CN106924349A - A kind of isopentene group flavonoid extract, its preparation method and application - Google Patents
A kind of isopentene group flavonoid extract, its preparation method and application Download PDFInfo
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- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The invention discloses a kind of preparation method of isopentene group flavonoid extract, methods described is optimized by each extracting parameter, the content of the isopentene group flavonoid extract for preparing is more than 50%, and favorable reproducibility, resin is reusable, and technological operation is easy, and preparation amount is big, product purity is high, and low stain.Meanwhile, the present invention also provides a kind of application of isopentene group flavonoid extract prepared by preparation method of the present invention in treatment NASH, fat-reducing or hypoglycemic.
Description
Technical field
Carried the present invention relates to a kind of chromocor extract, its preparation method and application, especially a kind of isopentene group flavonoids
Take thing, its preparation method and application.
Background technology
Traditional Chinese medical theory thinks that the root bark of white mulberry has removing heat from lung and relieving asthma, and effect of inducing diuresis for removing edema cures mainly lung heat cough and asthma, oedema swollen
Full oliguria, appearance skin edema etc..Pharmacological evaluation confirms that there is the root bark of white mulberry hypoglycemic, hypotensive, antiviral, diuresis etc. to act on.
Ancient times book on Chinese herbal medicine is such as《Mingyi Bielu》、《Big bright book on Chinese herbal medicine》Record it and control and quench one's thirst, it is alone i.e. effective.Its main active is flavones
Class, polysaccharide and alkaloid compound.Be connected with isopentene group in root bark of white mulberry flavonoids structure, with hypotensive,
Hypoglycemic, HIV-resistant activity, antibacterial, anticancer etc. are acted on.
At present, in root bark of white mulberry chromocor extract, the content of isopentene group flavonoid extract is relatively low, can't reach and use
It is required that.Useful polyamide purifies the report of root bark of white mulberry flavones, but the dead absorption of polyamide is serious, be difficult wash-out, the damage of flavones
Lose very greatly, and be 33.5% with the isopentene group Flavonoid Content after polyamide purifying, be also not reach drug registration much
The active component content that management method specifies accounts for more than the 50% of extract regulation.
The content of the invention
Based on this, a kind of iso-amylene base class is provided it is an object of the invention to overcome above-mentioned the deficiencies in the prior art part
The preparation method of chromocor extract.
To achieve the above object, the technical solution used in the present invention is：A kind of system of isopentene group flavonoid extract
Preparation Method, methods described comprises the following steps：
(1) by dry root bark of white mulberry pulverizing medicinal materials, using alcohol solution dipping 3.5~4 hours after, at 60~90 DEG C,
Refluxing extraction twice, 1.5~2 hours every time, merges extract solution, wherein, root bark of white mulberry medicinal material is molten with ethanol in each refluxing extraction
The mass volume ratio of liquid is (1:6~1:10)g/ml；
Or ethanol solution is soaked into root bark of white mulberry medicinal material after 12~24 hours at 45~50 DEG C, constant temperature constant speed carries out diacolation,
Percolate is collected, extract solution is obtained, wherein, root bark of white mulberry medicinal material is (1 with the mass volume ratio of ethanol solution:4~1:8)g/ml；
Wherein, in root bark of white mulberry medicinal material, sanggenon C, Saliggenon D, the weight/mass percentage composition of moracin are all higher than 0.1%, or
Sanggenon C, Saliggenon D, the weight/mass percentage composition sum of moracin are not less than 0.35%, the volume fraction of ethanol in ethanol solution
It is 60~80%；
(2) step (1) gained extract solution filtered, be concentrated under reduced pressure into crude drug concentration for 0.11~0.13g/ml, ethanol
Volume fraction is 30~45%, obtains concentrate；
(3) concentrate is adsorbed using macroporous absorbent resin, is then eluted with the water of 4BV~8BV, wash-out speed
It is 1.5BV/h to spend, then is carried out with the flow velocity of 1~2BV/h with the ethanol solution that the volume fraction of 6BV~8BV is 70%~90%
Wash-out, collects eluent；
(4) it is eluent is concentrated under reduced pressure, dry, obtain the isopentene group flavonoid extract.
Preferably, it is 1 according to the mass volume ratio of root bark of white mulberry medicinal material and ethanol solution in the step (1):10g/ml's
Ratio, the ethanol solution for adding volume fraction to be 80%, refluxing extraction is carried out 1.5 hours to root bark of white mulberry medicinal material；According still further to Sang Bai
Skin medicinal material is 1 with the mass volume ratio of ethanol solution:The ratio of 8g/ml, adds the ethanol solution that volume fraction is 80%, to mulberry
White skin medicinal material carries out refluxing extraction 1.5 hours, merges extract solution twice.Root bark of white mulberry medicinal material is carried according to above-mentioned steps (1)
Take, the efficiency high of extraction, median extraction yield is higher than 85.32%.
Preferably, in the step (1), the ethanol solution that volume fraction is 80% is soaked into root bark of white mulberry medicinal material at 50 DEG C
After 12 hours, with the ethanol solution that volume fraction is 80% temperature be 50 DEG C, flow velocity carry out diacolation for 0.5 times of volume/hour,
Percolate is collected, wherein in immersion process, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:4g/ml, diacolation process
In, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:8g/ml.
Preferably, it is in the step (2), the step of extract solution is filtered：To first liquid precipitate be extracted more than 1 hour, so
Afterwards by extract solution with 300 mesh filter plate circulating filtrations.Filter effect and speed are so may further ensure that, is reduced as far as possible yellow
The loss of ketone.
Further, since raw material grinding particle size is smaller, the dope in extract easily blocks filter cloth, therefore one section of filtering
Filter cloth should be pulled down cleaning by the time after slowing, and be filtered again.
Preferably, in the step (2), the thickening temperature of process concentrated under reduced pressure is not more than 70 DEG C, and vacuum is not less than
0.07MPa.Why concentration condition and concentrating degree are strictly controlled in step (2) of the present invention, because flavones product pole
Property it is smaller, the solubility in water is relatively low, if enrichment process concentration multiple flavones product higher will separate out, if concentration
Multiple is relatively low, and the carrying out of subsequent extracted technique is unfavorable for again.
Preferably, in the step (2), the Alcohol degree for starting to be reclaimed during concentration is higher, and the number of degrees for finally reclaiming are relatively low,
The alcohol that the number of degrees of recovery are high should be collected separately.
Preferably, in the step (3), the crude drug concentration of concentrate is 0.125g/ml；When being adsorbed to concentrate,
First eluted with the water of 6BV, then eluted with the ethanol solution that the volume fraction of 6BV is 80%.
Preferably, the step (3) is before absorption, also including by macroporous absorbent resin it is to be prepared the step of：
2.1750kg (1.2 cubes) resin fills post, post blade diameter length ratio about 1:5-8 (resin column of a diameter of 48cm, about height
It is 2.4m, column volume is 434L, needs 3 posts), can connect；
Resin regeneration step is as follows：
(1) by original water emptying in resin, then with the once washing post of 2BV, post water emptying will finally be washed.Control post 0.5
Hour.
(2) 4% 1200 liters of the NaOH aqueous solution is prepared, resin is completely soaked, is needed in immersion process always from bottom ventilation
Movable resin, soak time is 2 hours.Post is controlled after the completion of immersion, by buck emptying, then with 4% 1200 liters of the NaOH aqueous solution
Immersion one time, controls post after the completion of immersion, buck emptying is rushed to neutrality resin with a water.
(3) 4% 1200 liters of HCl/water solution is prepared, resin is completely soaked, needs to be lived from bottom ventilation always in immersion process
Dynamic resin, soak time is 2 hours, and resin is washed till neutrality by emptying sour water after the completion of immersion with a water afterwards.According to circumstances
Backwash can be carried out.
(4) must assure that resin lower prop water is neutrality before adsorbing.
It is worth noting that, macroporous absorbent resin in step (3) can for those skilled in the art generally commonly use it is big
Macroporous adsorbent resin, such as buy the LSA-10 model macroporous absorbent resins in Xi'an Sunresin New Materials Co., Ltd..
Preferably, in the step (4), desorbed solution is concentrated under reduced pressure, it is 1.15~1.20, solid content to obtain relative density
It is 20~25% concentrate.
Additionally, in the step (4), because concentrate can separate out active ingredient after de- taste, product is more sticky, is not suitable for
Using spray drying, and preferably use vacuum drying chamber and be vacuum dried, temperature≤70 DEG C are required in drying process, dry and dry
It is dry to carry out fully, to reduce the loss of isopentene group flavonoids.
Meanwhile, the present invention also provides a kind of isopentene group flavonoid extract prepared by above-mentioned preparation method, institute
State in extract, the weight/mass percentage composition of isopentene group flavonoid extract is more than 50%.
Preferably, in said extracted thing, the weight/mass percentage composition of sanggenon C is more than 6.4%, the quality percentage of Saliggenon D
Content is more than 3.4%.
Additionally, the present invention also provides a kind of above-mentioned isopentene group flavonoid extract in treatment NASH or subtracts
Application in fertilizer.
Relative to prior art, beneficial effects of the present invention are：
The isopentene group flavonoid extract prepared with preparation method of the present invention, its isopentene group flavonoids rate of transform
More than 90%, the content of isopentene group flavonoid extract is more than 50%, and favorable reproducibility in purified, and resin is repeatable to be made
With technological operation is easy, and preparation amount is big, and product purity is high, and low stain.
Brief description of the drawings
Fig. 1 is the liquid phase figure of the preparation-obtained isopentene group flavonoid extract sample of embodiment 1；
Fig. 2 is design sketch of the isopentene group flavonoid extract of the present invention in terms of NASH is treated；
Fig. 3 is design sketch of the isopentene group flavonoid extract of the present invention in terms of fat-reducing；
Fig. 4 is design sketch of the isopentene group flavonoid extract of the present invention to glucose tolerance；
Fig. 5 is design sketch of the isopentene group flavonoid extract of the present invention in terms of hypoglycemic；
Fig. 6 is design sketch of the isopentene group flavonoid extract of the present invention in terms of lipid-loweringing.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of embodiment of the preparation method of isopentene group flavonoid extract of the present invention, preparation described in the present embodiment
Method comprises the following steps：
(1) by dry root bark of white mulberry pulverizing medicinal materials, use volume fraction normal to root bark of white mulberry medicinal material for 80% ethanol solution
It is 1 according to the mass volume ratio of root bark of white mulberry medicinal material and ethanol solution after temperature immersion 4 hours:The ratio of 10g/ml, adds volume integral
Number is 80% ethanol solution, and refluxing extraction is carried out 1.5 hours to root bark of white mulberry medicinal material at 90 DEG C；According still further to root bark of white mulberry medicinal material and second
The mass volume ratio of alcoholic solution is 1:The ratio of 8g/ml, the ethanol solution for adding volume fraction to be 80%, enters to root bark of white mulberry medicinal material
Row refluxing extraction 1.5 hours, merges extract solution twice；Wherein, in root bark of white mulberry medicinal material, sanggenon C, Saliggenon D, the matter of moracin
Amount percentage composition is all higher than 0.1%, or the weight/mass percentage composition sum of sanggenon C, Saliggenon D, moracin is not less than 0.35%；
(2) step (1) gained is first extracted into liquid precipitate 1 hour, then by extract solution with 300 mesh filter plate circulating filtrations, so
Suction filtration afterwards, by smoke filtrate, 70 DEG C are concentrated under reduced pressure into crude drug concentration for 0.13g/ml, and the volume fraction of ethanol is 45%, is concentrated
Liquid；
(3) the LSA-10 models macroporous absorbent resin that will be bought in Xi'an Sunresin New Materials Co., Ltd. is carried out
After pretreatment regeneration, with the loading speed of 1BV/h, concentrate is adsorbed, then eluted with the water of 8BV, then with 6BV
Volume fraction be that 90% ethanol solution is eluted with the flow velocity of 1BV/h, untill being eluted to without flavones, collect eluent；
(4) 60 DEG C of eluent is concentrated under reduced pressure, it is the concentrate that 1.17, solid content is 23% to obtain relative density, true
Empty drying box is fully dried in 70 DEG C, obtains the isopentene group flavonoid extract.
Embodiment 2
A kind of embodiment of the preparation method of isopentene group flavonoid extract of the present invention, preparation described in the present embodiment
Method comprises the following steps：
(1) by dry root bark of white mulberry pulverizing medicinal materials, the ethanol solution that volume fraction is 80% is soaked into Sang Bai at 50 DEG C
After skin medicinal material 12 hours, with the ethanol solution that volume fraction is 80% temperature be 50 DEG C, flow velocity enters for 0.5 times of volume/hour
Row diacolation, collects percolate, and wherein in immersion process, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:4g/ml, oozes
During filtering, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:8g/ml；Wherein, in root bark of white mulberry medicinal material, sanggenon C,
Saliggenon D, the weight/mass percentage composition of moracin are all higher than 0.1%, or the quality percentage of sanggenon C, Saliggenon D, moracin contains
Amount sum is not less than 0.35%；
(2) step (1) gained is first extracted into liquid precipitate 1.5 hours, then by extract solution with 300 mesh filter plate circulating filtrations,
Then suction filtration, by smoke filtrate, 60 DEG C are concentrated under reduced pressure into crude drug concentration for 0.11g/ml, and the volume fraction of ethanol is 40%, obtains dense
Contracting liquid；
(3) the LSA-10 models macroporous absorbent resin that will be bought in Xi'an Sunresin New Materials Co., Ltd. is carried out
After pretreatment regeneration, with the loading speed of 1BV/h, concentrate is adsorbed, then eluted with the water of 4BV, then with 8BV
Volume fraction be that 70% ethanol solution is eluted with the flow velocity of 1.5BV/h, untill being eluted to without flavones, collect wash-out
Liquid；
(4) 60 DEG C of eluent is concentrated under reduced pressure, it is the concentrate that 1.20, solid content is 25% to obtain relative density, true
Empty drying box is fully dried in 70 DEG C, obtains the isopentene group flavonoid extract.
Embodiment 3
A kind of embodiment of the preparation method of isopentene group flavonoid extract of the present invention, preparation described in the present embodiment
Method comprises the following steps：
(1) it is first 1 according to the mass volume ratio of root bark of white mulberry medicinal material and ethanol solution by dry root bark of white mulberry pulverizing medicinal materials:
The ratio of 8g/ml, adds the ethanol solution that volume fraction is 60%, and 60 DEG C after root bark of white mulberry medicinal material soak at room temperature 3.5 hours are entered
Row refluxing extraction 2 hours；Mass volume ratio according still further to root bark of white mulberry medicinal material and ethanol solution is 1:The ratio of 6g/ml, adds body
Fraction is 60% ethanol solution, and refluxing extraction is carried out 1.5 hours to root bark of white mulberry medicinal material, merges extract solution twice, wherein, mulberry
In white skin medicinal material, sanggenon C, Saliggenon D, the weight/mass percentage composition of moracin are all higher than 0.1%, or sanggenon C, Saliggenon D,
The weight/mass percentage composition sum of moracin is not less than 0.35%；
(2) step (1) gained is first extracted into liquid precipitate 1 hour, then by extract solution with 300 mesh filter plate circulating filtrations, so
Suction filtration afterwards, by smoke filtrate, 70 DEG C are concentrated under reduced pressure into crude drug concentration for 0.125g/ml, and the volume fraction of ethanol is 30%, obtains dense
Contracting liquid；
(3) the LSA-10 models macroporous absorbent resin that will be bought in Xi'an Sunresin New Materials Co., Ltd. is carried out
After pretreatment regeneration, with the loading speed of 1BV/h, concentrate is adsorbed, then eluted with the water of 6BV, then with 6BV
Volume fraction be that 80% ethanol solution is eluted with the flow velocity of 1.5BV/h, untill being eluted to without flavones, collect wash-out
Liquid；
(4) 60 DEG C of eluent is concentrated under reduced pressure, it is the concentrate that 1.15, solid content is 20% to obtain relative density, true
Empty drying box is fully dried in 70 DEG C, obtains the isopentene group flavonoid extract.
Embodiment 4
A kind of embodiment of the preparation method of isopentene group flavonoid extract of the present invention, preparation described in the present embodiment
Method comprises the following steps：
(1) by dry root bark of white mulberry pulverizing medicinal materials, the ethanol solution that volume fraction is 60% is soaked into Sang Bai at 45 DEG C
After skin medicinal material 24 hours, with the ethanol solution that volume fraction is 80% temperature be 45 DEG C, flow velocity enters for 0.5 times of volume/hour
Row diacolation, collects percolate, and wherein in immersion process, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:4g/ml, oozes
During filtering, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:6g/ml；Wherein, in root bark of white mulberry medicinal material, sanggenon C,
Saliggenon D, the weight/mass percentage composition of moracin are all higher than 0.1%, or the quality percentage of sanggenon C, Saliggenon D, moracin contains
Amount sum is not less than 0.35%；
(2) step (1) gained is first extracted into liquid precipitate 1 hour, then by extract solution with 300 mesh filter plate circulating filtrations, so
Suction filtration afterwards, by smoke filtrate, 60 DEG C are concentrated under reduced pressure into crude drug concentration for 0.125g/ml, and the volume fraction of ethanol is 30%, obtains dense
Contracting liquid；
(3) the LSA-10 models macroporous absorbent resin that will be bought in Xi'an Sunresin New Materials Co., Ltd. is carried out
After pretreatment regeneration, with the loading speed of 1BV/h, concentrate is adsorbed, then eluted with the water of 4BV, then with 8BV
Volume fraction be that 70% ethanol solution is eluted with the flow velocity of 2BV/h, untill being eluted to without flavones, collect eluent；
(4) 60 DEG C of eluent is concentrated under reduced pressure, it is the concentrate that 1.19, solid content is 24% to obtain relative density, true
Empty drying box is fully dried in 70 DEG C, obtains the isopentene group flavonoid extract.
Embodiment 5
The present embodiment is carried out to the isopentene group Flavonoid Content in the preparation-obtained chromocor extract of embodiment 1~4
Liquid phase measurement, using instrument be the high performance liquid chromatograph of Waters companies 2695, the λ biabsorption detectors of Waters companies 2487,
Chromatographic condition is：Chromatographic column：Dikma Techonlogies (enlightening horse Diamonsil C185 μ, 200 × 4.6mm)；Mobile phase：
Acetonitrile -0.1% acetic acid water；Detection wavelength：283nm；Sample size：10μL；Detection wavelength：270nm；Column temperature：30℃；Flow velocity：
1.0mL/min；As shown in table 1, measurement result is as shown in Figure 1 (with made in embodiment 1 for mobile phase content in specific continuous mode
As a example by the measurement of the standby isopentene group flavonoids for obtaining), analysis result is as shown in table 2：
The mobile phase content of table 1
(this liquid-phase condition can just finish by 50 minutes, extend to 65 minutes be for continuous sample introduction)
The liquid-phase chromatographic analysis result of table 2
From the analysis result of table 2 can be seen that embodiment 1 in gained isopentene group flavonoid extract in Diels-
Alder compounds main component is 1~No. 4 peak, and total content is 45.74%, and isoamylene radical chromocor class is mainly No. 5 peaks, content
It is 11.45%, generally speaking, the total content of isopentene group flavonoids is 57.19%, more than 50%；It is made to embodiment 2~4
Isopentene group Flavonoid Content in the standby chromocor extract for obtaining has carried out liquid phase measurement, measurement result after the same method
Similar with the result in embodiment 1, generally speaking, the total content of isopentene group flavonoids is more than 50%, specific research
Process is no longer described in detail with this.
Embodiment 6
The present embodiment carries out investigation optimization to extractant solid-liquid ratio in extraction process.
Experimental procedure：Precision weighs each 3 parts of root bark of white mulberry medicinal powder 20g, is separately added into 6,8,10 times the 80% of amount of second
Alcoholic solution, 90 DEG C are extracted 1 time, extraction time 1.5h.6,8,10 times the 80% of amount of ethanol solution, 90 DEG C of extractions are separately added into again
1 time, extraction time 1.5h merges filtrate, suction filtration twice.Assay method according to isopentene group flavonoids in embodiment 5 is determined
Isopentene group Flavonoid Content, experimental data is as follows：
The solvent feed of table 3 is than optimization analyze data
By data above as can be seen that with the increase of solid-liquid ratio, the extraction yield of isopentene group flavonoids increases, first
Secondary extraction solid-liquid ratio is 1：10, it is 1 that second is extracted solid-liquid ratio：When 8, isopentene group Flavonoid Content highest, when more than the ratio
During example, concentration pressure is increased again, so it is 1 to extract solid-liquid ratio for the first time：10, it is 1 that second is extracted solid-liquid ratio：8.
Embodiment 7
The present embodiment carries out investigation optimization to extraction time in extraction process.
Experimental procedure：Precision weighs each 3 parts of root bark of white mulberry medicinal material 10g, adds the 80% ethanol solution extraction of 10 times of amounts and 8 times of amounts
Take 2 times, 90 DEG C of temperature, first time extraction time is respectively 2h, 2h, 1.5h, and second extraction time 2h, 1.5h, 1h merge two
Secondary filtrate, according to the assay method of isopentene group flavonoids in embodiment 5, determines isopentene group Flavonoid Content, experimental data
It is as follows：
The extraction time of table 4 optimizes analyze data
By data above as can be seen that being 1.5 hours in extraction time first time, second extraction time is 1.5 hours
When, isopentene group Flavonoid Content is maximum in extract solution.
Embodiment 8
The present embodiment carries out investigation optimization to the volume fraction of ethanol solution in extraction process.
Experimental procedure：Precision weighs each 4 parts of root bark of white mulberry medicinal material 10g, adds 10 times of amounts and the volume fraction of 8 times of amounts to be respectively
60%th, 70%, 80% ethanol solution, 90 DEG C are extracted 2 times, and each 1.5h merges filtrate twice, according to medicinal material assay
Method determines isopentene group Flavonoid Content, and experimental data is as follows：
The volume fraction optimization analyze data of the ethanol solution of table 5
By data above as can be seen that volumes of aqueous ethanol fraction be 80% when, isopentene group flavonoids in extract
Content is maximum, so the optimal volume fraction for extracting the ethanol solution of isopentene group flavonoids is 80%.
Embodiment 9
The present embodiment adsorbs optimal crude drug concentration and carries out investigation optimization to resin upper prop in extraction process.
Experimental procedure：Precision weighs tri- parts of root bark of white mulberry medicinal material 100g, adds the 80% ethanol solution extraction of 10 times of amounts and 8 times of amounts
Take 2 times, 90 DEG C of temperature, extraction time is 1.5h, using 300 mesh filter-cloth filterings, merge filtrate twice, suction filtration is mixed, measured
Volume, isopentene group Flavonoid Content is determined according to medicinal material assay method, crude drug concentration is concentrated into afterwards and is respectively
0.13g/ml, 0.125g/ml, 0.111g/ml, are adsorbed using macroporous absorbent resin, are washed using 8BV, and 6BV is used afterwards
80% ethanol solution is parsed, and measures desorbed solution volume, and detection wherein isopentene group Flavonoid Content calculates yield.It is real
Test data as follows：
The resin upper prop of table 6 adsorbs optimal crude drug concentration optimization analyze data
From data above, when upper prop adsorption liquid concentration is 0.125g/ml, resin concentration effect is best.
Embodiment 10
The present embodiment carries out investigation optimization to the most preferably washing amount of resin in extraction process.
Experimental procedure：Precision weighs root bark of white mulberry medicinal material 100g, adds the 80% ethanol solution extraction 2 of 10 times of amounts and 8 times of amounts
It is secondary, 90 DEG C of temperature, extraction time is 1.5h, using 300 mesh filter-cloth filterings, merges filtrate twice, and suction filtration is mixed, and measures body
Product, isopentene group Flavonoid Content is determined according to medicinal material assay method, crude drug concentration is concentrated into afterwards and is respectively
0.125g/ml, is adsorbed using macroporous absorbent resin, is washed using 8BV, during not every 1BV using molish react inspection
Whether survey in a lower prop water has sugared presence.
Experiment conclusion：Sugared presence is detected whether every 1BV during, has been drawn when being washed using 4BV, can be by sugar
Wash, to ensure that by the sugared determination washing column volume that all washes away be 6BV.
Embodiment 11
The present embodiment carries out investigation optimization to the optimal eluate concentration of resin in extraction process.
Experimental procedure：Precision weighs tri- parts of root bark of white mulberry medicinal material 100g, adds the 80% ethanol solution extraction of 10 times of amounts and 8 times of amounts
Take 2 times, 90 DEG C of temperature, extraction time is 1.5h, using 300 mesh filter-cloth filterings, merge filtrate twice, suction filtration is mixed, measured
Volume, isopentene group Flavonoid Content is determined according to medicinal material assay method, crude drug concentration is concentrated into afterwards and is respectively
0.125g/ml, is adsorbed using macroporous absorbent resin, is washed using 6BV, and the ethanol of 6BV 70%, 80%, 90% is used afterwards
Solution is parsed, and measures desorbed solution volume, and detection wherein isopentene group Flavonoid Content calculates yield, and experimental data is as follows：
The optimal desorbed solution concentration optimization analyze data of the resin of table 7
Experiment conclusion：From data above, when the desorbed solution number of degrees are 80%, the isopentene group flavonoids rate of transform compared with
It is high.
Embodiment 12
The present embodiment carries out investigation optimization to the optimal elution amount of resin in extraction process.
Experimental procedure：Precision weighs tri- parts of root bark of white mulberry medicinal material 100g, adds the 80% ethanol solution extraction of 10 times of amounts and 8 times of amounts
Take 2 times, 90 DEG C of temperature, extraction time is respectively 1.5h, using 300 mesh filter-cloth filterings, merge filtrate twice, suction filtration is mixed, amount
Volume is taken, isopentene group Flavonoid Content is determined according to medicinal material assay method, crude drug concentration is concentrated into afterwards and is respectively
0.125g/ml, is adsorbed using macroporous absorbent resin, is washed using 6BV, after respectively using 5BV, 5.5BV, 6BV 80%
Ethanol solution is parsed, and measures desorbed solution volume, and detection wherein isopentene group Flavonoid Content calculates yield, experimental data
It is as follows：
The resin of table 8 most preferably parsing amount optimization analyze data
Experiment conclusion：From data above, when desorbed solution volume is 6BV, the isopentene group flavonoids rate of transform is higher.
Embodiment 13
The present embodiment researchs and analyses isopentene group flavonoid extract of the present invention and is treating non-alcohol by taking embodiment 1 as an example
Property fatty liver or fat-reducing in application effect, result of study respectively as figures 2-6.
(1) effect disquisition of the isopentene group flavonoid extract of the present invention in NASH is treated
Specific experiment process is：After 80 SD male rats (body weight is 180-220g) adaptability are fed 1 week, it is randomly divided into
4 groups, every group 20, administration group (treatment), administration group (prevention), Normal group, model group are set as follows respectively,
After 3 months, take every group of liver of rat, and measure its liver weight, average, every group of liver weight situation of rat as shown in Fig. 2
High lipid food during nursing press weight/mass percentage composition by 12% lard, 48% basal feed, 15% sugar, 10% peanut,
10% yolk, 5% salt and 0.03% Pig cholate are made：
Isopentene group flavonoid extract administration group (treatment)：Therapeutic, (treatment group is high fat diet 7 weeks within 3 months
Start administration again afterwards)；
Isopentene group flavonoid extract administration group (prevention)：Preventive administration, (prevention group is side high lipid food within 3 months
Feed side administration)；
Normal group：SD male rats；
Model group：Pure high lipid food is fed；
Found in research process, in addition to the weight of liver has significant difference, the heart of each group rat, spleen, lung, kidney, skeletal muscle,
Femur, shin bone, palm fibre it is white than etc. there are no significant difference.Figure it is seen that compared with model group liver weight, iso-amylene base class
Chromocor extract administration group, either prevention group or treatment group can effectively control liver weight, improve fatty liver, especially prevent
Group is better, is almost as good as with normal rats difference.
(2) effect disquisition of the isopentene group flavonoid extract of the present invention in fat-reducing
Specific experiment process is：After 80 SD male rats (body weight is 180-220g) adaptability are fed 1 week, it is randomly divided into
4 groups, every group 20, administration group (treatment), administration group (prevention), Normal group, model group are set as follows respectively,
Every group of body weight of rat of periodic measurement, averages, and the body weight of every group of rat changes over time curve as shown in figure 3, feeding
High lipid food in journey press weight/mass percentage composition by 12% lard, 48% basal feed, 15% sugar, 10% peanut, 10% yolk,
5% salt and 0.03% Pig cholate are made：
Isopentene group flavonoid extract administration group (treatment)：Therapeutic, (treatment group is high fat diet 7 weeks within 3 months
Start administration again afterwards)；
Isopentene group flavonoid extract administration group (prevention)：Preventive administration, (prevention group is side high lipid food within 3 months
Feed side administration)；
Normal group：SD male rats；
Model group：Pure high lipid food is fed；
From figure 3, it can be seen that compared with model group body weight, the increasing of the obvious control body weight of active component (prevention) administration group energy
It is long.Isopentene group flavonoid extract administration group, either prevention group or treatment group can effective control body weight, especially in advance
Anti- group better, is almost as good as with normal rats difference, and treatment group is then after being administered, to allow rat body weight gradually to mitigate.
(3) effect disquisition of the isopentene group flavonoid extract of the present invention in hypoglycemic
Specific experiment process is：After 80 SD male rats (body weight is 180-220g) adaptability are fed 1 week, it is randomly divided into
4 groups, every group 20, administration group (treatment), administration group (prevention), Normal group, model group are set as follows respectively,
Every group of blood glucose value of rat of periodic measurement, is averaged, and oral glucose tolerance test (OGTT) is carried out to rat, and every group big
The blood glucose value of mouse changes over time curve as shown in Figures 4 and 5, and the high lipid food during nursing presses weight/mass percentage composition by 12%
Lard, 48% basal feed, 15% sugar, 10% peanut, 10% yolk, 5% salt and 0.03% Pig cholate are made：
Isopentene group flavonoid extract administration group (treatment)：Therapeutic, (treatment group is high fat diet 7 weeks within 3 months
Start administration again afterwards)；
Isopentene group flavonoid extract administration group (prevention)：Preventive administration, (prevention group is side high lipid food within 3 months
Feed side administration)；
Normal group：SD male rats；
Model group：Pure high lipid food is fed；
From fig. 4, it can be seen that root bark of white mulberry administration group (treatment) can significantly improve the tolerance to glucose；Can from Fig. 5
To find out, compared with model group, root bark of white mulberry administration group plays the role of significantly hypoglycemic.
(4) effect disquisition of the isopentene group flavonoid extract of the present invention in lipid-loweringing
Specific experiment process is：After 80 SD male rats (body weight is 180-220g) adaptability are fed 1 week, it is randomly divided into
4 groups, every group 20, administration group (treatment), administration group (prevention), Normal group, model group are set as follows respectively,
The kidney circumferential portion of rat is extractd after feeding 3 months, and weighs the weight of perirenal fat, averaged, every group of kidney week fat of rat
Fat weight change over time curve as shown in fig. 6, feed during high lipid food by weight/mass percentage composition by 12% lard,
48% basal feed, 15% sugar, 10% peanut, 10% yolk, 5% salt and 0.03% Pig cholate are made：
Isopentene group flavonoid extract administration group (treatment)：Therapeutic, (treatment group is high fat diet 7 weeks within 3 months
Start administration again afterwards)；
Isopentene group flavonoid extract administration group (prevention)：Preventive administration, (prevention group is side high lipid food within 3 months
Feed side administration)；
Normal group：SD male rats；
Model group：Pure high lipid food is fed；
From fig. 6, it can be seen that compared with model group perirenal fat amount, isopentene group flavonoid extract administration group, no matter
It is that prevention group or treatment group can effectively reduce perirenal fat, is almost as good as with normal rats difference.
It is last to should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope is protected, although being explained in detail to the present invention with reference to preferred embodiment, one of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent, without deviating from the essence of technical solution of the present invention
And scope.
Claims (10)
1. a kind of preparation method of isopentene group flavonoid extract, it is characterised in that methods described comprises the following steps：
(1) by dry root bark of white mulberry pulverizing medicinal materials, using alcohol solution dipping 3.5~4 hours after, at 60~90 DEG C, backflow
Extract twice, 1.5~2 hours every time, merge extract solution, wherein, root bark of white mulberry medicinal material and ethanol solution in each refluxing extraction
Mass volume ratio is (1:6~1:10)g/ml；
Or ethanol solution is soaked into root bark of white mulberry medicinal material after 12~24 hours at 45~50 DEG C, constant temperature constant speed carries out diacolation, collects
Percolate, obtains extract solution, wherein, root bark of white mulberry medicinal material is (1 with the mass volume ratio of ethanol solution:4~1:8)g/ml；
Wherein, in root bark of white mulberry medicinal material, sanggenon C, Saliggenon D, the weight/mass percentage composition of moracin are all higher than 0.1%, or mulberry root
Ketone C, Saliggenon D, the weight/mass percentage composition sum of moracin are not less than 0.35%, and the volume fraction of ethanol is 60 in ethanol solution
~80%；
(2) step (1) gained extract solution filtered, be concentrated under reduced pressure into crude drug concentration for 0.11~0.13g/ml, the volume of ethanol
Fraction is 30~45%, obtains concentrate；
(3) concentrate is adsorbed using macroporous absorbent resin, is then eluted with the water of 4BV~8BV, elution speed is
1.5BV/h, then eluted with the flow velocity of 1~2BV/h with the ethanol solution that the volume fraction of 6BV~8BV is 70%~90%,
Collect eluent；
(4) it is eluent is concentrated under reduced pressure, dry, obtain the isopentene group flavonoid extract.
2. the preparation method of isopentene group flavonoid extract as claimed in claim 1, it is characterised in that the step (1)
In, it is 1 according to the mass volume ratio of root bark of white mulberry medicinal material and ethanol solution:The ratio of 10g/ml, it is 80% to add volume fraction
Ethanol solution, refluxing extraction is carried out 1.5 hours to root bark of white mulberry medicinal material；According still further to root bark of white mulberry medicinal material and the quality volume of ethanol solution
Than being 1:The ratio of 8g/ml, the ethanol solution for adding volume fraction to be 80%, carries out refluxing extraction 1.5 small to root bark of white mulberry medicinal material
When, merge extract solution twice.
3. the preparation method of isopentene group flavonoid extract as claimed in claim 1, it is characterised in that the step (1)
In, it is 80% with volume fraction after at 50 DEG C the ethanol solution that volume fraction is 80% is soaked into root bark of white mulberry medicinal material 12 hours
Ethanol solution temperature be 50 DEG C, flow velocity be 0.5 times of volume/hour to carry out diacolation, collection percolate, wherein immersion process
In, root bark of white mulberry medicinal material is 1 with the mass volume ratio of ethanol solution:4g/ml, during diacolation, root bark of white mulberry medicinal material and ethanol solution
Mass volume ratio be 1:8g/ml.
4. the preparation method of isopentene group flavonoid extract as claimed in claim 1, it is characterised in that the step (2)
In, it is the step of extract solution is filtered：To first liquid precipitate be extracted more than 1 hour, then extract solution will be circulated throughout with 300 mesh filter plates
Filter.
5. the preparation method of isopentene group flavonoid extract as claimed in claim 1, it is characterised in that the step (3)
In, the crude drug concentration of the concentrate is 0.125g/ml；When being adsorbed to concentrate, first eluted with the water of 6BV,
Eluted with the ethanol solution that the volume fraction of 6BV is 80% again.
6. the preparation method of isopentene group flavonoid extract as claimed in claim 1, it is characterised in that the step (4)
In, eluent is concentrated under reduced pressure, it is the concentrate that 1.15~1.20, solid content is 20~25% to obtain relative density.
7. the isopentene group flavonoid extract that a kind of preparation method as described in any one of claim 1~6 is prepared.
8. isopentene group flavonoid extract as claimed in claim 7, it is characterised in that in the extract, isopentene group
The weight/mass percentage composition of flavonoids is more than 50%.
9. isopentene group flavonoid extract as claimed in claim 7, it is characterised in that in the extract, sanggenon C
Weight/mass percentage composition is more than 6.4%, and the weight/mass percentage composition of Saliggenon D is more than 3.4%.
10. isopentene group flavonoid extract is treating NASH, fat-reducing as described in any one of claim 7~9
Or the application in hypoglycemic.
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| CN108703966A (en) * | 2018-07-26 | 2018-10-26 | 大连天星本草生物科技有限公司 | A kind of application of Saliggenon D in the drug or pharmaceutical composition for preparing treatment hyperlipidemia and/or obesity |
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