CN201810900857.7A Active CN108969555B (en) | 2017-09-25 | 2017-09-25 | A Chinese medicinal composition comprising herba Epimedii with kidney invigorating, blood and essence replenishing, and immunity improving effects, and its preparation method |
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| CN1548430A (en) * | 2003-05-08 | 2004-11-24 | 中国科学院地球化学研究所 | Supercritical CO2 extraction process for refining neotanshinone IIA from red sage |
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