CN103073912A - Method for preparing purified azalea from rhododendron dauricum - Google Patents
Method for preparing purified azalea from rhododendron dauricum Download PDFInfo
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- CN103073912A CN103073912A CN2012105953438A CN201210595343A CN103073912A CN 103073912 A CN103073912 A CN 103073912A CN 2012105953438 A CN2012105953438 A CN 2012105953438A CN 201210595343 A CN201210595343 A CN 201210595343A CN 103073912 A CN103073912 A CN 103073912A
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Abstract
The invention discloses a method for preparing purified azalea from rhododendron dauricum. The method comprises the following steps: crushing the azalea into coarse powder, adding 85% methanol with the amount 15 times that of the coarse powder, performing reflux extraction for 120 minutes, and filtering; concentrating the filtrate to 3 baume after methanol recovery, adjusting the pH value of the concentrated liquor to 2.5 with a solution of which the volume ratio of hydrochloric acid to water is 1 to 1, standing for 20 minutes, and filtering; passing the filtrate through a broad spectrum macroporous resin absorption column, collecting the eluate, recovering methanol from the eluate, and concentrating and drying the eluate to obtain a azalea semi-finished product; passing the obtained azalea semi-finished product through a silica gel column, and washing out impurities with a solution of which the volume ratio of acetone to methanol is 3 to 1, and then eluting with a solution of which the volume ratio of acetone to methanol is 7 to 1, and collecting the eluate; refining the collected azalea eluate to obtain an azalea finished product, of which the content of azalea is more than 70%. The method is mainly characterized by utilizing macroporous resin-silica gel chromatography, so that coupling is convenient and quick, sources of raw materials are extensive, production cost is low, separation effect is obvious, and extraction purity is high.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to the method that a kind of Folium Cuculus polioephalus prepares azalea, particularly relate to and a kind ofly utilize macroporous adsorbent resin co-solvent extraction to prepare the method for purifying azalea.
Background technology:
Folium Cuculus polioephalus Rhododendron dauricum, call Rhododendron dauricum, reach fragrant, the Da Daxiang of son, the high 1～2m of half evergreen shrubs, multi-branched.The leaf alternate, nearly keratin, oval oval to the ovum shape, long 1.5～3.5cm, full edge.Spend 1～4 to give birth to the branch top.The corolla funnel-form, red-violet colour, diameter 2.5～3.5cm.Leaf contains perfume oil and tonka bean camphor etc., the available perfume oil of carrying, modulation essence; Also be used as medicine bitter cold in nature.Has the cough-relieving apophlegmatic function, the treating acute and chronic bronchitis.Stem, bar, fruit contain careless tannin, can obtain through refining tannin extract.
Azalea is a kind of tree peony anthocyanins that extracts purifying and get from natural phant, is natural pigment, the color and luster nature, and tint permanence is good, mainly is used as the tinting material of beverage, candy, jam and cake etc.In recent years, it is found that and contain a large amount of azalea pigments in the natural phant cuckoo, therefrom extract the azalea pigment and obtained encouraging progress that raw material cuckoo source is wider.
Summary of the invention
The object of the invention is to provide a kind of Folium Cuculus polioephalus to prepare the method for purifying azalea; The object of the invention also be to provide a kind of convenient and swift, raw material sources abundant, low production cost, separating effect is obvious, dna purity the is high method of utilizing macroporous adsorbent resin-silica gel column chromatography coupled method enriching and purifying azalea.
The present invention seeks to be achieved through the following technical solutions.
The method that Folium Cuculus polioephalus of the present invention prepares the purifying azalea comprises the steps:
Rhododendron is ground into meal, and 85%～100% methanol eddy that adds 15～20 times of amounts of meal quality extracted 120～180 minutes, filtered; Be concentrated into 3～5 Baumes behind the filtrate recovery methyl alcohol and get concentrated solution, then use 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 2.5～3 with concentrated solution pH value, places after 20～40 minutes to filter; HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5%～20% methyl alcohol again, then use 50%～80% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1～3: 1 acetone and carbinol mixture are washed impurity, and then use acetone: the volume ratio of methyl alcohol is 5～7: 1 acetone and carbinol mixture wash-out, gets the azalea elutriant; The azalea elutriant is made with extra care to get azalea, and its content is more than 70%.
The method that Folium Cuculus polioephalus of the present invention prepares the purifying azalea comprises the steps:
Take by weighing the rhododendron that is ground into meal, 85% methanol eddy that adds 20 times of amounts of meal quality extracted 180 minutes, filtered; Be concentrated into 5 Baumes behind the filtrate recovery methyl alcohol and get concentrated solution, then use 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 3 with concentrated solution pH value, places after 40 minutes to filter; HPD400 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5% methyl alcohol again, then use 50% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 5: 1 acetone and carbinol mixture wash-out, gets the azalea elutriant; The azalea elutriant is made with extra care to get azalea.
Described macroporous resin adsorption step adopts wet method dress post, keeps liquid level, and the filtrate behind the adjust pH is passed through adsorption column, flow velocity per minute 0.05ml/g resin.
Described silica gel column chromatography step adopts wet method dress post, keeps liquid level, work in-process are mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix is as for silicagel column top, elution flow rate per minute 0.1ml/g silica gel.The silica gel activating condition is, 110 degrees centigrade 30 minutes.
Adopt activated carbon decolorizing, recrystallization method to make with extra care among the present invention.Press the 4g/100ml elutriant and add injection active carbon, 25～40 degrees centigrade were stirred 20～40 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate; Intermediate is with 40 degrees centigrade of thermosols of 7～9 times of methyl alcohol, and filter: filtrate cools crystallize out, and suction filtration gets the azalea finished product.
Treating process comprises the steps: among the present invention
Press the 4g/100ml elutriant and add injection active carbon, 25 degrees centigrade were stirred 40 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate; Intermediate filters with 40 degrees centigrade of thermosols of 9 times of methyl alcohol; Filtrate cools crystallize out, and suction filtration gets the azalea finished product.
Finished product is with 7 times of recrystallizing methanol in the treating process among the present invention, and filtrated stock reclaims methyl alcohol, and concentrate drying gets the azalea work in-process.
The present invention uses macroporous adsorbent resin-silica gel column chromatography coupled method enriching and purifying azalea, and is good to the adsorption selectivity of azalea, and the fast parsing of absorption is also fast, and loading capacity is larger; Raw material sources are abundant, low production cost, and separating effect is obvious, and dna purity is high, can obtain azalea work in-process and content the azalea finished product 70% or more of content more than 45%, has overcome the shortcoming that conventional extraction yield is relatively low, dna purity is low.
The present invention selects that physico-chemical property is stable, surface-area is large, exchange velocity is very fast, physical strength is high, contamination resistance is strong, the macroporous adsorbent resin of Heat stability is good, be not dissolved in acid, alkali and organic matchmaker, better to the organism selectivity, the impact that not existed by inorganic salts and strong ion low molecular compound, can from solution, adsorb selectively azalea by physical adsorption, absorption is fast, parsing is also fast, and loading capacity is larger.
The present invention selects the silica gel chromatography purifying and in conjunction with gac and recrystallizing and refining, separating effect is better.
Embodiment:
Embodiment 1:
Take by weighing rhododendron 10kg, be ground into meal, the methanol eddy that adds 18 times of amounts 90% extracted 140 minutes, filtered; Filtrate is reclaimed methyl alcohol, is concentrated into 4 Baumes, and with 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 2.8 with concentrated solution pH value, places filtration 40 minutes; HPD100 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 15% methyl alcohol again, then use 70% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 2: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 6: 1 acetone and carbinol mixture wash-out, gets azalea elutriant 2L; Add the 80g injection active carbon, 30 degrees centigrade were stirred 30 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate 35g; Intermediate filters with 40 degrees centigrade of thermosols of 8 times of methyl alcohol, and filtrate cools crystallize out, and suction filtration gets azalea finished product 20g, content 73%.
Embodiment 2:
Take by weighing rhododendron 15kg, be ground into meal, the methanol eddy that adds 20 times of amounts 95% extracted 160 minutes, filtered; Filtrate is reclaimed methyl alcohol, is concentrated into 5 Baumes, and with 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 3 with concentrated solution pH value, places filtration 40 minutes; HPD400 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 10% methyl alcohol again, then use 60% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 7: 1 acetone and carbinol mixture wash-out, gets azalea elutriant 3.5L; Add the 140g injection active carbon, 40 degrees centigrade were stirred 40 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate 60g; Intermediate filters with 40 degrees centigrade of thermosols of 9 times of methyl alcohol, and filtrate cools crystallize out, and suction filtration gets azalea finished product 32g, content 71.3%.
Embodiment 3:
Take by weighing rhododendron 20kg, be ground into meal, the methanol eddy that adds 15 times of amounts 87% extracted 120 minutes, filtered; Filtrate is reclaimed methyl alcohol, is concentrated into 3 Baumes, and with 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 2.5 with concentrated solution pH value, places filtration 40 minutes; AB-8 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5% methyl alcohol again, then use 80% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 3: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 5: 1 acetone and carbinol mixture wash-out, gets azalea elutriant 5L; Add the 200g injection active carbon, 25 degrees centigrade were stirred 20 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate 70g; Intermediate filters with 40 degrees centigrade of thermosols of 8 times of methyl alcohol, and filtrate cools crystallize out, and suction filtration gets azalea finished product 36g, content 72.5%.
Embodiment 4:
Take by weighing rhododendron 5kg, be ground into meal, the methanol eddy that adds 20 times of amounts 98% extracted 160 minutes, filtered; Filtrate is reclaimed methyl alcohol, is concentrated into 3 Baumes, and with 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 2.6 with concentrated solution pH value, places filtration 40 minutes; DM-130 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5% methyl alcohol again, then use 50% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 7: 1 acetone and carbinol mixture wash-out, gets azalea elutriant 1200ml; Add the 48g injection active carbon, 40 degrees centigrade were stirred 25 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate 20g; Intermediate filters with 40 degrees centigrade of thermosols of 7 times of methyl alcohol, and filtrate cools crystallize out, and suction filtration gets azalea finished product 12g, content 73.2%.
Claims (7)
1. a Folium Cuculus polioephalus prepares the method for purifying azalea, it is characterized in that the method comprises the steps:
Rhododendron is ground into meal, and 85%～100% methanol eddy that adds 15～20 times of amounts of meal quality extracted 120～180 minutes, filtered; Be concentrated into 3～5 Baumes behind the filtrate recovery methyl alcohol and get concentrated solution, then use 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 2.5～3 with concentrated solution pH value, places after 20～40 minutes to filter; HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5%～20% methyl alcohol again, then use 50%～80% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1～3: 1 acetone and carbinol mixture are washed impurity, and then use acetone: the volume ratio of methyl alcohol is 5～7: 1 acetone and carbinol mixture wash-out, gets the azalea elutriant; The azalea elutriant is made with extra care to get azalea.
2. Folium Cuculus polioephalus as claimed in claim 1 prepares the method for purifying azalea, it is characterized in that the method comprises the steps:
Take by weighing the rhododendron that is ground into meal, 85% methanol eddy that adds 20 times of amounts of meal quality extracted 180 minutes, filtered; Be concentrated into 5 Baumes behind the filtrate recovery methyl alcohol and get concentrated solution, then use 1: 1 hydrochloric acid of volume ratio: the aqueous solution transfers to 3 with concentrated solution pH value, places after 40 minutes to filter; HPD400 type macroporous resin adsorption post on the filtrate, adsorb the complete impurity that washes with water, wash impurity with 5% methyl alcohol again, then use 50% methanol-eluted fractions, get azalea work in-process elutriant, concentrate drying got the azalea work in-process after azalea work in-process elutriant reclaimed methyl alcohol; With silica gel column chromatography on the gained azalea work in-process, and use acetone: the volume ratio of methyl alcohol is that 1: 1 acetone and carbinol mixture washed impurity, then uses acetone: the volume ratio of methyl alcohol is 5: 1 acetone and carbinol mixture wash-out, gets the azalea elutriant; The azalea elutriant is made with extra care to get azalea.
3. Folium Cuculus polioephalus as claimed in claim 1 or 2 prepares the method for purifying azalea, it is characterized in that the step of macroporous resin adsorption described in the method adopts wet method dress post, keep liquid level, the filtrate behind the adjust pH is passed through adsorption column, flow velocity per minute 0.05ml/g resin.
4. Folium Cuculus polioephalus as claimed in claim 1 or 2 prepares the method for purifying azalea, it is characterized in that the step of silica gel column chromatography described in the method adopts wet method dress post, keep liquid level, work in-process are mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix is as for silicagel column top, elution flow rate per minute 0.1ml/g silica gel.The silica gel activating condition is, 110 degrees centigrade 30 minutes.
5. Folium Cuculus polioephalus as claimed in claim 1 or 2 prepares the method for purifying azalea, it is characterized in that adopting in the method activated carbon decolorizing, recrystallization method to make with extra care, press 4g/100ml azalea elutriant and add injection active carbon, 25～40 degrees centigrade were stirred 20～40 minutes, filtered; Concentrate drying got intermediate after filtrate was reclaimed mix reagent; Intermediate is with 40 degrees centigrade of thermosols of 7～9 times of methyl alcohol, and filter: filtrate cools crystallize out, and suction filtration gets the azalea finished product.
6. Folium Cuculus polioephalus as claimed in claim 5 prepares the method for purifying azalea, it is characterized in that treating process comprises the steps: in the method
Press the 4g/100ml elutriant and add injection active carbon, 25 degrees centigrade were stirred 40 minutes, filtered; Filtrate is reclaimed mix reagent, and concentrate drying gets intermediate; Intermediate is with 40 degrees centigrade of thermosols of 9 times of methyl alcohol, and filter: filtrate cools crystallize out, and suction filtration gets the azalea finished product.
7. Folium Cuculus polioephalus as claimed in claim 6 prepares the method for purifying azalea, it is characterized in that in the method finished product with 7 times of recrystallizing methanol, and filtrated stock reclaims methyl alcohol, and concentrate drying gets the azalea work in-process.
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| CN201210595343.8A CN103073912B (en) | 2012-12-13 | 2012-12-13 | A kind of Folium Cuculus polioephalus prepares the method for purifying azalea |
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| CN201210595343.8A CN103073912B (en) | 2012-12-13 | 2012-12-13 | A kind of Folium Cuculus polioephalus prepares the method for purifying azalea |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038302A (en) * | 2014-08-10 | 2015-11-11 | 王选明 | Device for extracting rhododendron pigment |
| CN105440732A (en) * | 2015-11-06 | 2016-03-30 | 大兴安岭林格贝寒带生物科技股份有限公司 | Method for enriching and purifying carmine radish anthocyanin |
| CN112724702A (en) * | 2020-12-29 | 2021-04-30 | 贵州省植物园 | Method for extracting azalea pigment |
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Patent Citations (4)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038302A (en) * | 2014-08-10 | 2015-11-11 | 王选明 | Device for extracting rhododendron pigment |
| CN105440732A (en) * | 2015-11-06 | 2016-03-30 | 大兴安岭林格贝寒带生物科技股份有限公司 | Method for enriching and purifying carmine radish anthocyanin |
| CN112724702A (en) * | 2020-12-29 | 2021-04-30 | 贵州省植物园 | Method for extracting azalea pigment |
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| CN103073912B (en) | 2015-08-26 |
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