Summary of the invention
Purpose of the present invention aims to provide and a kind ofly can make full use of caffeic acid derivant high-quality percentage ratio in the Echinacea raw material growth course, helps the abundant extraction of effective ingredient, improves yield, the preparation method of the Echinacea extract that reduces cost.
The objective of the invention is to realize by following manner:
What raw material adopted is the Echinacea herb of fresh state, through extracting, concentrate Echinacea extract.
The inventor discover the present invention adopt the Echinacea of fresh bud stage blade, alabastrum and wounded in the battle side shoot extract best in quality, yield is best.
Above raw material is through alcohol extraction, and alcoholic solvent reclaims, and obtains Echinacea extract behind the extracting solution concentrate drying.
Fresh state is in the Echinacea aerial parts of bud stage, or is in the blade of the bud stage Echinacea of fresh state, includes alabastrum and wounded in the battle side shoot, gets squeezeding juice and raw material slag through cold pressing, and squeezeding juice concentrates, and drying is Echinacea extract.
The raw material slag is through alcohol extraction, and alcoholic solvent reclaims, and extracting solution concentrates, and drying obtains the extract of Echinacea.
Raw material slag after described the squeezing the juice was with the reflux, extract, of 70%-95% ethanol or methanol 2 times, each 1~4 hour.The extracting solution concentrating under reduced pressure, is Echinacea extract after drying at solvent recovery.
Described cold pressing is to mix with fresh Echinacea with the water of weight ratio 1~2: 1.
Described squeezeding juice after macroporous resin adsorption with the Different concentrations of alcohol eluting, get eluent, eluent reclaims, concentrates, and is Echinacea extract after the drying, and is refining that total caffeic acid derivant quality percentage ratio is the Echinacea extract of 10%-60% through ethyl acetate again.
The root of the Echinacea of fresh state through water or alcohol extraction, obtains Echinacea extract behind the extracting solution concentrate drying.
The root of the Echinacea of fresh state through squeeze the juice squeezeding juice and slag, after squeezeding juice drying or the lyophilizing Echinacea root juice powder, squeeze the juice slag behind alcohol or water extraction, reclaim, concentrate, dry Echinacea root extract.
The present invention has realized extracting total caffeic acid derivant to greatest extent from Echinacea, has simplified the Technology flow process of extracting purification, has saved production cost, and the deep development for the Echinacea product provides infrastructural support simultaneously.
In the raw material of Echinacea was investigated, the inventor had crucial discovery, and promptly the mass fraction of the chicoric acid of caffeic acid derivant exceeds 2.5~5.5 times than the plant after drying in the fresh plant.Concrete data see the following form.
|
Seedling |
Flower in earlier stage |
Alabastrum |
Just spend |
Contain flower |
Wither |
Bright product (meter of giving money as a gift) |
3.4 |
2.7 |
4.6 |
4.1 |
3.5 |
2.2 |
Dry product (meter of giving money as a gift) |
0.8 |
0.6 |
1.7 |
1.35 |
1.27 |
0.4 |
No matter which growth period the Echinacea plant is in as can be seen from the above table, and the content of its bright product all is higher than the content of dry product.
Technology of the present invention is simple, and effective ingredient can farthest be kept.The present invention has adopted the Echinacea of fresh state as extracting raw material; In the general used former plant of drying in the sun, the chicoric acid content of caffeic acid derivant (meter of giving money as a gift) is in 0.01%~1.5% scope, and the inventor discovers that by experiment the chicoric acid content (meter of giving money as a gift) of genus coffea acid derivative in the fresh former plant can reach 1%~4.5%, as seen both gaps are fairly obvious, because original raw material causes the forfeiture of the effective ingredient of Echinacea in daily dry run.The inventor discovers that also the bud stage that is accumulated in of Echinacea secondary metabolite caffeic acid derivant is a top level in addition, especially in blade and alabastrum.Thereby the inventor adopts fresh Echinacea to extract, especially the blade of bud stage, alabastrum and to contain colored side shoot be optimum feed stock.The present invention can save material and manufacturing cost greatly owing to the content of the extract effective ingredient caffeic acid derivant that has adopted fresh Echinacea raw material to make is much higher than the extract of being made by dry product, helps the purification of subsequent handling.Its correlational study of the present invention yet there are no relevant report.
The inventor is by following experimentation, and having determined to be in the bud stage Echinacea is that the best of wanting required for the present invention is collected the stage.
We pass through the investigation to the whole growth cycle of fresh medical material, find effective biological total amount the highest period, to reach the reduction industrial production cost, increase the purpose of product profit, the fresh medical material that found that the Echinacea of bud stage is the optimum feed stock condition mode.(seeing accompanying drawing)
The specific embodiment
Embodiment 1
Choose fresh, do not have the yellow aerial parts that withers, do not have addling, is in the Echinacea plant of bud stage, after the chopping, with 95% ethanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, reclaims solvent, concentrates, dry chicoric acid mass fraction is 6% Echinacea extract.
Embodiment 2
Choose fresh, do not have the yellow aerial parts that withers, do not have addling, is in the Echinacea plant of bud stage, after the chopping, with the methanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, concentrates, dry chicoric acid mass fraction is 5% Echinacea extract.
Embodiment 3
The Echinacea extract of total chicoric acid mass fraction 6% that embodiment 1 is obtained is through ethyl acetate extraction 3 times, and it is 17% Echinacea extract that concentrate drying promptly gets total chicoric acid mass fraction.
Embodiment 4
Choose fresh, do not have the yellow aerial parts that withers, do not have addling, is in the Echinacea plant of seedling phase, after the chopping, with 90% ethanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, reclaims, concentrates, cooling, standing separation get precipitate, and it is 5% Echinacea extract that drying precipitate is got total chicoric acid mass fraction.
Embodiment 5
Choose fresh, do not have the yellow aerial parts that withers, do not have addling, is in the Echinacea plant of full-bloom stage, after the chopping, with 90% ethanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, reclaims, concentrates, cooling, standing separation get precipitate, and it is 4% Echinacea extract that drying precipitate is got the chicoric acid mass fraction.
Embodiment 6
Choose fresh, do not have the yellow aerial parts that withers, do not have addling, is in the Echinacea plant of blossom fall phase, after the chopping, with 90% ethanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, reclaims, concentrates, cooling, standing separation get precipitate, and it is 4% Echinacea extract that drying precipitate is got the chicoric acid mass fraction.
Embodiment 7
Choose fresh, as not have the Echinacea plant that yellowly withers, do not have addling, is in bud stage leaf and alabastrum, alabastrum side shoot part, after the chopping, with 90% ethanol of 2 times of bright medical material weight reflux, extract, together 2 times, each 2 hours.Merge extractive liquid, reclaims, concentrates, cooling, standing separation get precipitate, and it is 9% Echinacea extract that drying precipitate is got the chicoric acid mass fraction.
Embodiment 8
Choose fresh, do not have a yellow aerial parts that withers, do not have addling, is in the Echinacea plant of bud stage.With weight ratio is the water and the fresh plant input juice extractor of 2 times of amounts.The back filter pressing separation of squeezing the juice obtains squeezeding juice and raw material slag.Squeezeding juice concentrates, obtain the chicoric acid mass fraction after the drying is 3% Echinacea extract.
Embodiment 9
The raw material slag part that embodiment 8 is obtained is with methanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, concentrates, promptly gets the extract that contains total caffeic acid derivant 7% after the drying.Be 20% Echinacea extract with this Echinacea extract with the refining chicoric acid mass fraction that obtains of ethyl acetate backflow again.
After squeezeding juice is crossed macroporous resin adsorption,, reclaim, concentrate, promptly get total chicoric acid mass fraction after the drying and be 30% Echinacea extract again with 3 times of column volumes of ethanol elution of 80%, and with eluent earlier with 3 times of column volumes of ethanol elution (putting in addition) of 10%.This extract with ethyl acetate backflow twice, is obtained the chicoric acid mass fraction and is 45% Echinacea extract.
Embodiment 10
The raw material slag part that embodiment 9 is obtained is with 95% ethanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, obtains the chicoric acid mass fraction after the drying and be 7% Echinacea extract.
Embodiment 11
Choose fresh, do not have yellow leaf and the wounded in the battle side shoot part of withering, not having addling, be in the Echinacea plant of blossom fall phase, be the water and the fresh plant input juice extractor of 2 times of amounts with weight ratio.Obtain squeezeding juice and raw material slag with the separation of cylinder filter press technique after squeezing the juice.
With raw material slag part with 90% ethanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, obtains containing the chicoric acid mass fraction after the drying and be 9% Echinacea extract.
After squeezeding juice is crossed macroporous resin,, reclaim, concentrate, promptly get total chicoric acid mass fraction after the drying and be 6% Echinacea extract again with 3 times of column volumes of ethanol elution of 90%, and with eluent earlier with 3 times of column volumes of ethanol elution (putting in addition) of 10%.
Embodiment 12
Choose fresh, do not have a yellow aerial parts that withers, do not have addling, is in the Echinacea plant of seedling phase.With weight ratio is the water and the fresh plant input juice extractor of 1 times of amount.The back filter pressing of squeezing the juice obtains squeezeding juice and raw material slag.
With raw material slag part with 90% ethanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, after the drying the chicoric acid mass fraction be 5% Echinacea extract.
After squeezeding juice is crossed macroporous resin,, reclaim, concentrate, promptly get total chicoric acid mass fraction after the drying and be 20% Echinacea extract again with 3 times of column volumes of ethanol elution of 90%, and with eluent earlier with 3 times of column volumes of ethanol elution (putting in addition) of 10%.
Embodiment 13
Choose fresh, do not have a yellow aerial parts that withers, do not have addling, is in the Echinacea plant of anthesis.With weight ratio is the water and the fresh plant input juice extractor of 2 times of amounts.The filter pressing of squeezing the juice obtains squeezeding juice and raw material slag.
With raw material slag part with 90% ethanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, obtains containing the chicoric acid mass fraction after the drying and be 4% Echinacea extract.
After squeezeding juice is crossed macroporous resin,, reclaim, concentrate, promptly get total chicoric acid mass fraction after the drying and be 18% Echinacea extract again with 3 times of column volumes of ethanol elution of 90%, and with eluent earlier with 3 times of column volumes of ethanol elution (putting in addition) of 10%.
Embodiment 14
Choose fresh, do not have a yellow aerial parts that withers, do not have addling, is in the Echinacea plant of blossom fall phase.With weight ratio is the water and the fresh plant input juice extractor of 2 times of amounts.Obtain squeezeding juice and raw material slag with the separation of cylinder filter press technique after squeezing the juice.
With raw material slag part with 90% ethanol, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, obtains containing the chicoric acid mass fraction after the drying and be 2% Echinacea extract.
After squeezeding juice is crossed macroporous resin,, reclaim, concentrate, promptly get total chicoric acid mass fraction after the drying and be 12% Echinacea extract again with 3 times of column volumes of ethanol elution of 90%, and with eluent earlier with 3 times of column volumes of ethanol elution (putting in addition) of 10%.
Embodiment 15
Choose the root of fresh Echinacea, the ethanol with 95%, reflux, extract, 2 times, each 2 hours.The extracting solution concentrating under reduced pressure is recovered to does not have alcohol flavor substantially, and drying obtains total chicoric acid mass fraction and be 4% Echinacea extract.
Embodiment 16
Choose the root of fresh Echinacea, water is squeezed the juice.With the squeezeding juice concentrating under reduced pressure, a part is dry, obtains total chicoric acid mass fraction and be 2% Echinacea root juice powder, and it is 3% Echinacea extract that another part lyophilizing gets the chicoric acid mass fraction.
Embodiment 17
After the squeezeding juice of embodiment 16 crossed macroporous resin,, reclaim, concentrate, promptly get the Echinacea root extract after the drying again with 3 times of column volumes of ethanol elution of 80%, and with eluent earlier with 3 times of column volumes of ethanol elution of 10%.This extract with ethyl acetate backflow twice, is obtained total chicoric acid mass fraction and is 15% Echinacea root extract.