CN103073912B - A kind of Folium Cuculus polioephalus prepares the method for purifying azalea - Google Patents
A kind of Folium Cuculus polioephalus prepares the method for purifying azalea Download PDFInfo
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- CN103073912B CN103073912B CN201210595343.8A CN201210595343A CN103073912B CN 103073912 B CN103073912 B CN 103073912B CN 201210595343 A CN201210595343 A CN 201210595343A CN 103073912 B CN103073912 B CN 103073912B
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Abstract
The present invention discloses a kind of method that Folium Cuculus polioephalus prepares purifying azalea, and the method is: rhododendron is ground into meal, and the methanol eddy adding 15 times amount 85% extracts 120 minutes, filters; Filtrate, reclaims methyl alcohol, is concentrated into 3 Baumes, the hydrochloric acid by volume ratio 1: 1: concentrated solution pH value is adjusted to 2.5 by water, places 20 minutes, filters; Broad spectrum type macroporous resin adsorption post on filtrate, collects elutriant, and reclaim methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with the acetone of volume ratio 3: 1: methanol wash column impurity, continue with the acetone of volume ratio 7: 1: methanol-eluted fractions, collect elutriant; Carried out refining to obtain azalea finished product by collected azalea elutriant, its content is more than 70%.The maximum feature of the inventive method utilizes that the coupling of macroporous adsorbent resin-silica gel column chromatography is convenient and swift, abundant raw material source, low production cost, separating effect are obvious, DNA purity is high.
Description
Technical field:
The invention belongs to field of natural organic chemistry, relate to a kind of method that Folium Cuculus polioephalus prepares azalea, particularly relate to a kind of macroporous adsorbent resin co-solvent that utilizes and extract the method preparing purifying azalea.
Background technology:
Folium Cuculus polioephalus Rhododendron dauricum, call Rhododendron dauricum, reach that son is fragrant, Da Daxiang, the high 1 ~ 2m of half evergreen shrubs, multi-branched.Leaf alternate, nearly keratin, oval oval to ovum shape, long 1.5 ~ 3.5cm, Quan Yuan.Spend 1 ~ 4 raw branch top.Corolla funnel-form, red-violet colour, diameter 2.5 ~ 3.5cm.Leaf containing perfume oil and tonka bean camphor etc., availablely carries perfume oil, modulation essence; Also be used as medicine, bitter cold in nature.There is cough-relieving apophlegmatic function, treating acute and chronic bronchitis.Stem, bar, fruit, containing careless tannin, can obtain through refining tannin extract.
The tree peony anthocyanins that azalea is a kind of extraction purification from natural phant and obtains is natural pigment, natural in color, and tint permanence is good, is mainly used as the tinting material of beverage, candy, jam and cake etc.In recent years, it is found that containing a large amount of azalea pigments in natural phant cuckoo, therefrom extract azalea pigment and achieve encouraging progress, 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 is also to provide a kind of convenient and swift, abundant raw material source, low production cost, separating effect are obvious, DNA purity is high method 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 purifying azalea comprises the steps:
Rhododendron is ground into meal, and 85% ~ 100% methanol eddy adding meal quality 15 ~ 20 times amount extracts 120 ~ 180 minutes, filters; Filtrate is concentrated into 3 ~ 5 Baumes after reclaiming methyl alcohol and obtains concentrated solution, then uses the hydrochloric acid of volume ratio 1: 1: concentrated solution pH value is adjusted to 2.5 ~ 3 by the aqueous solution, places after 20 ~ 40 minutes and filters; HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, use the methanol wash column impurity of 5% ~ 20% again, then the methanol-eluted fractions of 50% ~ 80% is used, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1 ~ 3: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 5 ~ 7: 1, obtains azalea elutriant; Carried out refining to obtain azalea by azalea elutriant, its content is more than 70%.
The method that Folium Cuculus polioephalus of the present invention prepares purifying azalea comprises the steps:
Take the rhododendron being ground into meal, 85% methanol eddy adding meal quality 20 times amount extracts 180 minutes, filters; Filtrate is concentrated into 5 Baumes after reclaiming methyl alcohol and obtains concentrated solution, then uses the hydrochloric acid of volume ratio 1: 1: concentrated solution pH value is adjusted to 3 by the aqueous solution, places after 40 minutes and filters; HPD400 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 5%, then use the methanol-eluted fractions of 50%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 5: 1, obtains azalea elutriant; Azalea elutriant is carried out refining to obtain azalea.
Described macroporous resin adsorption step adopts wet method dress post, retains liquid level, by the filtrate after adjust pH by adsorption column, and flow velocity per minute 0.05ml/g resin.
Described silica gel column chromatography step adopts wet method dress post, retains liquid level, and work in-process are mixed activation after silica gel by weight at 1: 1, and by the mixture mixed as above silicagel column, elution flow rate per minute 0.1ml/g silica gel.Silica gel activating condition is, 110 degrees Celsius 30 minutes.
Adopt activated carbon decolorizing in the present invention, recrystallization method refines.Add injection active carbon by 4g/100ml elutriant, 25 ~ 40 degrees Celsius are stirred 20 ~ 40 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate; Intermediate 7 ~ 9 times of methyl alcohol, 40 degrees Celsius of thermosols, filter: filtrate cools crystallize out, and suction filtration obtains azalea finished product.
In the present invention, treating process comprises the steps:
Add injection active carbon by 4g/100ml elutriant, 25 degrees Celsius are stirred 40 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate; Intermediate 9 times of methyl alcohol, 40 degrees Celsius of thermosols, filter; Filtrate cools crystallize out, and suction filtration obtains azalea finished product.
Finished product 7 times of recrystallizing methanol in treating process in the present invention, filtrated stock, reclaim methyl alcohol, concentrate drying obtains azalea work in-process.
The present invention's application macroporous adsorbent resin-silica gel column chromatography coupled method enriching and purifying azalea, good to the adsorption selectivity of azalea, absorption is fast resolves also soon, and loading capacity is larger; Abundant raw material source, low production cost, separating effect is obvious, and DNA purity is high, can obtain the azalea work in-process of content more than 45% and the azalea finished product of content more than 70%, overcome the shortcoming that traditional extraction rate is relatively low, DNA purity is low.
The present invention selects that stable in physicochemical property, surface-area are comparatively 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 organism selectivity, not by the impact that inorganic salts and strong ion low molecular compound exist, from solution, azalea can be adsorbed selectively by physical adsorption, absorption is fast, parsing is also fast, and loading capacity is larger.
The present invention selects silica gel chromatography purifying and binding activities charcoal and recrystallizing and refining, and separating effect is better.
Embodiment:
Embodiment 1:
Take rhododendron 10kg, be ground into meal, the methanol eddy adding 18 times amount 90% extracts 140 minutes, filters; Filtrate, reclaims methyl alcohol, is concentrated into 4 Baumes, the hydrochloric acid by volume ratio 1: 1: concentrated solution pH value is adjusted to 2.8 by the aqueous solution, places 40 minutes, filters; HPD100 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 15%, then use the methanol-eluted fractions of 70%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 2: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 6: 1, obtains azalea elutriant 2L; Add 80g injection active carbon, 30 degrees Celsius are stirred 30 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate 35g; Intermediate 8 times of methyl alcohol, 40 degrees Celsius of thermosols, filter, filtrate cools crystallize out, and suction filtration obtains azalea finished product 20g, content 73%.
Embodiment 2:
Take rhododendron 15kg, be ground into meal, the methanol eddy adding 20 times amount 95% extracts 160 minutes, filters; Filtrate, reclaims methyl alcohol, is concentrated into 5 Baumes, the hydrochloric acid by volume ratio 1: 1: concentrated solution pH value is adjusted to 3 by the aqueous solution, places 40 minutes, filters; HPD400 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 10%, then use the methanol-eluted fractions of 60%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 7: 1, obtains azalea elutriant 3.5L; Add 140g injection active carbon, 40 degrees Celsius are stirred 40 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate 60g; Intermediate 9 times of methyl alcohol, 40 degrees Celsius of thermosols, filter, filtrate cools crystallize out, and suction filtration obtains azalea finished product 32g, content 71.3%.
Embodiment 3:
Take rhododendron 20kg, be ground into meal, the methanol eddy adding 15 times amount 87% extracts 120 minutes, filters; Filtrate, reclaims methyl alcohol, is concentrated into 3 Baumes, the hydrochloric acid by volume ratio 1: 1: concentrated solution pH value is adjusted to 2.5 by the aqueous solution, places 40 minutes, filters; AB-8 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 5%, then use the methanol-eluted fractions of 80%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 3: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 5: 1, obtains azalea elutriant 5L; Add 200g injection active carbon, 25 degrees Celsius are stirred 20 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate 70g; Intermediate 8 times of methyl alcohol, 40 degrees Celsius of thermosols, filter, filtrate cools crystallize out, and suction filtration obtains azalea finished product 36g, content 72.5%.
Embodiment 4:
Take rhododendron 5kg, be ground into meal, the methanol eddy adding 20 times amount 98% extracts 160 minutes, filters; Filtrate, reclaims methyl alcohol, is concentrated into 3 Baumes, the hydrochloric acid by volume ratio 1: 1: concentrated solution pH value is adjusted to 2.6 by the aqueous solution, places 40 minutes, filters; DM-130 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 5%, then use the methanol-eluted fractions of 50%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 7: 1, obtains azalea elutriant 1200ml; Add 48g injection active carbon, 40 degrees Celsius are stirred 25 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate 20g; Intermediate 7 times of methyl alcohol, 40 degrees Celsius of thermosols, filter, filtrate cools crystallize out, and suction filtration obtains azalea finished product 12g, content 73.2%.
Claims (7)
1. Folium Cuculus polioephalus prepares a method for purifying azalea, it is characterized in that the method comprises the steps:
Rhododendron is ground into meal, and 85% ~ 100% methanol eddy adding meal quality 15 ~ 20 times amount extracts 120 ~ 180 minutes, filters; Filtrate is concentrated into 3 ~ 5 degree Beaume concentrated solutions after reclaiming methyl alcohol, then uses the hydrochloric acid of volume ratio 1: 1: concentrated solution pH value is adjusted to 2.5 ~ 3 by the aqueous solution, places after 20 ~ 40 minutes and filters; HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, use the methanol wash column impurity of 5% ~ 20% again, then the methanol-eluted fractions of 50% ~ 80% is used, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1 ~ 3: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 5 ~ 7: 1, obtains azalea elutriant; Azalea elutriant is carried out refining to obtain 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 the rhododendron being ground into meal, 85% methanol eddy adding meal quality 20 times amount extracts 180 minutes, filters; Filtrate is concentrated into 5 degree Beaume concentrated solutions after reclaiming methyl alcohol, then uses the hydrochloric acid of volume ratio 1: 1: concentrated solution pH value is adjusted to 3 by the aqueous solution, places after 40 minutes and filters; HPD400 type macroporous resin adsorption post on filtrate, adsorb and completely wash impurity with water, then use the methanol wash column impurity of 5%, then use the methanol-eluted fractions of 50%, obtain azalea work in-process elutriant, after azalea work in-process elutriant reclaims methyl alcohol, concentrate drying obtains azalea work in-process; By silica gel column chromatography on gained azalea work in-process, and with acetone: the volume ratio of methyl alcohol be 1: 1 acetone and carbinol mixture wash impurity, then use acetone: the volume ratio of methyl alcohol is acetone and the carbinol mixture wash-out of 5: 1, obtains azalea elutriant; Azalea elutriant is carried out refining to obtain 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, retain liquid level, by the filtrate after adjust pH by 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, retain liquid level, work in-process are mixed activation rear silica gel by weight at 1: 1, and the mixture mixed is placed in above silicagel column, elution flow rate per minute 0.1ml/g silica gel, silica gel activating condition is, 110 degrees Celsius 30 minutes.
5. Folium Cuculus polioephalus as claimed in claim 1 or 2 prepares the method for purifying azalea, it is characterized in that in the method, adopting activated carbon decolorizing, recrystallization method refines, add injection active carbon by 4g/100ml azalea elutriant, 25 ~ 40 degrees Celsius are stirred 20 ~ 40 minutes, filter; After filtrate reclaims mix reagent, concentrate drying obtains intermediate; Intermediate 7 ~ 9 times of methyl alcohol, 40 degrees Celsius of thermosols, filter; Filtrate cools crystallize out, and suction filtration obtains azalea finished product.
6. Folium Cuculus polioephalus as claimed in claim 5 prepares the method for purifying azalea, it is characterized in that in the method, treating process comprises the steps:
Add injection active carbon by 4g/100ml elutriant, 25 degrees Celsius are stirred 40 minutes, filter; Filtrate, reclaim mix reagent, concentrate drying obtains intermediate; Intermediate 9 times of methyl alcohol, 40 degrees Celsius of thermosols, filter; Filtrate cools crystallize out, and suction filtration obtains azalea finished product.
7. Folium Cuculus polioephalus as claimed in claim 6 prepares the method for purifying azalea, it is characterized in that finished product 7 times of recrystallizing methanol in the method, filtrated stock, and reclaim methyl alcohol, concentrate drying obtains azalea finished product.
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| CN105885470B (en) * | 2014-08-10 | 2017-11-24 | 嵊州北航投星空众创科技有限公司 | A kind of equipment that can be used in extracting azalea pigment |
| CN105440732B (en) * | 2015-11-06 | 2017-08-29 | 大兴安岭林格贝寒带生物科技股份有限公司 | The method of enriching and purifying rouge radish anthocyanidin |
| CN112724702A (en) * | 2020-12-29 | 2021-04-30 | 贵州省植物园 | Method for extracting azalea pigment |
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| CN102433018A (en) * | 2011-11-17 | 2012-05-02 | 安徽杜鹃花生物科技有限公司 | Method for extracting azalea pigment |
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| CN1037263A (en) * | 1988-05-04 | 1989-11-22 | 浙江省科学院柑桔研究所 | From azalea, produce edible natural pigment-azalea |
| CN102532219A (en) * | 2010-12-20 | 2012-07-04 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying anthocyanin in lonicera caerulea |
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