CN104784231B - A kind of method that flavone aglycone is obtained from gen-seng haulms - Google Patents
A kind of method that flavone aglycone is obtained from gen-seng haulms Download PDFInfo
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Abstract
The present invention relates to a kind of method that flavone aglycone is prepared from gen-seng haulms, this method comprises the following steps：By ultrasonic extraction gen-seng haulms general flavone crude extract the step of, prepare the step of gen-seng haulms general flavone crude extract solution, the flavone glycoside in the gen-seng haulms general flavone crude extract solution be converted into the step of converting of flavone aglycone, drying steps.By the method that flavone aglycone is prepared from gen-seng haulms of the present invention, its operating procedure is simple, the time is short, cost is low, high conversion rate, is adapted to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of Hemodynamics aglycon, specifically, that is, utilizes hydrochloric acid method for hydrolysis
The method that flavone aglycone is obtained from gen-seng haulms.The present invention is the preparation method on effective component of chinese medicine, and in particular to from
The method that flavone aglycone is prepared in gen-seng haulms.
Background technology
Ginseng (Panax ginseng C.A.Meyer) is Araliaceae (Araliaceae) Panax (Panax) plant person
The root of ginseng, it is rare Chinese medicine.For physically weak custom is de-, cold weak pulse of limb, the deficiency syndrome of the lung are breathed with cough, insomnia of palpitating with fear, neurasthenia, tired mind and
Various qi-blood-body fluid deficiency diseases.Ancient medicine books《Sheng Nong's herbal classic》The ginseng medicinal effects of record are mainly underground part
Divide, i.e. the root and palpus of ginseng.Modern study deepens continuously at any time, is that the research of flower, fruit, cauline leaf etc. is got over to ginseng aerial part
Come more.Also, it was found that the composition of the effect of in ginseng aerial part contains and under ground portion identical functional component, some compositions
Content it is higher than under ground portion.Saponins, flavonoids, organic acid, volatile oil are obtained from gen-seng haulms part at present
Class, polysaccharide etc..But present gen-seng haulms largely go out of use in addition to ginsenoside extraction is used on a small quantity.It is yellow to gen-seng haulms
The further investigation of ketone also just started in recent years.
Flavone compound is the secondary metabolite being widely present in plant, combines to form flavone glycoside with sugar more,
Only only a few exists in the form of aglycon.Flavone compound has many bioactive functions, including anti-oxidant, anti-
Cancer, anti-hypertension and antibacterial activity etc..With going deep into its physiological and biochemical research, it is found that flavone aglycone has than flavone glycoside
Higher biological value, flavone aglycone are directly absorbed in small intestine, and glucoside type is acted on by microorganism in colon etc. to hydrolyze,
Further absorbed after degraded generation aglycon by colon wall.Therefore, production flavone aglycone has even more important meaning.Structural formula
It is as follows：
The A of Chinese patent CN 101768613 disclose the production method that flavone aglycone is extracted in a kind of Leaves of Hippophae L, this method
Aglycon mainly is prepared using microorganism conversion, conversion ratio is 14%~23%.Although microbial method reaction condition is gentle, can be most
The destruction of composition in limits protection raw material, but conversion reaction time length, and screen superior strain is one huge
Engineering, the shortcomings that also conversion ratio is low.
The A of Chinese patent CN 103142685 disclose a kind of extracting method of total-flavonoid aglycone in Hickory Leaves, this method
Mainly extracted using ethanol, recycle polyamide to handle to obtain the flavone aglycone of purity 87.47%.
At present, there is not yet the research for being converted into flavone aglycone through hydrochloric acid hydrolysis on Hemodynamics glucosides is reported.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Hemodynamics aglycon.Ginseng is prepared using chemical method
Cauline leaf flavone aglycone, so as to improve the content of flavone aglycone in the physiologically active of Hemodynamics and final products.The present invention
Converted using chemical method, i.e., flavone glycoside in gen-seng haulms is converted using hydrochloric acid, ultimately produce Kaempferol, quercitrin
The flavone aglycone such as element and Isorhamnetin.The operating procedure of this method is simple, and the time is short, and cost is low, high conversion rate, is adapted to industry
Metaplasia is produced.
It is an object of the invention to provide a kind of method that flavone aglycone is prepared from gen-seng haulms, this method includes following
Step：By ultrasonic extraction gen-seng haulms general flavone crude extract the step of, prepare gen-seng haulms general flavone crude extract solution
The step of, the flavone glycoside in the gen-seng haulms general flavone crude extract solution is converted into by flavone aglycone by Hydrochloric Acid Hydrolysis Method
Step of converting, drying steps.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, passes through ultrasonic extraction ginseng stem-leaf total
In the step of flavones crude extract, concentration of alcohol is selected from 20%~100% scope.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, passes through ultrasonic extraction ginseng stem-leaf total
In the step of flavones crude extract, the ultrasonic extraction time is selected from the scope of 10~50 minutes.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, passes through ultrasonic extraction ginseng stem-leaf total
In the step of flavones crude extract, ultrasonic extraction temperature can be selected from 40~80 DEG C of scope.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, passes through ultrasonic extraction ginseng stem-leaf total
In the step of flavones crude extract, ultrasonic extraction power is selected from 200~400W scope.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, passes through ultrasonic extraction ginseng stem-leaf total
In the step of flavones crude extract, solid-liquid ratio is selected from 1:10~1:50 scope.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, preparing gen-seng haulms general flavone crude extract
In the step of solution, above-mentioned gen-seng haulms general flavone crude extract is made into alcoholic solution using low molecule alcohol compound.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, by above-mentioned gen-seng haulms general flavone crude extract
Alcoholic solution is made into using methanol.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, by Hydrochloric Acid Hydrolysis Method by the ginseng stem
Flavone glycoside in leaf flavonoids crude extract solution is converted into the step of converting of flavone aglycone.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, gen-seng haulms Huang is prepared in Hydrochloric Acid Hydrolysis Method
In the step of ketoside member, hydrolysis time is selected from the scope of 1~6 hour.
The method of the present invention that flavone aglycone is prepared from gen-seng haulms, gen-seng haulms Huang is prepared in Hydrochloric Acid Hydrolysis Method
In the step of ketoside member, concentration of hydrochloric acid is selected from 1mol/L~6mol/L scope.
By the method that flavone aglycone is prepared from gen-seng haulms of the present invention, its operating procedure is simple, the time is short, cost
Low, high conversion rate, it is adapted to industrialized production.During the utilization of natural active matter, often poorly efficient composition therein is turned
Turn to efficient composition.And chemical hydrochloric acid method is suitable for small molecule natural component, technique is simple, and the time is short, and cost is low, conversion ratio
Height, it is adapted to industrialized production.Through concentrating on studies for many years, the preparation of Panasenoside's member is carried out using gen-seng haulms.So that
It is primary raw material with the gen-seng haulms to go out of use, Hemodynamics glycoside hydrolysis is converted into flavonoid glycoside using Hydrochloric Acid Hydrolysis Method
Member, and raw material sources enrich.
Brief description of the drawings
Fig. 1 is 4 kinds of flavones monomer mixed sample HPLC chromatograms, by peak sequence according to for rutin, Quercetin, Kaempferol,
Isorhamnetin；
Fig. 2 is the HPLC chromatogram of sample liquid before hydrochloric acid hydrolysis；
Fig. 3 is the HPLC chromatogram of sample liquid after hydrochloric acid hydrolysis.
Embodiment
Below, the accompanying drawing in the embodiment of the present invention will be combined, the technical scheme in the embodiment of the present invention will be carried out in detail
Description, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on this hair
Embodiment in bright, the every other reality that those of ordinary skill in the art are obtained on the premise of creative work is not made
Example is applied, belongs to the scope of protection of the invention.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
And also include the other element being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Fig. 1 is four kinds of flavones monomer mixed sample HPLC chromatograms, by peak sequence according to for rutin, Quercetin, Kaempferol,
Isorhamnetin；Fig. 2 is the HPLC chromatogram of sample liquid before hydrochloric acid hydrolysis；Fig. 3 is the HPLC chromatogram of sample liquid after hydrochloric acid hydrolysis
Figure.Contain abundant rutin, a small amount of Kaempferol in gen-seng haulms it can be seen from Fig. 2,3 chromatograms；It is several after hydrochloric acid hydrolyzes
Kaempferol is completely converted into, also a small amount of Quercetin and Isorhamnetin.
In the present invention, the method that flavone aglycone is obtained from gen-seng haulms, it comprises the following steps：Gen-seng haulms are entered
Row is dried, after crushing, is soaked the stipulated time with determined solid-liquid ratio, is recycled ultrasonic technique to be extracted, filter, concentrate, oil
Ether obtains gen-seng haulms general flavone crude extract after decolourizing；Secondly, by gen-seng haulms general flavone crude extract with methanol be made into regulation it is dense
The solution of degree；Hydrochloric acid solution is added in above-mentioned solution with defined volume ratio, hydrolyzed under certain condition；Hydrolyzate is depressurized
Concentrate as medicinal extract；Drying process.
In the present invention, gen-seng haulms use the identified gen-seng haulms of county of Wangqing production；Rutin uses China
Pharmaceutical biological product calibrating is provided；Absolute ethyl alcohol, natrium nitrosum, aluminum nitrate, sodium hydroxide etc. are pure using domestic analysis.
(1) gen-seng haulms general flavone crude extract is prepared
Gen-seng haulms are dried, crushed and certain time is soaked with regulation solid-liquid ratio after 20 mesh sieves, utilize ultrasonic skill
Art is extracted, then obtains gen-seng haulms general flavone crude extract by filtering, concentrate, after petroleum ether decolouring.Using ultrasonic assistant,
Carried by the research of concentration of alcohol, ultrasonic extraction time, ultrasonic extraction temperature, ultrasonic extraction power and solid-liquid ratio from gen-seng haulms
Take general flavone.
In the step of gen-seng haulms general flavone crude extract, influence of the concentration of alcohol to general flavone content is further studied,
Specifically, gen-seng haulms powder 1Kg, solid-liquid ratio 1 are accurately weighed:20,20min is soaked, with ultrasonic extraction power 200W, is surpassed
20min is extracted under the conditions of 60 DEG C of sound Extracting temperature, investigates the influence to gen-seng haulms general flavone content under different ethanol concentration.
In the present invention, concentration of alcohol can select 20%~100% scope, preferably 40%~100% scope,
Most preferably 80%.With the increase of concentration of alcohol, gen-seng haulms general flavone content is in rising trend；Concentration of alcohol reaches 80%
When general flavone content substantially achieve peak, be further added by concentration of alcohol, general flavone content change is little.When concentration of alcohol exceedes
In the case of 80%, with the increase of concentration, the color of extract solution gradually becomes the low polar impurity such as bottle green, chlorophyll molten
Content in agent is continuously increased, and influences subsequent purification process, therefore not preferred.
In the step of gen-seng haulms general flavone crude extract, shadow of the ultrasonic extraction time to general flavone content is further studied
Ring, specifically, accurately weigh gen-seng haulms 1Kg, 80% concentration of alcohol is solvent, solid-liquid ratio 1:20,20min is soaked, with super
Investigated under the conditions of sound extraction power 200W, ultrasonic extraction temperature 60 C different ultrasonic extraction times (10,20,30,40,50min)
Influence to gen-seng haulms general flavone content.
In the present invention, extraction time can be selected from the scope of 10~50 minutes, preferably 20~50 minutes, be more preferably
40 minutes, with the increase of extraction time, general flavone content was in rising trend, when the ultrasonic extraction time is 40 minutes, general flavone
Content highest；Continue to increase extraction time, general flavone content declines on the contrary.
In the step of gen-seng haulms general flavone crude extract, shadow of the ultrasonic extraction temperature to flavones content is further studied
Ring, i.e. accurate to weigh gen-seng haulms powder 1Kg, 80% concentration of alcohol is solvent, solid-liquid ratio 1:20,20min is soaked, with super
20min is extracted under the conditions of sound extraction power 200W, investigates different ultrasonic extraction temperature (40,50,60,70,80 DEG C) to ginseng stem
The influence of leaf flavonoids content.
In the present invention, ultrasonic extraction temperature can be selected from the scope of 40~80 DEG C of scope, preferably 60~80 DEG C, with
The rising of ultrasonic extraction temperature, general flavone content is also in rising trend；In the case of more than 60 DEG C, general flavone content rises
Trend unobvious.Therefore, ultrasonic extraction temperature is set as 60 DEG C.
In the step of gen-seng haulms general flavone crude extract, shadow of the ultrasonic extraction power to flavones content is further studied
Ring, i.e. accurate to weigh gen-seng haulms powder 1Kg, 80% concentration of alcohol is solvent, solid-liquid ratio 1:20, soak 20min, 60 DEG C
Under the conditions of, 20min is extracted, investigates different ultrasonic extraction power 200,250,300,350,400W to gen-seng haulms general flavone content
Influence.
In the present invention, ultrasonic extraction power is selected from 200~400W scope, preferably 300~400W scope, more preferably
For 350W.With the increase of ultrasonic extraction power, general flavone content also increases, and reaches maximum when power reaches 350W, then
Decline again.
In the step of gen-seng haulms general flavone crude extract, influence of the solid-liquid ratio to general flavone content is further studied, i.e.
Gen-seng haulms powder 1Kg accurately is weighed, 80% concentration of alcohol is solvent, with different feed liquid ratio (1:10、1:20、1:30、1:40、
1:50) 20min is soaked, 20min is extracted under the conditions of power 200W, 60 DEG C, different feed liquid is investigated and compares gen-seng haulms general flavone
The influence of content.In the present invention, liquid ratio can be selected from 1:10~1:50 scope, preferably 1:10~1:30 scope,
More preferably 1:20.When solid-liquid ratio is 1:When 20, general flavone content reaches highest.
(2) gen-seng haulms general flavone crude extract solution is prepared
In the step of preparing gen-seng haulms general flavone crude extract solution, above-mentioned gen-seng haulms general flavone crude extract is used
Low molecule alcohol compound is made into 15mg/mL solution, and it is 1~4 that the low molecule alcohol compound, which can be selected from carbon number,
Any one above compound in low molecule alcohol compound, but preferably use methanol.
(3) Hydrochloric Acid Hydrolysis Method prepares Hemodynamics aglycon
Gen-seng haulms general flavone crude extract is made into 15mg/mL solution with methanol；Solution is put into closed hydrolysis pipe, added
Enter hydrochloric acid solution, constant temperature hydrolysis.
In the step of Hydrochloric Acid Hydrolysis Method prepares Hemodynamics aglycon, hydrolysis time can select 1~6h, be preferably
3~6h.With the extension of time, three kinds of Aglycones contents rise in hydrolyzate；The content highest when the time reaching 3h；Then slightly
Decline, but change less, illustrate that hydrolytic process is basically completed during 3h.
In addition, in the step of Hydrochloric Acid Hydrolysis Method prepares Hemodynamics aglycon, hydrolysis temperature can select 40~80
DEG C scope, preferably 60 DEG C.With the rising of temperature, three kinds of Aglycones contents occur what is risen, decline and rise in hydrolyzate
Change；The content highest when temperature reaches 60 DEG C, therefore it is preferred that.
In the step of Hydrochloric Acid Hydrolysis Method prepares Hemodynamics aglycon, concentration of hydrochloric acid can select 1mol/L~
6mol/L, preferably 2mol/L~6mol/L, with the increase of concentration of hydrochloric acid, three kinds of Aglycones contents also increase in hydrolyzate；But
After when concentration is 2mol/L, content reaches highest, change is little；Continuing, which increases content, begins to decline.It is probably because strong acid bar
Under part, not only glycosidic bond is broken, and aglycon can also be decomposed.
(4) hydrolyzate is concentrated under reduced pressure as medicinal extract；Drying process.
Embodiment 1
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 2mol/L hydrochloric acid solutions is added, is placed in 60 DEG C of waters bath with thermostatic control
Middle hydrolysis 3h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 6.08%, conversion ratio 95.89%.
Embodiment 2
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 4mol/L hydrochloric acid solutions is added, is placed in 50 DEG C of waters bath with thermostatic control
Middle hydrolysis 3h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 5.54%, conversion ratio 95.48%.
Embodiment 3
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 4mol/L hydrochloric acid solutions is added, is placed in 70 DEG C of waters bath with thermostatic control
Middle hydrolysis 4h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 5.58%, conversion ratio 95.53%.
Embodiment 4
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 2mol/L hydrochloric acid solutions is added, is placed in 50 DEG C of waters bath with thermostatic control
Middle hydrolysis 5h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 4.49%, conversion ratio 94.43%.
Embodiment 5
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 4mol/L hydrochloric acid solutions is added, is placed in 60 DEG C of waters bath with thermostatic control
Middle hydrolysis 4h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 6.02%, conversion ratio 95.85%.
Embodiment 6
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 3mol/L hydrochloric acid solutions is added, is placed in 60 DEG C of waters bath with thermostatic control
Middle hydrolysis 5h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 5.95%, conversion ratio 95.79%.
Embodiment 7
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 3mol/L hydrochloric acid solutions is added, is placed in 70 DEG C of waters bath with thermostatic control
Middle hydrolysis 3h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 6.24%, conversion ratio 96.00%.
Embodiment 8
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 3mol/L hydrochloric acid solutions is added, is placed in 50 DEG C of waters bath with thermostatic control
Middle hydrolysis 4h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 4.83%, conversion ratio 94.82%.
Embodiment 9
Weigh the powder after 1Kg gen-seng haulms drying and crushings；Add the 20L EtOH Sonicate ripple of volume fraction 67% extraction
50min, concentrated after filtering, decolourize to obtain gen-seng haulms general flavone crude extract three times using 3 times of volume petroleum ethers；Methanol is added to be made into
15mg/mL solution；Solution is put into closed hydrolysis pipe, 1/4 volume 2mol/L hydrochloric acid solutions is added, is placed in 70 DEG C of waters bath with thermostatic control
Middle hydrolysis 5h；It is concentrated under reduced pressure as medicinal extract；Drying process, Hemodynamics aglycon is obtained, with Quercetin, Kaempferol, Isorhamnetin
Meter, Aglycones content 6.16%, conversion ratio 95.95%.
The drafting of test example 1, standard curve
120 DEG C of rutin standard items 5mg dried to constant weight are dissolved with 70% ethanol and are settled to 25mL, being made into concentration is
0.20mg/mL standard liquids.Accurate absorption standard liquid 0,0.2,0.4,0.6,0.8,1.0mL are respectively placed in 10mL test tubes,
2mL is supplemented to 70% ethanol, adds 5% NaNO2Solution 0.3mL, 6min is stood after shaking up, then add 10%Al (NO3)3
Solution 0.3mL, shake up and stand 6min, finally add 4%NaOH solution 2mL, shake up to stand 10min and determine after 510nm wavelength and inhale
Luminosity A.Using rutin quality as abscissa, absorbance A is that ordinate carries out linear regression, obtains equation：Y=0.003x+0.0039,
R2=0.9999.Determination of Total Flavonoids and content are calculated as follows：
It is accurate to draw extract solution 0.2mL, add 70% ethanol and mend to 2mL, inhaled by standard curve preparation manipulation step measurements
Luminosity.The general flavone content represented with rutin is drawn by standard curve.
In formula：X is to calculate rutin content, μ g according to standard curve；
V is prepare liquid constant volume cumulative volume, mL；
V0To determine the volume of absorbance sample liquid, mL；
M is gen-seng haulms quality, g.
Further the present invention program is illustrated in conjunction with specific embodiments, but they are not limitation of the invention.
Test example 2, make standard curve
1) using four kinds of rutin, Quercetin, Kaempferol, Isorhamnetin monomeric compounds as standard items, it is made into respectively with methanol
0.2mg/mL standard liquids；Each 1mL that draws is made into mixed standard solution；0.45um micro-pore-film filtrations are utilized after mixing, with sample introduction
Volume 5,10,15,20uL make HPLC analyses, and sample size is returned with peak area, obtains standard curve.
2) HPLC chromatogram condition：Inertsustain C18Chromatographic column (4.6mm × 150mm, 5um).Mobile phase is acetonitrile
(A) -0.4% phosphoric acid water (B) gradient elution, 0~10min (10%~20%A), 10~30min (20%~40%A), 30~
40min (40%~10%A), 40~55min (10%A)；Column temperature is 40 DEG C, sample size 10uL；Detection wavelength 360nm；Flow velocity
0.8mL/min。
3) result such as table 1：
The retention time of four kinds of monomeric compounds, standard curve, R2And the range of linearity is shown in Table 1.
1. 4 kinds of flavones standard curves of table
By the present invention, raw material is more, preparation method is simple, high conversion rate, is more than 95%.Small molecule naturally into
Point, technique is simple, and the time is short, and cost is low, high conversion rate, is adapted to industrialized production.Ultrasonic technique can accelerate the broken of cell,
Be advantageous to the dissolution of active ingredient.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using the present invention.
Any those skilled in the art the invention discloses technical scope in, various repair can be made to the present embodiment easily
Change, and principle described herein is applied to other examples and applied without by creative work.Therefore, the invention is not restricted to this
In embodiment, do not depart from scope make improvement and modification should all be included within the scope of the present invention.
Claims (11)
1. a kind of method that flavone aglycone is prepared from gen-seng haulms, this method comprise the following steps：By ultrasonic extraction,
Again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of, prepare gen-seng haulms general flavone it is thick
The step of extract solution, by Hydrochloric Acid Hydrolysis Method the flavone glycoside in the gen-seng haulms general flavone crude extract solution is converted into
The step of converting of flavone aglycone, and drying steps.
2. the method according to claim 1 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：Pass through ultrasonic skill
Art extraction, again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of in, concentration of alcohol choosing
From 20% ~ 100% scope.
3. the method according to claim 1 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：Pass through ultrasonic skill
Art extraction, again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of in, during ultrasonic extraction
Between be selected from the scope of 10 ~ 50 minutes.
4. the method according to claim 1 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：Pass through ultrasonic skill
Art extraction, again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of in, ultrasonic extraction temperature
Degree is selected from 40 ~ 80 DEG C of scope.
5. the method according to claim 1 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：Pass through ultrasonic skill
Art extraction, again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of in, ultrasonic extraction work(
Rate is selected from 200 ~ 400W scope.
6. the method according to claim 1 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：Pass through ultrasonic skill
Art extraction, again by filtering, concentrate, petroleum ether decolourize after gen-seng haulms general flavone crude extract the step of in, solid-liquid ratio is selected from
1:10~1:50 scope.
7. the method according to any one of claim 1 to 6 that flavone aglycone is prepared from gen-seng haulms, its feature exist
In：In the step of preparing gen-seng haulms general flavone crude extract solution,
Above-mentioned gen-seng haulms general flavone crude extract is made into alcoholic solution using low molecule alcohol compound.
8. the method according to claim 7 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：By above-mentioned ginseng
Stem leaf total flavones crude extract is made into alcoholic solution using methanol.
9. the method according to any one of claim 1 to 6 that flavone aglycone is prepared from gen-seng haulms, its feature exist
In：Flavone glycoside in the gen-seng haulms general flavone crude extract solution is converted into by flavone aglycone by Hydrochloric Acid Hydrolysis Method.
10. the method according to claim 9 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：In hydrochloric acid water
Solution was prepared in the step of Hemodynamics aglycon, and hydrochloric acid hydrolysis time is selected from the scope of 1 ~ 6 hour.
11. the method according to claim 9 that flavone aglycone is prepared from gen-seng haulms, it is characterised in that：In hydrochloric acid water
Solution was prepared in the step of Hemodynamics aglycon, and concentration of hydrochloric acid is selected from the mol/L of 1 mol/L ~ 6 scope.
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| 竹叶黄酮糖苷的水解及其苷元的抗氧化性能研究;张英等;《中国粮油学报》;20110630;第16卷(第3期);第34-37页，尤其是第34页右栏第1.2.1和第36页左栏第4段 * |
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