CN106831778A - A kind of method that N-Oxysophocarpine is extracted in the tattooing from wolf's fang - Google Patents
A kind of method that N-Oxysophocarpine is extracted in the tattooing from wolf's fang Download PDFInfo
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- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
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Abstract
A kind of present invention extracts N-Oxysophocarpine method in disclosing tattooing from wolf's fang, comprises the following steps：（1）Heated after mushroom and water mixing, filtering takes filtrate and wolf's fang tattooing is pre-processed；（2）By pretreated wolf's fang tattooing, with the solution soak extraction 2 times at least containing a kind of organic solvent, merge the filtrate of 2 times, filtrate decompression is concentrated to give N-Oxysophocarpine crude extract medicinal extract, filter residue uses acetic acid solution soak extraction 2 times again, merge 2 filtrates, filter vacuum is concentrated to give N-Oxysophocarpine crude extract medicinal extract；The crude extract medicinal extract that merging is obtained, by collecting filtrate after the heavy removal of impurities of water, filtrate is dried by after vacuum concentration, vacuum drying, silica gel post separation, Crystallization Separation, recrystallization, that is, obtain N-Oxysophocarpine.The present invention can be recycled wolf's fang tattooing, and operating process is simple, directly extracted and be can obtain N-Oxysophocarpine, and recovery rate is high, and product purity is high, can reach more than 99%.
Description
Technical field
The invention belongs to technical field of biological extraction, and in particular to extract the side of N-Oxysophocarpine in a kind of tattooing from wolf's fang
Method.
Background technology
Sophara viciifolia also known as Sophora viciifolia, are the perennial shrub of pulse family Sophora, be born in more 400~1500m of height above sea level tailo or
River valley area, is distributed widely in the province such as China North China, Jiangsu, Zhejiang, Hubei, Henan, Shaanxi, Gansu and southwest.Sophara viciifolia
All contain alkaloid in root, stem, leaf, flower, fruit and seed, various biologies such as including oxymatrine, sophocarpine, Sophoridine
Alkali.Sophara viciifolia is widely used as a kind of medicinal material among the people, and N-Oxysophocarpine is the principle active component of Chinese herbal medicine, with anti-
Inflammation, liver protection, antitumor, anti-arrhythmia cordis, immunological regulation, increasing leukocyte and sterilization, desinsection, diuresis, relieving asthma, anti-arrhythmia
It is the important source material for developing various human administrations, articles for washing and desinsection class biological pesticide Deng effect.
At present, the recovery rate that N-Oxysophocarpine is directly extracted from plant is low, is usually extracted from plant using first
To sophocarpine, recycle industrial production process that sophocarpine is prepared into N-Oxysophocarpine, this kind of procedure is complicated, high cost.
Chinese patent（CN102786523 A）A kind of method that sophocarpine is prepared from Sophora alopecuroide is disclosed, using various in Sophora alopecuroide
The different principle of alkaloid polarity, matrine, sophocarpine are separated with other alkali, then isolate sophocarpine.But, this method
Can only extract and obtain sophocarpine.N-Oxysophocarpine is mainly obtained by industrial production process, causes preparation technology cumbersome, for example,
Chinese patent（CN1354181 A）It is, by sophocarpine addition hydrogen peroxide, then reaction solution to be extracted or is concentrated under reduced pressure to give
N-Oxysophocarpine.
Chinese patent（CN 1473830A）A kind of method that matrine is extracted from Sophora viciifolia is disclosed, is by Sophora viciifolia
Aerial part salt acid soak, then by refluxing toluene, boil, plus reducing agent, extraction, after acid adding is obtained Banlangen,
By Banlangen centrifugation, matrine and Sophoridine are prepared after over hydrogenation, recrystallization.But, prepared in the technique
In the Banlangen for obtaining, the recovery rate of sophocarpine and N-Oxysophocarpine is extremely low, and is had to human body using toluene in the technique
Evil, it is difficult to popularization and application.
Alkaloid extraction is only carried out to Sophara viciifolia seed at present and series product development is utilized, and Sophara viciifolia setting percentage pole
It is low, flower only less than 10% can it is ripe be seed, more than 90% flower causes fallen flowers to waste in growth course；In addition, wolf
The collection difficulty of tooth thorn seed is big and collection rate is low, and flower collection rate is high and easily collecting.Therefore, wolf's fang tattooing is developed
Utilize, extracting N-Oxysophocarpine therein has positive effect.
The content of the invention
For the defect of prior art, the present invention extracts the method for N-Oxysophocarpine, tool in providing a kind of tattooing from wolf's fang
Have the advantages that recovery rate is high, purity is high.
The present invention is achieved by the following technical solutions.
A kind of method that N-Oxysophocarpine is extracted in tattooing from wolf's fang, comprises the following steps：
（1）Pretreatment：Mushroom is weighed, according to solid-liquid ratio 1g：30 mL add water, and 40-50 DEG C is heated 40-60min, after cooling, mistake
Filter, mushroom is recycled, and the mushroom filtrate for obtaining is standby；By wolf's fang tattooing and the mushroom filtrate for obtaining according to solid-liquid ratio 1:8 mix
Close, 2h is soaked at 3-6 DEG C, stirring is stirred once every 20min, filtering obtains pretreated wolf's fang tattooing；
（2）Extract：By step（1）Pretreated wolf's fang tattooing, according to solid-liquid ratio 1g：8 mL are added at least containing a kind of organic
The solution of solvent, soaks 72h, filtering and collecting filter liquid and filter residue, and filter residue is according to solid-liquid ratio 1g：8 mL containing one kind with least having
The solution of machine solvent continues to soak 48 h, filtering and collecting filter liquid and filter residue, and the filtrate that merging is obtained for 2 times is rotated by filtrate
Evaporation under reduced pressure is concentrated to give N-Oxysophocarpine crude extract medicinal extract；By filter residue according to solid-liquid ratio 1g：10 mL add mass concentration be
The acetic acid solution of 1%-5%, soaks 72h, filtering and collecting filter liquid and filter residue, and filter residue is according to solid-liquid ratio 1g：10 mL mass concentrations
Be 1%-5% acetic acid solution continue soak 48 h, filtering and collecting filter liquid, it is thick that filtrate obtains N-Oxysophocarpine by vacuum concentration
Extract medicinal extract；The N-Oxysophocarpine crude extract medicinal extract that merging is obtained for 2 times, it is standby；
（3）Water sinks removal of impurities：By step（2）The 3-5 times of water of quality is added in the N-Oxysophocarpine crude extract medicinal extract for finally giving, is used
Ammoniacal liquor adjusts pH to 11, is filtered after 48 h are stood at room temperature, collects filtrate；
（4）By step（3）The filtrate for obtaining after vacuum concentration obtains condensed cream, condensed cream vacuum drying, using methyl alcohol and
Dichloromethane for eluent be dried after silica gel post separation, addition ether carry out Crystallization Separation, addition acetone recrystallization,
Obtain N-Oxysophocarpine sterling.
Preferably, step（1）Described at least containing a kind of solution of organic solvent be methyl alcohol, ethanol, chloroform or dichloro
Any one in methane.
Preferably, step（1）Described in be at least for volume ratio containing a kind of solution of organic solvent（85-95）：（5-
15）Methyl alcohol and the mixture of chloroform, volume ratio be 9:1 methyl alcohol and the mixture of acetic acid or volume ratio are（30-50）：
（50-70）Concentrated ammonia liquor and chloroform mixture in any one.
Preferably, the mass concentration of above-mentioned concentrated ammonia liquor is 27%.
Preferably, step（2）And step（4）Described in vacuum concentration be：By filtrate 60-65 DEG C, vacuum-
20-25min is concentrated in vacuo under 0.075 to -0.081MPa, condensed cream is obtained.
Preferably, above-mentioned vacuum drying is：To be concentrated in vacuo the condensed cream that obtains 55 DEG C -60 DEG C, pressure -0.081 to -
6-8h is vacuum dried under the conditions of 0.085MPa, powdered N-Oxysophocarpine crude product is obtained.
Preferably, it is above-mentioned to use methyl alcohol and the dichloromethane to be for the concrete operations that eluent carries out silica gel post separation：According to
Mass ratio is 1：（2-3）, by N-Oxysophocarpine crude product and the silica gel mixed sample upper prop of 200 mesh, methyl alcohol and dichloromethane are used to wash
De- liquid, first according to methyl alcohol：The mass ratio of dichloromethane is 2：3 are eluted, the impurity such as removal fat-soluble pigment, lipid, while
The N-Oxysophocarpine known in eluent is examined with TLC, when N-Oxysophocarpine is positive in detecting eluent, then is pressed
According to methyl alcohol：The mass ratio of dichloromethane is 2：6 are eluted, until when detecting N-Oxysophocarpine in eluent and being negative, receiving
Collection eluent；Will collect eluent decompression stepwise distillation reclaim dichloromethane and methyl alcohol, when eluent distill to it is dry when, according to
N-Oxysophocarpine crude product is 1g with the solid-liquid ratio of dichloromethane:1mL adds dichloromethane, obtains dichloromethane-N-Oxysophocarpine
Solution.
Preferably, the concrete operations that above-mentioned addition ether carries out Crystallization Separation are：According to volume ratio 1:1, to dichloromethane-
Ether is added in N-Oxysophocarpine solution, is filtered, obtain filtrate, be 1 according to the volume ratio of filtrate and ether:（3-5）, to filtrate
Middle addition ether, stands still for crystals 12h, filtering, obtains N-Oxysophocarpine crystalline product, and filtrate reclaims dichloro through stepwise distillation of depressurizing
Methane and ether.
Preferably, carrying out dry concrete operations after above-mentioned addition acetone recrystallization is：According to solid-liquid ratio 1g:（3-5）ML,
To acetone is added in N-Oxysophocarpine crystalline product, N-Oxysophocarpine monomer is recrystallized to give, is then dried at 100-105 DEG C
3-4h, obtains N-Oxysophocarpine finished product.N-Oxysophocarpine finished product content test is carried out using liquid chromatogram.
Advantages of the present invention：
The present invention uses wolf's fang tattooing to extract N-Oxysophocarpine for raw material, can carry out the wolf's fang tattooing that fallen flowers are wasted reclaiming profit
With, raw material sources are wide and collect low cost, and operating process is simple, directly extract and can obtain N-Oxysophocarpine, and recovery rate is high,
Product purity is high, can reach more than 99%.
Specific embodiment
Embodiment 1
The content detection of N-Oxysophocarpine in raw material wolf's fang tattooing
（1）The preparation of mark product solution：Precision weighs the mg of N-Oxysophocarpine mark product 10.0, with being settled to 10 mL after ultrapure water dissolves
In volumetric flask, the mark product mother liquor containing the mg/mL of N-Oxysophocarpine 1.00 is made；
（2）The preparation of sample solution：The g of Sophara viciifolia style product 0.5 accurately is weighed, is placed in 100 mL triangular flasks, added
10mL analyzes pure concentrated ammonia liquor and is allowed to moisten, and adds 30mL and analyzes pure chloroform, and 30 min are extracted in shaking, after standing 4h, filtering,
Filter residue is continuously extracted 3 times, merges extract solution, and then 80 DEG C of recovery chloroforms, obtain dried object, dried object ultra-pure water constant volume
To 25 mL, after 0.5 μm of filtering with microporous membrane, collection filtrate is sample solution, standby；
（3）Chromatographic condition：From ZORBAXC18 chromatographic columns (150 mm × 4.6 mm, 5 μm)；The nm of Detection wavelength 220；Mobile phase
It is phosphoric acid-methanol solution (volume ratio 90 of 0.04 mol/ L：10, analyze pure)；The mL/min of flow velocity 1.0；20 DEG C of bars of column temperature
Under part, precision draws mark product solution and the μ L of sample solution 10 difference sample introductions are determined.
（4）Testing index：Detected through above method, the content of N-Oxysophocarpine is 2.4% in sample material wolf's fang tattooing.
Embodiment 2
A kind of method that N-Oxysophocarpine is extracted in tattooing from wolf's fang, comprises the following steps：
（1）Pretreatment：Mushroom is weighed, according to solid-liquid ratio 1g：30 mL add water, and 50 DEG C of heating 40min after cooling, are filtered, fragrant
Mushroom recycles, and the mushroom filtrate for obtaining is standby；By 50g wolf's fang tattooing and mushroom filtrate obtained above according to solid-liquid ratio 1:8
Mixing, 2h is soaked at 3 DEG C, and stirring is stirred once every 20min, and filtering obtains pretreated wolf's fang tattooing；
（2）Extract：By step（1）Pretreated wolf's fang tattooing, according to solid-liquid ratio 1g：8 mL add 400mL methanol solutions, leaching
Bubble 72h, filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：8 mL are continued to soak 48 h with 400mL methanol solutions,
The rotated evaporation under reduced pressure of filtrate is concentrated to give oxidation Chinese scholartree really by filtering and collecting filter liquid and filter residue, the filtrate that merging is obtained for 2 times
Alkali crude extract medicinal extract；By filter residue according to solid-liquid ratio 1g：10 mL add the acetic acid solution that 500mL mass concentrations are 1%, soak 72h,
Filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：10 mL are continued with the acetic acid solution that 500mL mass concentrations are 1%
48 h, filtering and collecting filter liquid are soaked, filtrate is concentrated in vacuo 20min under 60 DEG C, the MPa of vacuum -0.081 and obtains aoxidizing Chinese scholartree
Fruit alkali crude extract medicinal extract；The N-Oxysophocarpine crude extract medicinal extract that merging is obtained for 2 times, it is standby；
（3）Water sinks removal of impurities：By step（2）3 times of water of quality are added in the N-Oxysophocarpine crude extract medicinal extract for finally giving, ammonia is used
Water adjusts pH to 11, is filtered after 48 h are stood at room temperature, collects filtrate；
（4）Vacuum concentration：By step（3）The filtrate for obtaining is concentrated in vacuo 20min under 60 DEG C, the MPa of vacuum -0.081, obtains
To condensed cream, density is 1.45g/mL；
（5）Vacuum drying：By step（4）Condensed cream be vacuum dried 6h under the conditions of 55 DEG C, pressure -0.085MPa, obtain powder
Last shape N-Oxysophocarpine crude product；
（6）Use methyl alcohol and dichloromethane carries out silica gel post separation for eluent：It is 1 according to mass ratio：2, by N-Oxysophocarpine
The silica gel mixed sample upper prop of crude product and 200 mesh, it is eluent to use methyl alcohol and dichloromethane, first according to methyl alcohol：The matter of dichloromethane
Amount is than being 2：3 are eluted, the impurity such as removal fat-soluble pigment, lipid, while examining the oxygen known in eluent with TLC
Change sophocarpine, when N-Oxysophocarpine is positive in detecting eluent, according still further to methyl alcohol：The mass ratio of dichloromethane is 2：6
Eluted, until when detecting N-Oxysophocarpine in eluent and being negative, collecting eluent；The eluent decompression point that will be collected
Section Distillation recovery dichloromethane and methyl alcohol, when eluent distill to it is dry when, according to N-Oxysophocarpine crude product and the material of dichloromethane
Liquor ratio is 1g:1mL adds dichloromethane, obtains dichloromethane-N-Oxysophocarpine solution；
（7）Adding ether carries out Crystallization Separation：According to volume ratio 1:1, to adding second in dichloromethane-N-Oxysophocarpine solution
Ether, filtering, obtains filtrate, is 1 according to the volume ratio of filtrate and ether:3, to ether is added in filtrate, stand still for crystals 12h, mistake
Filter, obtains N-Oxysophocarpine crystalline product, and filtrate reclaims dichloromethane and ether through stepwise distillation of depressurizing；
（8）It is dried after adding acetone recrystallization：According to solid-liquid ratio 1g:3mL, to adding third in N-Oxysophocarpine crystalline product
Ketone, is recrystallized to give N-Oxysophocarpine monomer, then dries 3h at 105 DEG C, obtains N-Oxysophocarpine finished product.
The all chemistry of agents useful for same are pure.
Embodiment 3
A kind of method that N-Oxysophocarpine is extracted in tattooing from wolf's fang, comprises the following steps：
（1）Pretreatment：Mushroom is weighed, according to solid-liquid ratio 1g：30 mL add water, and 40 DEG C of heating 60min after cooling, are filtered, fragrant
Mushroom recycles, and the mushroom filtrate for obtaining is standby；By 50g wolf's fang tattooing and mushroom filtrate obtained above according to solid-liquid ratio 1:8
Mixing, 2h is soaked at 6 DEG C, and stirring is stirred once every 20min, and filtering obtains pretreated wolf's fang tattooing；
（2）Extract：By step（1）Pretreated wolf's fang tattooing, according to solid-liquid ratio 1g：8 mL add 400mL methanol solutions, leaching
Bubble 72h, filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：8 mL are continued to soak 48 h with 400mL methanol solutions,
The rotated evaporation under reduced pressure of filtrate is concentrated to give oxidation Chinese scholartree really by filtering and collecting filter liquid and filter residue, the filtrate that merging is obtained for 2 times
Alkali crude extract medicinal extract；By filter residue according to solid-liquid ratio 1g：10 mL add the acetic acid solution that 500mL mass concentrations are 5%, soak 72h,
Filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：10 mL are continued with the acetic acid solution that 500mL mass concentrations are 5%
48 h, filtering and collecting filter liquid are soaked, filtrate is concentrated in vacuo 25min under 65 DEG C, vacuum -0.075MPa and obtains oxidation Chinese scholartree really
Alkali crude extract medicinal extract；The N-Oxysophocarpine crude extract medicinal extract that merging is obtained for 2 times, it is standby；
（3）Water sinks removal of impurities：By step（2）5 times of water of quality are added in the N-Oxysophocarpine crude extract medicinal extract for finally giving, ammonia is used
Water adjusts pH to 11, is filtered after 48 h are stood at room temperature, collects filtrate；
（4）Vacuum concentration：By step（3）The filtrate for obtaining is concentrated in vacuo 25min under 65 DEG C, vacuum -0.075MPa, obtains
Condensed cream, density is 1.38g/mL；
（5）Vacuum drying：By step（4）Condensed cream be vacuum dried 8h under the conditions of 60 DEG C, pressure -0.081MPa, obtain powder
Last shape N-Oxysophocarpine crude product；
（6）Use methyl alcohol and dichloromethane carries out silica gel post separation for eluent：It is 1 according to mass ratio：3, by N-Oxysophocarpine
The silica gel mixed sample upper prop of crude product and 200 mesh, it is eluent to use methyl alcohol and dichloromethane, first according to methyl alcohol：The matter of dichloromethane
Amount is than being 2：3 are eluted, the impurity such as removal fat-soluble pigment, lipid, while examining the oxygen known in eluent with TLC
Change sophocarpine, when N-Oxysophocarpine is positive in detecting eluent, according still further to methyl alcohol：The mass ratio of dichloromethane is 2：6
Eluted, until when detecting N-Oxysophocarpine in eluent and being negative, collecting eluent；The eluent decompression point that will be collected
Section Distillation recovery dichloromethane and methyl alcohol, when eluent distill to it is dry when, according to N-Oxysophocarpine crude product and the material of dichloromethane
Liquor ratio is 1g:1mL adds dichloromethane, obtains dichloromethane-N-Oxysophocarpine solution；
（7）Adding ether carries out Crystallization Separation：According to volume ratio 1:1, to adding second in dichloromethane-N-Oxysophocarpine solution
Ether, filtering, obtains filtrate, is 1 according to the volume ratio of filtrate and ether:5, to ether is added in filtrate, stand still for crystals 12h, mistake
Filter, obtains N-Oxysophocarpine crystalline product, and filtrate reclaims dichloromethane and ether through stepwise distillation of depressurizing；
（8）It is dried after adding acetone recrystallization：According to solid-liquid ratio 1g:5mL, to adding third in N-Oxysophocarpine crystalline product
Ketone, is recrystallized to give N-Oxysophocarpine monomer, then dries 4h at 100 DEG C, obtains N-Oxysophocarpine finished product.
The all chemistry of agents useful for same are pure.
Embodiment 4
A kind of method that N-Oxysophocarpine is extracted in tattooing from wolf's fang, comprises the following steps：
（1）Pretreatment：Mushroom is weighed, according to solid-liquid ratio 1g：30 mL add water, and 45 DEG C of heating 50min after cooling, are filtered, fragrant
Mushroom recycles, and the mushroom filtrate for obtaining is standby；By 50g wolf's fang tattooing and mushroom filtrate obtained above according to solid-liquid ratio 1:8
Mixing, 2h is soaked at 4 DEG C, and stirring is stirred once every 20min, and filtering obtains pretreated wolf's fang tattooing；
（2）Extract：By step（1）Pretreated wolf's fang tattooing, according to solid-liquid ratio 1g：8 mL add 400mL methanol solutions, leaching
Bubble 72h, filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：8 mL are continued to soak 48 h with 400mL methanol solutions,
The rotated evaporation under reduced pressure of filtrate is concentrated to give oxidation Chinese scholartree really by filtering and collecting filter liquid and filter residue, the filtrate that merging is obtained for 2 times
Alkali crude extract medicinal extract；By filter residue according to solid-liquid ratio 1g：10 mL add the acetic acid solution that 500mL mass concentrations are 3%, soak 72h,
Filtering and collecting filter liquid and filter residue, filter residue is according to solid-liquid ratio 1g：10 mL are continued with the acetic acid solution that 500mL mass concentrations are 3%
48 h are soaked, filtering and collecting filter liquid, filtrate is concentrated in vacuo 23min under 63 DEG C, vacuum -0.077MPa, obtain aoxidizing Chinese scholartree
Fruit alkali crude extract medicinal extract；The N-Oxysophocarpine crude extract medicinal extract that merging is obtained for 2 times, it is standby；
（3）Water sinks removal of impurities：By step（2）4 times of water of quality are added in the N-Oxysophocarpine crude extract medicinal extract for finally giving, ammonia is used
Water adjusts pH to 11, is filtered after 48 h are stood at room temperature, collects filtrate；
（4）Vacuum concentration：By step（3）The filtrate for obtaining is concentrated in vacuo 23min under 63 DEG C, vacuum -0.077MPa, obtains
Condensed cream, density is 1.40g/mL；
（5）Vacuum drying：By step（4）Condensed cream be vacuum dried 7h under the conditions of 58 DEG C, pressure -0.083Mpa, obtain powder
Last shape N-Oxysophocarpine crude product；
（6）Use methyl alcohol and dichloromethane carries out silica gel post separation for eluent：It is 1 according to mass ratio：3, by N-Oxysophocarpine
The silica gel mixed sample upper prop of crude product and 200 mesh, it is eluent to use methyl alcohol and dichloromethane, first according to methyl alcohol：The matter of dichloromethane
Amount is than being 2：3 are eluted, the impurity such as removal fat-soluble pigment, lipid, while examining the oxygen known in eluent with TLC
Change sophocarpine, when N-Oxysophocarpine is positive in detecting eluent, according still further to methyl alcohol：The mass ratio of dichloromethane is 2：6
Eluted, until when detecting N-Oxysophocarpine in eluent and being negative, collecting eluent；The eluent decompression point that will be collected
Section Distillation recovery dichloromethane and methyl alcohol, when eluent distill to it is dry when, according to N-Oxysophocarpine crude product and the material of dichloromethane
Liquor ratio is 1g:1mL adds dichloromethane, obtains dichloromethane-N-Oxysophocarpine solution；
（7）Adding ether carries out Crystallization Separation：According to volume ratio 1:1, to adding second in dichloromethane-N-Oxysophocarpine solution
Ether, filtering, obtains filtrate, is 1 according to the volume ratio of filtrate and ether:4, to ether is added in filtrate, stand still for crystals 12h, mistake
Filter, obtains N-Oxysophocarpine crystalline product, and filtrate reclaims dichloromethane and ether through stepwise distillation of depressurizing；
（8）It is dried after adding acetone recrystallization：According to solid-liquid ratio 1g:4mL, to adding third in N-Oxysophocarpine crystalline product
Ketone, is recrystallized to give N-Oxysophocarpine monomer, then dries 4h at 105 DEG C, obtains N-Oxysophocarpine finished product.
The all chemistry of agents useful for same are pure.
Embodiment 5
Weigh 10 parts of Sophara viciifolia style product, every part of 50g, respectively with ethanol, chloroform, dichloromethane, volume ratio 95:5、90:10、
85:15 methyl alcohol and the mixed liquor of chloroform, volume ratio are 9:1 methyl alcohol and the mixed liquor of acetic acid, volume ratio are 30:70、40:
60、50:50 concentrated ammonia liquor（Mass concentration is 27%）With the mixed liquor of chloroform, instead of step（2）In methyl alcohol, extracted, its
He is designated as comparative example 5 respectively with 4,10 parts of samples of embodiment（1）, comparative example 5（2）, comparative example 5（3）, comparative example 5（4）, contrast
Example 5（5）, comparative example 5（6）, comparative example 5（7）, comparative example 5（8）, comparative example 5（9）, comparative example 5（10）.
Comparative example 1
Using Chinese patent（CN 1473830A）The method of embodiment 1, detects its step（Three）The matrine crude product that middle B is obtained
The content of middle N-Oxysophocarpine.
Comparative example 2
3 parts of Sophara viciifolia style product are weighed, every part of 50g omits step（1）, pretreatment is not used, directly from step（2）Start to carry
Take, respectively with embodiment 2,3,4,3 parts of samples are designated as comparative example 2 to other steps respectively（1）, comparative example 2（2）, comparative example 2（3）.
Using the detection method of embodiment 1, carry out detecting N-Oxysophocarpine finished product content using liquid chromatogram, aoxidized
The purity of sophocarpine finished product.1 is shown in Table to the N-Oxysophocarpine testing result that different embodiments are obtained, recovery rate is according to below equation
It is calculated：Wolf's fang tattooing N-Oxysophocarpine recovery rate (%)=(the net quality ÷ raw materials wolf's fang tattooing of N-Oxysophocarpine in sample
N-Oxysophocarpine quality) × 100%.
The testing result of the different embodiment N-Oxysophocarpines of table 1
As shown in Table 1, embodiment 2-4 first carries out soak extraction using methyl alcohol to wolf's fang tattooing, and filtrate decompression is concentrated to give slightly
Extract condensed cream, then using mass concentration 1-5% acetic acid to filter residue soak extraction, acetic acid concentration at 3%, N-Oxysophocarpine
Recovery rate and purity are of a relatively high；When methyl alcohol is replaced using other solvents, during the mixed liquor extraction of concentrated ammonia liquor and chloroform, Chinese scholartree is aoxidized
The recovery rate and purity of fruit alkali are of a relatively high；And the method for using comparative example 1, N-Oxysophocarpine contains in detection matrine crude product
During amount, its purity is 0, and being extracted using the method can not obtain N-Oxysophocarpine；Using the method for comparative example 2, not to Sophara viciifolia
Flower is pre-processed, and when directly being extracted, the recovery rate and purity of its N-Oxysophocarpine are significantly lower than first to be adopted to wolf's fang tattooing
With pretreatment and then the method extracted.
Claims (9)
1. a kind of method that N-Oxysophocarpine is extracted in tattooing from wolf's fang, comprises the following steps：
（1）Pretreatment：Mushroom is weighed, according to solid-liquid ratio 1g：30 mL add water, and 40-50 DEG C is heated 40-60min, after cooling, mistake
Filter, mushroom is recycled, and the mushroom filtrate for obtaining is standby；By wolf's fang tattooing and the mushroom filtrate for obtaining according to solid-liquid ratio 1:8 mix
Close, 2h is soaked at 3-6 DEG C, stirring is stirred once every 20min, filtering obtains pretreated wolf's fang tattooing；
（2）Extract：By step（1）Pretreated wolf's fang tattooing, according to solid-liquid ratio 1g：8 mL are added at least containing a kind of organic
The solution of solvent, soaks 72h, filtering and collecting filter liquid and filter residue, and filter residue is according to solid-liquid ratio 1g：8 mL containing one kind with least having
The solution of machine solvent continues to soak 48 h, filtering and collecting filter liquid and filter residue, and the filtrate that merging is obtained for 2 times is rotated by filtrate
Evaporation under reduced pressure is concentrated to give N-Oxysophocarpine crude extract medicinal extract；By filter residue according to solid-liquid ratio 1g：10 mL add mass concentration be
The acetic acid solution of 1%-5%, soaks 72h, filtering and collecting filter liquid and filter residue, and filter residue is according to solid-liquid ratio 1g：10 mL mass concentrations
Be 1%-5% acetic acid solution continue soak 48 h, filtering and collecting filter liquid, it is thick that filtrate obtains N-Oxysophocarpine by vacuum concentration
Extract medicinal extract；The N-Oxysophocarpine crude extract medicinal extract that merging is obtained for 2 times, it is standby；
（3）Water sinks removal of impurities：By step（2）The 3-5 times of water of quality is added in the N-Oxysophocarpine crude extract medicinal extract for finally giving, is used
Ammoniacal liquor adjusts pH to 11, is filtered after 48 h are stood at room temperature, collects filtrate；
（4）By step（3）The filtrate for obtaining after vacuum concentration obtains condensed cream, condensed cream vacuum drying, using methyl alcohol and
Dichloromethane for eluent be dried after silica gel post separation, addition ether carry out Crystallization Separation, addition acetone recrystallization,
Obtain N-Oxysophocarpine sterling.
2. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 1, it is characterised in that：Step
（1）Described at least containing a kind of solution of organic solvent be methyl alcohol, ethanol, chloroform or dichloromethane in any one.
3. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 1, it is characterised in that：Step
（1）Described in be at least for volume ratio containing a kind of solution of organic solvent（85-95）：（5-15）Methyl alcohol and chloroform mixing
Thing, volume ratio are 9:1 methyl alcohol and the mixture of acetic acid or volume ratio are（30-50）：（50-70）Concentrated ammonia liquor and chloroform
Mixture in any one.
4. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 3, it is characterised in that：It is described
The mass concentration of concentrated ammonia liquor is 27%.
5. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 1, it is characterised in that：Step
（2）And step（4）Described in vacuum concentration be：By filtrate under 60-65 DEG C, vacuum -0.075 to -0.081MPa vacuum
Concentration 20-25min, obtains condensed cream.
6. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 5, it is characterised in that：It is described
It is vacuum dried and is：Condensed cream is vacuum dried 6-8h under the conditions of 55 DEG C -60 DEG C, pressure -0.081 to -0.085MPa, obtains powder
Shape N-Oxysophocarpine crude product.
7. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 6, it is characterised in that：It is described
Methyl alcohol and the dichloromethane is used to be for the concrete operations that eluent carries out silica gel post separation：It is 1 according to mass ratio：（2-3）, by oxygen
Change the silica gel mixed sample upper prop of sophocarpine crude product and 200 mesh, it is eluent to use methyl alcohol and dichloromethane, first according to methyl alcohol：Dichloro
The mass ratio of methane is 2：3 are eluted, while examining the N-Oxysophocarpine known in eluent with TLC, are washed when detecting
When N-Oxysophocarpine is positive in de- liquid, according still further to methyl alcohol：The mass ratio of dichloromethane is 2：6 are eluted, until detecting
When N-Oxysophocarpine is negative in eluent, eluent is collected；Dichloromethane is reclaimed in the eluent decompression stepwise distillation that will be collected
And methyl alcohol, when eluent distill to it is dry when, be 1g according to the solid-liquid ratio of N-Oxysophocarpine crude product and dichloromethane:1mL adds two
Chloromethanes, obtains dichloromethane-N-Oxysophocarpine solution.
8. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 7, it is characterised in that：It is described
Add ether to carry out the concrete operations of Crystallization Separation to be：According to volume ratio 1:1, add in dichloromethane-N-Oxysophocarpine solution
Enter ether, filter, obtain filtrate, be 1 according to the volume ratio of filtrate and ether:（3-5）, to ether is added in filtrate, stand knot
Brilliant 12h, filtering obtains N-Oxysophocarpine crystalline product, and filtrate reclaims dichloromethane and ether through stepwise distillation of depressurizing.
9. the method that N-Oxysophocarpine is extracted in a kind of tattooing from wolf's fang according to claim 8, it is characterised in that：It is described
Carrying out dry concrete operations after addition acetone recrystallization is：According to solid-liquid ratio 1g:（3-5）ML, crystallizes to N-Oxysophocarpine and produces
Acetone is added in product, N-Oxysophocarpine monomer is recrystallized to give, then 3-4h is dried at 100-105 DEG C, oxidation Chinese scholartree is obtained really
Alkali finished product.
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| CN1500785A (en) * | 2002-11-18 | 2004-06-02 | 大兴安岭林格贝有机食品有限责任公司 | Sophora flavescens alkaloid and production technology thereof |
| CN1473830A (en) * | 2003-06-02 | 2004-02-11 | 平 刘 | Process for extracting matrine and sophoridine from sophora viciifolia or sophora moocroftiana |
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Application publication date: 20170613 |