CN101264117B - Mugwort flavone extracting technique and uses thereof - Google Patents
Mugwort flavone extracting technique and uses thereof Download PDFInfo
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- CN101264117B CN101264117B CN2008100180367A CN200810018036A CN101264117B CN 101264117 B CN101264117 B CN 101264117B CN 2008100180367 A CN2008100180367 A CN 2008100180367A CN 200810018036 A CN200810018036 A CN 200810018036A CN 101264117 B CN101264117 B CN 101264117B
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Abstract
The invention discloses a extracting process of mugwort flavonoids and the application of mugwort flavonoids in treating facial acne, which uses mugwort as raw material. The invention is characterized in that: water is added for extracting, decompressing or atmospheric concentration and spray drying; then petroleum ether extraction, ethanol or ethyl acetate or butyl acetate extraction are made before concentrated and dried to get the mugwort flavonoids. The extracting process of mugwort flavonoids has the advantages of promoting to comprehensively use limited mugwort resource, stimulating farmers to develop plant industry of mugwort, increasing income of farmers, responding to plant grass and seeds, actively preventing water and soil loss and bringing great convenience.
Description
Technical field
The present invention relates to natural organic chemistry and extract the field, specifically a kind of production method of extracting the flavonoids of artemisia argyi compounds, and with the application of flavonoids of artemisia argyi as the medicine material of preparation treatment facial acne.
Background technology
Radix Artemisia ordosicae wild or artificial growth has very strong antibacterial action, and the Radix Artemisia ordosicae sootiness can be used for indoor sterilization.The Radix Artemisia ordosicae effective ingredient is hindered bacillus, bacillus pyocyaneus, bacillus subtilis, Bacillus alcaligenes and tubercule bacillus (human-like H to staphylococcus aureus, beta hemolytic streptococcus, escherichia coli, Bacillus proteus, diphtheria corynebacterium, typhoid fever and pair
37RV) all kill or inhibitory action.The traditional Chinese medical science or custom among the people are twisted into Radix Artemisia ordosicae that rod point uses the sootiness wound and other focus reaches the purpose of healing, though with the Radix Artemisia ordosicae sootiness, for multiple pathomycete inhibitory action is arranged also, this primary using method was both dangerous, not environmental protection again.
Radix Artemisia ordosicae effective ingredient-flavone compound is carried out extraction separation, and, do not see bibliographical information as the medicine material of producing or prepare the treatment facial acne.
Summary of the invention
The object of the present invention is to provide a kind of reasonable development, utilize the Radix Artemisia ordosicae resource, the flavonoids of artemisia argyi extraction process that the stronger flavone compound of resistance against diseases in the Radix Artemisia ordosicae is effectively extracted.
Another object of the present invention is to provide of the application of a kind of flavonoids of artemisia argyi as the medicine material of producing or prepare the treatment facial acne.
For achieving the above object, the technical scheme taked of the present invention is:
A kind of extraction process of flavonoids of artemisia argyi is a raw material with the Radix Artemisia ordosicae, and this technology may further comprise the steps:
1. extract and take by weighing the Radix Artemisia ordosicae that portion crushes, join in the extraction pot, add 5～10 times water, be heated to 90～100 ℃ of reflux, extract, while stirring 30～60 minutes, stop heating then, leach extracting solution, pump into and wait in the concentration tank to concentrate; For the second time add 4～10 times of water in the extraction pot and continued to be heated to 90～100 ℃ of reflux, extract, 30～60 minutes, filter, filtrate pumps in the concentration tank and prepares to concentrate with extracting solution merging for the first time;
2. concentrate the felon herb raffinate that step is pumped into concentration tank in 1., ℃ reduce pressure in warming while stirring to 80～100 or normal pressure concentrates, and it is 40 of mass fraction～60% o'clock that the concentration of concentrated solution is concentrated into solid content, closes heating system, stop to concentrate, pump in temporary jar and prepare spray drying;
3. dry with 2. middle decompression of above-mentioned steps or the concentrated good felon herb raffinate of normal pressure, pump into and carry out spray drying in the spray drying tower, the control inlet temperature is between 110～180 ℃, and leaving air temp is between 60～90 ℃, and dried biennial wormwood extract moisture mass fraction should be controlled in 6%;
4. extraction
A, petroleum ether extraction
Take by weighing the 3. middle good biennial wormwood extract powder of spray drying of a above-mentioned steps, join in the extraction container, the petroleum ether that adds 60～90 ℃ of 5～10 times of boiling ranges simultaneously, be heated to 60～95 ℃ with water-bath, heating system is closed in reflux extraction 30～60 minutes, open vacuum pump, make the negative pressure that produces 0.001～0.005MPa in the extraction container, Open valve, it is medium to be recycled to allow petroleum ether flow into recycling can automatically; Add for the second time the petroleum ether of 3～10 times of equal boiling ranges, stirring and washing 5～10 minutes takes negative pressure to leach petroleum ether to recycling can then equally, waits to be recycled; Further use heating in water bath biennial wormwood extract to 60～95 ℃, make the petroleum ether volatilization that remains in the biennial wormwood extract surface, after condensation, reclaim unrecovered oil ether again;
B, ethanol or ethyl acetate or n-butyl acetate extraction
Get the biennial wormwood extract powder portion that above-mentioned steps a handles well with petroleum ether, join in the extraction pot, with 5～10 times of ethanol or ethyl acetate or butyl acetate, be heated to 60～95 ℃ with water-bath, heating system is closed in reflux extraction 30～60 minutes, heat filtering obtains pending mother solution;
5. concentrate, drying gets the mother solution that step is extracted with ethanol or ethyl acetate or butyl acetate in 4., adds in the concentration tank, the 300～750mmHg that reduces pressure is concentrated into paste, stop to concentrate, emit concentrate, under 85～105 ℃, carry out drying, dry thing through pulverize finished product.
Product index:
1. physical and chemical index:
Sense organ: pale brown, buff powder
Moisture :≤12.0%
Ash :≤2.5%
Alcohol soluble substance: 〉=98%
2. microbiological indicator:
Total number of bacteria :≤1000cfu/g
Coliform MPN/100g :≤40
Salmonella: must not detect
Pathogenic bacterium: must not detect
3. heavy metal index:
Arsenic (in As) :≤0.0002%
Plumbous (in Pb) :≤0.002%
A kind of flavonoids of artemisia argyi is as the application of the medicine material of producing or prepare the treatment facial acne, and is through clinical verification, evident in efficacy.
Clinical practice: get the flavonoids of artemisia argyi that above-mentioned technology is extracted, use distilled water: the ratio of medical ethanol=1: 1.5～3 is mixed with the concentration mass fraction and is respectively: 0.5%, 1.0% externally applied liniment 0.3%,, respectively with volunteer 10 people/groups, 5 male 5 woman/groups (age is between 16～45 years old), totally 4 groups, wherein 1 group of experimental group in contrast carries out facial patients with acne external curing test.Through 3 times/day, continuous 15 days on probation, and the result shows: 0.3% group of 10 philtrum 15 days the time have 9 people (1 44 years old women feels to begin several days effectively, several days subsequently do not have effect) facial acne obviously to cure, the every bit of long acne has incrustation, decortication phenomenon, and skin color is more just in convalescent period; 0.5% group of 10 philtrum has 7 days rear face acnes of 9 people (1 people is stolen together with bag with medicine) medication to begin incrustation, occurs the scaling phenomenon after 12 days, the skin part of long acne is that color is slightly dark than other position skin after 15 days; 1.0% group of 10 philtrum has 5 days rear face acnes of 9 people (1 people does not use because of going on business on time) medication on time to begin incrustation, occurs the scaling phenomenon after 10 days, the skin part of long acne is that color is slightly dark than other position skin after 12 days; Matched group after 15 days everyone facial acne do not have significant change.
The extraction process of above-mentioned flavonoids of artemisia argyi provided by the invention and application thereof, to promote the limited Radix Artemisia ordosicae resource of comprehensive utilization, stimulate the peasant to develop Radix Artemisia ordosicae plant husbandry, increase farmers' income, respond planting grasses and trees, preventing erosion plays a positive role.Simultaneously flavonoids of artemisia argyi is used to prepare the medicine material of treatment facial acne, brings great convenience for people's use.
The specific embodiment
Below in conjunction with embodiment the present invention is further elaborated.
Embodiment 1:
1. extract
Take by weighing the Radix Artemisia ordosicae that portion crushes, join in 20 liters of rustless steel multi-function extractors, add 5 times water, be heated to 90 ℃ of reflux, extract, while stirring 60 minutes, stop heating then and leach extracting solution, pump into and wait in the concentration tank to concentrate; For the second time add 4 times of water in the extraction pot and continued to be heated to 90 ℃ of reflux, extract, 60 minutes, filter, filtrate pumps in the concentration tank and prepares to concentrate with extracting solution merging for the first time.
2. concentrate
Above-mentioned steps 1. in first and second time extraction and filter good felon herb raffinate in concentration tank, warming while stirring to 95 ℃ concentrates, and when the concentrated solution solid content is controlled at mass fraction 60%, closes heating system, stop to concentrate, pump in temporary jar and prepare spray drying.
3. dry
The 2. middle good felon herb raffinate of concentrating under reduced pressure of above-mentioned steps pumps into (water evaporation quantity 3～5kg/h) in the centrifugal spray drying tower high speed nebulizer, open heating system, between 110 ℃ of the control inlet temperature, leaving air temp carries out spray drying for 60 ℃, and dried biennial wormwood extract moisture mass fraction should be controlled in 6%.
4. extraction
A, petroleum ether extraction
Take by weighing the 3. middle good biennial wormwood extract powder of spray drying of a above-mentioned steps, join in the 3000ml three footpath bottles, add 60～90 ℃ of petroleum ether of 5 times of boiling ranges, load onto spherical condensation tube, electronic stirring, Beckman thermometer, be heated to 65 ℃ of reflux extractions 60 minutes with water-bath.Close heating system, stop heating, remove Beckman thermometer, load onto negative pressure and mix suction pipe, open vacuum pump, make the negative pressure that produces 0.005MPa in the 3000ml three footpath bottles, Open valve, it is medium to be recycled to allow petroleum ether flow into returnable bottle automatically; The petroleum ether that adds for the second time 3 times, stirring and washing 10 minutes, it is to be recycled to take negative pressure to leach petroleum ether etc. then equally; Further biennial wormwood extract is heated to 65 ℃ with water-bath, make the petroleum ether volatilization that remains in the biennial wormwood extract surface, after condensation, also it is reclaimed again, can be removed alkanes, volatile oil, waxiness class material in the biennial wormwood extract like this, to guarantee the purity of flavone compound.
B, alcohol extraction
Get the biennial wormwood extract powder portion that above-mentioned steps a handles well with petroleum ether, join in the 3000ml three footpath bottles, add 5 times of volume of ethanol simultaneously, load onto spherical condensation tube, electronic stirring, Beckman thermometer, be heated to 95 ℃ of reflux extractions 60 minutes with water-bath.Close heating system, stop heating, heat filtering obtains pending mother solution, and residue is to be recycled.
5. concentrated, dry
Get above-mentioned steps 4. with the good mother solution of ethanol extraction, join in the 3000ml round-bottomed flask, be concentrated into paste with Rotary Evaporators decompression (300mmHg that begins to reduce pressure progressively brings up to 700mmHg with negative pressure after 5 times of volume ethanol concentrate out 4 times), stop to concentrate, pour into and under 85 ℃, place drying baker dry in the pallet, dry thing through pulverize product.
Embodiment 2:
1. extract
Take by weighing the Radix Artemisia ordosicae that portion crushes, join in 20 liters of rustless steel multi-function extractors, add 7 times water, be heated to 95 ℃ of reflux, extract, while stirring 45 minutes, stop heating then and leach extracting solution, pump into and wait in the concentration tank to concentrate; For the second time add 7 times of water in the extraction pot and continued to be heated to 95 ℃ of reflux, extract, 45 minutes, filter, filtrate pumps in the concentration tank and prepares to concentrate with extracting solution merging for the first time.
2. concentrate
Above-mentioned steps 1. in first and second time extraction and filter good felon herb raffinate in the concentrating under reduced pressure jar, concentrating under reduced pressure ℃ is carried out in warming while stirring to 80, open vacuum pump and reduce pressure, vacuum is remained on about 750mmHg, when the concentrated solution solid content is controlled at mass fraction 50% while concentrating.Close heating system, stop to concentrate, pump in temporary jar and prepare spray drying.
3. dry
The 2. middle good felon herb raffinate of concentrating under reduced pressure of above-mentioned steps, (water evaporation quantity 3～5kg/h) in the pump-in pressure formula spray drying tower high speed nebulizer, open heating system, 150 ℃ of control inlet temperature, leaving air temp carries out spray drying for 70 ℃, and dried biennial wormwood extract moisture mass fraction should be controlled in 6%.
4. extraction
A, petroleum ether extraction
Take by weighing the 3. middle good biennial wormwood extract powder of spray drying of a above-mentioned steps, join in the 3000ml three footpath bottles, add the petroleum ether of 60～90 ℃ of 7 times of boiling ranges, load onto spherical condensation tube, electronic stirring, Beckman thermometer, be heated to 85 ℃ of reflux extractions 45 minutes with water-bath.Close heating system, stop heating, remove Beckman thermometer, load onto negative pressure and mix suction pipe, open vacuum pump, make the negative pressure that produces 0.003MPa in the 3000ml three footpath bottles, Open valve, it is medium to be recycled to allow petroleum ether flow into returnable bottle automatically; The petroleum ether that adds for the second time 7 times, stirring and washing 8 minutes, it is to be recycled to take negative pressure to leach petroleum ether etc. then equally; Petroleum ether to the biennial wormwood extract remained on surface is also reclaimed.
B, ethyl acetate extraction
Get the biennial wormwood extract powder portion that above-mentioned steps a handles well with petroleum ether, join in the 3000ml three footpath bottles, the ethyl acetate that adds 7 times of volumes is simultaneously loaded onto spherical condensation tube, electronic stirring, Beckman thermometer, is heated to 85 ℃ of reflux extractions 45 minutes with water-bath.Close heating system, stop heating, heat filtering obtains pending mother solution, and residue reclaims.
5. concentrated, dry
Get above-mentioned steps 4. in the good mother solution of ethyl acetate extraction, join in the 3000ml round-bottomed flask, be concentrated into paste with the Rotary Evaporators 300mmHg that reduces pressure, stop to concentrate, pour in the pallet dry in drying baker under 95 ℃, dry thing through pulverize product.
Embodiment 3:
1. extract
Take by weighing the Radix Artemisia ordosicae that portion crushes, join in 20 liters of rustless steel multi-function extractors, add 10 times water, be heated to 100 ℃ of reflux, extract, while stirring 30 minutes, stop heating then, leach extracting solution, pump into and wait in the concentration tank to concentrate.For the second time add 10 times of water in the extraction pot and continued to be heated to 100 ℃ of reflux, extract, 30 minutes, filter, filtrate pumps in the concentration tank and prepares to concentrate with extracting solution merging for the first time.
2. concentrate
Above-mentioned steps 1. in first and second time extraction and filter good felon herb raffinate in the concentrating under reduced pressure jar, concentrating under reduced pressure ℃ is carried out in warming while stirring to 100, open vacuum pump and reduce pressure while concentrating, vacuum is remained on about 750mmHg, the concentrated solution solid content is controlled at mass fraction 40%.Close heating system, stop to concentrate, pump in temporary jar and prepare spray drying.
3. dry
The 2. middle good felon herb raffinate of concentrating under reduced pressure of above-mentioned steps pumps into (water evaporation quantity 3～5kg/h) in the spray drying tower high speed nebulizer, open heating system, 180 ℃ of control inlet temperature, leaving air temp carries out spray drying for 90 ℃, and dried biennial wormwood extract moisture mass fraction should be controlled in 6%.
4. extraction
A, petroleum ether extraction
Take by weighing the 3. middle good biennial wormwood extract powder of spray drying of a above-mentioned steps, join in the 3000ml three footpath bottles, the petroleum ether that adds 60～90 ℃ of 10 times of boiling ranges is loaded onto spherical condensation tube, electronic stirring, Beckman thermometer, is heated to 95 ℃ of reflux extractions 30 minutes with water-bath.Close heating system, stop heating, remove Beckman thermometer, load onto negative pressure and mix suction pipe, open vacuum pump, make the negative pressure that produces 0.001MPa in the 3000ml three footpath bottles, Open valve, it is medium to be recycled to allow petroleum ether flow into returnable bottle automatically; The petroleum ether that adds for the second time 10 times, stirring and washing 5 minutes, it is to be recycled to take negative pressure to leach petroleum ether etc. then equally; Petroleum ether to the biennial wormwood extract remained on surface is also reclaimed.
B, n-butyl acetate extraction
Get the biennial wormwood extract powder portion that above-mentioned steps a handles well with petroleum ether, join in the 3000ml three footpath bottles, the butyl acetate that adds 10 times of volumes is simultaneously loaded onto spherical condensation tube, electronic stirring, Beckman thermometer, is heated to 95 ℃ of reflux extractions 30 minutes with water-bath.Close heating system, stop heating, heat filtering, obtain pending mother solution, residue reclaims separately.
5. concentrated, dry
Get the mother solution that above-mentioned steps is extracted with butyl acetate in 4., join in the 3000ml round-bottomed flask, be concentrated into paste, stop to concentrate with the Rotary Evaporators 750mmHg that reduces pressure, pour into and under 105 ℃, place drying baker dry in the pallet, dry thing through pulverize product.
Claims (2)
1. the extraction process of a flavonoids of artemisia argyi is characterized in that with the Radix Artemisia ordosicae being raw material, and this technology may further comprise the steps:
1. extract and take by weighing the Radix Artemisia ordosicae that portion crushes, join in the extraction pot, add 5～10 times water, be heated to 90～100 ℃ of reflux, extract, while stirring 30～60 minutes, stop heating then, leach extracting solution, pump into and wait in the concentration tank to concentrate; For the second time add 4～10 times of water in the extraction pot and continued to be heated to 90～100 ℃ of reflux, extract, 30～60 minutes, filter, filtrate pumps in the concentration tank and prepares to concentrate with extracting solution merging for the first time;
2. concentrate the felon herb raffinate that step is pumped into concentration tank in 1., ℃ reduce pressure in warming while stirring to 80～100 or normal pressure concentrates, and it is 40 of mass fraction～60% o'clock that the concentration of concentrated solution is concentrated into solid content, closes heating system, stop to concentrate, pump in temporary jar and prepare spray drying;
3. dry with 2. middle decompression of above-mentioned steps or the concentrated good felon herb raffinate of normal pressure, pump into and carry out spray drying in the spray drying tower, the control inlet temperature is between 110～180 ℃, and leaving air temp is between 60～90 ℃, and dried biennial wormwood extract moisture mass fraction should be controlled in 6%;
4. extraction
A, petroleum ether extraction
Take by weighing the 3. middle good biennial wormwood extract powder of spray drying of a above-mentioned steps, join in the extraction container, the petroleum ether that adds 60～90 ℃ of 5～10 times of boiling ranges simultaneously, be heated to 60～95 ℃ with water-bath, heating system is closed in reflux extraction 30～60 minutes, open vacuum pump, make the negative pressure that produces 0.001～0.005MPa in the extraction container, Open valve, it is medium to be recycled to allow petroleum ether flow into recycling can automatically; Add for the second time the petroleum ether of 3～10 times of equal boiling ranges, stirring and washing 5～10 minutes takes negative pressure to leach petroleum ether to recycling can then equally, waits to be recycled; Further biennial wormwood extract is heated to 60～95 ℃, makes the petroleum ether volatilization that remains in the biennial wormwood extract surface, after condensation, reclaim unrecovered oil ether again with water-bath;
B, ethanol or ethyl acetate or n-butyl acetate extraction
Get the biennial wormwood extract powder portion that above-mentioned steps a handles well with petroleum ether, join in the extraction pot, with 5～10 times of ethanol or ethyl acetate or butyl acetate, be heated to 60～95 ℃ with water-bath, heating system is closed in reflux extraction 30～60 minutes, heat filtering obtains pending mother solution;
5. concentrate, drying gets the mother solution that step is extracted with ethanol or ethyl acetate or butyl acetate in 4., adds in the concentration tank, the 300～750mmHg that reduces pressure is concentrated into paste, stop to concentrate, emit concentrate, under 85～105 ℃, carry out drying, dry thing through pulverize finished product.
2. the application of flavonoids of artemisia argyi in preparation treatment facial acne medicine that obtains according to the described extraction process of claim 1.
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| KR101326932B1 (en) * | 2009-11-26 | 2013-11-11 | (주)아모레퍼시픽 | Composition for Promotion of Peroxisome proliferator activated receptor delta |
| CN102600225B (en) * | 2012-04-20 | 2013-10-16 | 河南省医药科学研究院 | Wormwood leaf extract and application thereof in preparation of anti-hepatitis B virus medicines |
| CN102716380B (en) * | 2012-07-04 | 2013-10-30 | 甘肃省商业科技研究所 | Compound acne-removal cream and production method thereof |
| CN103340917A (en) * | 2013-06-15 | 2013-10-09 | 安徽盛海堂中药饮片有限公司 | Extraction method for flavonoids in mugwort |
| CN105816709A (en) * | 2016-04-11 | 2016-08-03 | 安徽仁之堂药业有限公司 | High efficient preparation method of traditional Chinese medicine massa medicata fermentata formula granules |
| CN111548531A (en) * | 2020-06-15 | 2020-08-18 | 南京淳达科技发展有限公司 | Special linear material auxiliary agent for core-layer CPE packaging film and preparation method thereof |
| CN116941642A (en) * | 2023-05-22 | 2023-10-27 | 广州奕华生物科技有限公司 | Preparation method and application of natural plant bacteriostat |
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