CN108079048A - The method that general flavone is extracted in Canton love-pea vine - Google Patents
The method that general flavone is extracted in Canton love-pea vine Download PDFInfo
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
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Abstract
The invention discloses a kind of method that general flavone is extracted in Canton love-pea vine, this method is divided into four steps：First Canton love-pea vine is dried, is crushed, again with ionic liquid mixing, through ultrasonic wave extraction, decoloration removal of impurities is then carried out by chitosan, activated carbon, macroreticular resin, the Canton love-pea vine total flavone that recovery rate is 95.7 98.4%, purity is 86.8 90.3% is made after concentrated vacuum drying.This method is easy to operate, and general flavone purity obtained has greatly improved compared with the prior art, is conducive to the comprehensive exploitation of Canton love-pea vine.
Description
Technical field
The present invention relates to traditional Chinese medicine extraction processing technique fields, and in particular to a kind of method that general flavone is extracted in Canton love-pea vine.
Background technology
Canton love-pea vine alias hookedhairypod tickclover leaf hunts waist grass, yellow food grass, native Radix Glycyrrhizae, medicinal material name Canton love-pea vine.Be distributed mainly on Guangdong,
Guangxi is that China is peculiar.Because it is found at first in Community in Baiyunshan, Guangzhou, therefore also known as abrus cantoniensis Hance, it is used as medicine with complete stool and (removes beans
Pod).Canton love-pea vine herb is containing jequirity (L-abrine), flavonoid glycoside, choline, sterol, saponin(e, amino acid, carbohydrate, tannin, anthraquinone
Class compound, cool in nature, slightly sweet flavor have clearing heat and promoting diuresis, removing toxic substances, dispersing the depressed liver-qi and alleviating pain, promoting blood circulation and removing blood stasis and other effects, anxious, slow for treating
Property hepatitis, cirrhotic ascites, cholecystitis, stomachache, arthralgia pain due to rheumatism, beat numbness pain, venomous snake bite, mastitis, the urinary system that oozes infection etc.
Illness.Flavone compound is to treatment coronary heart disease, senile dementia, cerebral thrombus, the nervous system disease and eliminates free radical, suppression
Bacterium, anticancer etc. have remarkable result, and without side-effects, great exploitation prospect.Therefore, it is how efficiently yellow to Canton love-pea vine
Ketone compounds are extracted and isolated and purified, and are paid attention to be subject to domestic and foreign scholars, but presently relevant research is still less.
A kind of preparation method of Canton love-pea vine total flavone of disclosure of the invention that number of patent application is CN201110177604.X:It will
Dry Canton love-pea vine pulverizes and sieves, and using water as extractant, is extracted using cellulase, and general flavone quality is adjusted after extracting solution filtering
Concentration and pH value obtain sample solution, are then adsorbed using AB-8 types macroporous absorbent resin, ethanol elution, are concentrated under reduced pressure and freeze and is dry
Dry, the Canton love-pea vine total flavone rate of transform obtained is more than 90%, and the content of general flavone is more than 30% in purified.Prepared by this method
Canton love-pea vine total flavone purity is relatively low, does not utilize production application.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of methods that general flavone is extracted in Canton love-pea vine.
The present invention is achieved by the following technical programs:
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:8-15:The ratio of 12-20 is uniformly mixed, and adjusts pH5.7-7.0, the ultrasonic wave extraction 25- under the conditions of temperature is 40-58 DEG C
56min adds in chitosan solution, then through decolorization and impurity removal by active carbon, filters to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 2-3 times, and then ethanol solution dissolving is adjusted
PH5.7-7.0, then through decolorization and impurity removal by active carbon, then flow through macroreticular resin, be rinsed with water 2-3 times, then with macroreticular resin volume
5.3-10 ethanol solution elution again, obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
In the step S1, the drying temperature is 40-60 DEG C, drying time 10-15h.
Canton love-pea vine powder footpath is 60-100 mesh in the step S1.
The ultrasonic frequency 60-70KHz, power 360-500W that the extraction of ultrasonic extraction ripple uses in the step S2.
The chitosan solution mass concentration added in the step S2 is 0.3-1.5%.
It is 50-75% that the volumes of aqueous ethanol fraction used is eluted in the step S3.
Eluent is concentrated into the 25-35% of original volume in the step S4.
It is dry for vacuum drying, vacuum degree 80-120Pa in the step S4.
Canton love-pea vine total flavone moisture content is 2%-5% in the step S4.
Canton love-pea vine total flavone purity >=93% in the step S4
The beneficial effects of the present invention are:The present invention is mixed by Canton love-pea vine powder with ionic liquid, and then ultrasonic wave carries again
The recovery rate of general flavone in Canton love-pea vine can be improved by taking, up to more than 95%；Using chitosan, activated carbon, macroreticular resin knot
It closes use and carries out decoloration removal of impurities, Canton love-pea vine total flavone of the purity more than 86% is made after concentrated vacuum drying.This method is grasped
Make simply, general flavone purity obtained has greatly improved compared with the prior art, is conducive to the comprehensive exploitation of Canton love-pea vine.
Specific embodiment
Technical scheme is further described with reference to embodiments, but claimed scope is not limited to
In described.
Embodiment one
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:8:12 ratio is uniformly mixed, and adjusts pH5.7, and the ultrasonic wave extraction 25min under the conditions of temperature is 40 DEG C adds in chitosan
Solution, then through decolorization and impurity removal by active carbon, filter to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 2 times, and then ethanol solution dissolving adjusts pH5.7,
Again through decolorization and impurity removal by active carbon, macroreticular resin is then flowed through, is rinsed with water 2 times, then it is molten with the ethyl alcohol of 5.3 times of macroreticular resin volume
Liquid elutes, and obtains eluent；
S4, drying:Eluent concentrates, then dry Canton love-pea vine total flavone.
In step S1, drying temperature is 40 DEG C, drying time 10h.
Canton love-pea vine powder footpath is 60 mesh in step S1.
The ultrasonic frequency 50KHz, power 360W that the extraction of ultrasonic extraction ripple uses in step S2.
The chitosan solution mass concentration added in step S2 is 0.3%.
It is 50% that volumes of aqueous ethanol fraction is eluted in step S3.
Eluent is concentrated into the 25% of original volume in step S4.
It is dry for vacuum drying, vacuum degree 80Pa in step S4.
Canton love-pea vine total flavone moisture content is 2% in step S4.
Embodiment two
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:10:14 ratio is uniformly mixed, and adjusts pH6.2, and the ultrasonic wave extraction 30min under the conditions of temperature is 43 DEG C adds in shell and gathers
Sugar juice, then through decolorization and impurity removal by active carbon, filter to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 3 times, and then ethanol solution dissolving adjusts pH6.5,
Again through decolorization and impurity removal by active carbon, macroreticular resin is then flowed through, is rinsed with water 3 times, then it is molten with the ethyl alcohol of 6.0 times of macroreticular resin volume
Liquid elutes, and obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
In step S1, drying temperature is 48 DEG C, drying time 11h.
Canton love-pea vine powder footpath is 70 mesh in step S1.
The ultrasonic frequency 54KHz, power 378W that the extraction of ultrasonic extraction ripple uses in step S2.
The chitosan solution mass concentration added in step S2 is 0.6%.
It is 55% that volumes of aqueous ethanol fraction is eluted in step S3.
Eluent is concentrated into the 23% of original volume in step 4.
It is dry for vacuum drying, vacuum degree 87Pa in step S4.
Canton love-pea vine total flavone moisture content is 3% in step S4.
Embodiment three
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:13:16 ratio is uniformly mixed, and adjusts pH6.5, and the ultrasonic wave extraction 38min under the conditions of temperature is 48 DEG C adds in shell and gathers
Sugar juice, then through decolorization and impurity removal by active carbon, filter to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 3 times, and then ethanol solution dissolving adjusts pH6.7,
Again through decolorization and impurity removal by active carbon, macroreticular resin is then flowed through, is rinsed with water 2 times, then it is molten with the ethyl alcohol of 7.7 times of macroreticular resin volume
Liquid elutes, and obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
In step S1, drying temperature is 51 DEG C, drying time 12h.
Canton love-pea vine powder footpath is 82 mesh in step S1.
The ultrasonic frequency 58KHz, power 410W that the extraction of ultrasonic extraction ripple uses in step S2.
The chitosan solution mass concentration added in step S2 is 0.7%.
It is 63% that volumes of aqueous ethanol fraction is eluted in step S3.
Eluent is concentrated into the 30% of original volume in step S4.
It is dry for vacuum drying, vacuum degree 109Pa in step S4.
Canton love-pea vine total flavone moisture content is 4% in step S4.
Example IV
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:15:18 ratio is uniformly mixed, and adjusts pH7.0, and the ultrasonic wave extraction 48min under the conditions of temperature is 53 DEG C adds in shell and gathers
Sugar juice, then through decolorization and impurity removal by active carbon, filter to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 3 times, and then ethanol solution dissolving adjusts pH7.0,
Again through decolorization and impurity removal by active carbon, macroreticular resin is then flowed through, is rinsed with water 2 times, then it is molten with the ethyl alcohol of 8.6 times of macroreticular resin volume
Liquid elutes, and obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
In step S1, drying temperature is 56 DEG C, drying time 13h.
Canton love-pea vine powder footpath is 94 mesh in step S1.
The ultrasonic frequency 66KHz, power 460W that the extraction of ultrasonic extraction ripple uses in step S2.
The chitosan solution mass concentration added in step S2 is 1.2%.
It is 70% that volumes of aqueous ethanol fraction is eluted in step S3.
Eluent is concentrated into the 32% of original volume in step S4.
It is dry for vacuum drying, vacuum degree 97Pa in step S4.
Canton love-pea vine total flavone moisture content is 5% in step S4.
Embodiment five
A kind of method that general flavone is extracted in Canton love-pea vine, this method comprise the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are with weight ratio
For 1:8:20 ratio is uniformly mixed, and adjusts pH7.0, and the ultrasonic wave extraction 56min under the conditions of temperature is 58 DEG C adds in chitosan
Solution, then through decolorization and impurity removal by active carbon, filter to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 2 times, and then ethanol solution dissolving adjusts pH5.7,
Again through decolorization and impurity removal by active carbon, macroreticular resin is then flowed through, is rinsed with water 2 times, then it is molten with the ethyl alcohol of 10 times of macroreticular resin volume
Liquid elutes, and obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
In step S1, drying temperature is 60 DEG C, drying time 15h.
Canton love-pea vine powder footpath is 100 mesh in step S1.
The ultrasonic frequency 70KHz, power 500W that the extraction of ultrasonic extraction ripple uses in step S2.
The chitosan solution mass concentration added in step S2 is 1.5%.
It is 75% that volumes of aqueous ethanol fraction is eluted in step S3.
Eluent is concentrated into the 35% of original volume in step S4.
It is dry for vacuum drying, vacuum degree 120Pa in step S4.
Canton love-pea vine total flavone moisture content is 2% in step S4.
Experimental example one
Canton love-pea vine total flavone is prepared using the method that number of patent application is CN201110177604.X:By dry Canton love-pea vine
40 mesh sieves are crushed, using water as extractant, are extracted using cellulase, cellulase dosage is Canton love-pea vine material quality
0.3%, the ratio between the volume of extractant water and Canton love-pea vine material quality 12ml/g, pH value 4.4,45 DEG C of hydrolysis temperature, enzymolysis time
85min obtains extracting solution；General flavone mass concentration is adjusted after extracting solution filtering and pH value obtains sample solution, it is then big using AB-8 types
Macroporous adsorbent resin adsorbs, loading flow velocity 1.0BV/h, general flavone mass concentration 1.7mg/ml in sample solution, sample solution pH value
5.0；Eluent, the eluant, eluent be volume parts 63% ethyl alcohol, eluant, eluent flow velocity 0.8BV/h, eluting agent
For 2.3BV, eluent is obtained；It is concentrated under reduced pressure and is freeze-dried, obtain Canton love-pea vine total flavone product.
The general flavone that embodiment one to embodiment five, experimental example one are prepared into is measured into its general flavone recovery rate, total respectively
Flavones purity, as a result such as following table.
1 general flavone recovery rate of table and purity situation
| Number | General flavone recovery rate % | General flavone purity % |
| Embodiment one | 97.3 | 89.7 |
| Embodiment two | 96.8 | 86.8 |
| Embodiment three | 95.7 | 88.1 |
| Example IV | 97.8 | 90.3 |
| Embodiment five | 98.4 | 87.9 |
| Experimental example one | 92.0 | 36.0 |
As can be known from the above table, Canton love-pea vine total flavone its recovery rate is extracted as 95.7-98.4%, pure using the method for the present invention
It spends for 86.8-90.3%, and the recovery rate of experimental example one is 92.0%, purity 36.0%.Therefore, this method is compared with existing
Method has larger promotion in recovery rate, purity, has significant effect.
Claims (10)
1. the method for general flavone is extracted in a kind of Canton love-pea vine, which is characterized in that this method comprises the following steps:
S1, Canton love-pea vine drying crush to obtain Canton love-pea vine powder；
S2, Canton love-pea vine powder and 1- butyl -3- methylimidazoles acetate, 1- alkene butyl -3- methylimidazole villaumites are using weight ratio as 1:
8-15:The ratio of 12-20 is uniformly mixed, and adjusts pH5.7-7.0, the ultrasonic wave extraction 25- under the conditions of temperature is 40-58 DEG C
56min adds in chitosan solution, then through decolorization and impurity removal by active carbon, filters to take filtrate；
S3, filtrate are dissolved after being concentrated and dried with ethanol solution, are recrystallized 2-3 times, and then ethanol solution dissolving adjusts pH5.7-
7.0, then through decolorization and impurity removal by active carbon, then flow through macroreticular resin, be rinsed with water 2-3 times, then with macroreticular resin volume 5.3-10
Ethanol solution elution again, obtains eluent；
S4, eluent concentration, then dry Canton love-pea vine total flavone.
2. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:It is described in the step S1
Drying temperature is 40-60 DEG C, drying time 10-15h.
3. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Canton love-pea vine in the step S1
Powder footpath is 60-100 mesh.
4. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Ultrasound carries in the step S2
The ultrasonic frequency 60-70KHz, power 360-500W that ripple extraction is taken to use.
5. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:It is added in the step S2
Chitosan solution mass concentration is 0.3-1.5%.
6. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Being eluted in the step S3 makes
Volumes of aqueous ethanol fraction is 50-75%.
7. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Eluent in the step S4
It is concentrated into the 25-35% of original volume.
8. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Drying is in the step S4
Vacuum drying, vacuum degree 80-120Pa.
9. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Canton love-pea vine in the step S4
General flavone moisture content is 2%-5%.
10. the method for general flavone is extracted in Canton love-pea vine according to claim 1, it is characterised in that:Chicken bone in the step S4
Careless general flavone purity >=93%.
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| CN109010504A (en) * | 2018-09-05 | 2018-12-18 | 杨鑫 | A kind of extracting method of lycium ruthenicum general flavone |
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