CN108218821A - The method extracted from acorn cup, purify anthocyanidin - Google Patents
The method extracted from acorn cup, purify anthocyanidin Download PDFInfo
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- CN108218821A CN108218821A CN201810270845.0A CN201810270845A CN108218821A CN 108218821 A CN108218821 A CN 108218821A CN 201810270845 A CN201810270845 A CN 201810270845A CN 108218821 A CN108218821 A CN 108218821A
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- anthocyanidin
- method described
- resins
- aqueous solution
- extraction
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- 229930014669 anthocyanidin Natural products 0.000 title claims abstract description 63
- 150000001452 anthocyanidin derivatives Chemical class 0.000 title claims abstract description 63
- 235000008758 anthocyanidins Nutrition 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 230000002378 acidificating effect Effects 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims description 84
- 239000011347 resin Substances 0.000 claims description 84
- 238000010828 elution Methods 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002250 absorbent Substances 0.000 claims description 13
- 230000002745 absorbent Effects 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 229920005990 polystyrene resin Polymers 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 2
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 239000000706 filtrate Substances 0.000 description 16
- 238000005406 washing Methods 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 11
- 239000000284 extract Substances 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000001994 activation Methods 0.000 description 8
- 238000005352 clarification Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 239000002674 ointment Substances 0.000 description 8
- 238000002203 pretreatment Methods 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- LRFVTYWOQMYALW-UHFFFAOYSA-N 9H-xanthine Chemical compound O=C1NC(=O)NC2=C1NC=N2 LRFVTYWOQMYALW-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000001058 brown pigment Substances 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 1
- 244000178937 Brassica oleracea var. capitata Species 0.000 description 1
- 235000005976 Citrus sinensis Nutrition 0.000 description 1
- 240000002319 Citrus sinensis Species 0.000 description 1
- 235000009917 Crataegus X brevipes Nutrition 0.000 description 1
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 description 1
- 235000009685 Crataegus X maligna Nutrition 0.000 description 1
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 description 1
- 235000009486 Crataegus bullatus Nutrition 0.000 description 1
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 description 1
- 235000009682 Crataegus limnophila Nutrition 0.000 description 1
- 240000000171 Crataegus monogyna Species 0.000 description 1
- 235000004423 Crataegus monogyna Nutrition 0.000 description 1
- 235000002313 Crataegus paludosa Nutrition 0.000 description 1
- 235000009840 Crataegus x incaedua Nutrition 0.000 description 1
- 235000016623 Fragaria vesca Nutrition 0.000 description 1
- 240000009088 Fragaria x ananassa Species 0.000 description 1
- 235000011363 Fragaria x ananassa Nutrition 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000001549 Ipomoea eriocarpa Species 0.000 description 1
- 235000005146 Ipomoea eriocarpa Nutrition 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 241000218231 Moraceae Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 240000000851 Vaccinium corymbosum Species 0.000 description 1
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 1
- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 235000021014 blueberries Nutrition 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010227 cup method (microbiological evaluation) Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000002864 food coloring agent Nutrition 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019462 natural additive Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
Abstract
The present invention provides a kind of methods extracted from acorn cup, purify anthocyanidin.The method extracted from acorn cup, purify anthocyanidin, includes the following steps：Acorn cup is extracted with acidic aqueous solution, obtains leaching liquor, the temperature of the extraction is 70~80 DEG C, and the pH value of the acidic aqueous solution is 1.3 hereinafter, being purified to the leaching liquor, obtains anthocyanidin.Procyanidine in acorn cup is mainly dissolved out by the present invention using acidic aqueous solution, and procyanidine is changed into anthocyanidin, improve the purity of anthocyanidin by purifying again later, it is final to realize the extraction purpose such as recovery rate height, purity height, production efficiency height, the present invention can reach more than 2% to the recovery rate of anthocyanidin, and anthocyanidin purity after purification is up to more than 90%.
Description
Technical field
The present invention relates to drug and field of health care food, more particularly, to the side that anthocyanidin is extracted, purified from acorn cup
Method.
Background technology
Anthocyanidin is the flavonoid class belonged in phenolic compound, is water colo(u)r.It is widely present in plant petals, fruit
Tissue in.Its color and luster changes with the difference of pH, thus assigns plant different colors.Research shows that anthocyanidin is current
The most effective antioxidant that the mankind have found, with the development of science and technology, people increasingly pay attention to the safety of food additives,
The exploitation of natural additive has become the general trend that Development of Additives uses.Anthocyanidin can not only be used as fortification in food
Agent, and food preservative and food color are alternatively arranged as applied in usual drink and food.
Mainly there is purple sweetpotato, grape, blood orange, red cabbage, blueberry, eggplant, cherry, red in the extraction source of anthocyanidin at present
The plants such as the certain kind of berries, strawberry, mulberries, hawthorn, morning glory, however so numerous plants can not still meet the needs of growing, need
Find new extraction source supply anthocyanidin.
In view of this, it is special to propose the present invention.
Invention content
The purpose of the present invention is to provide it is a kind of from acorn cup extract, purify anthocyanidin method, the method from
It is extracted in acorn cup, the anthocyanidin of purification of high-purity, a new sources is provided for anthocyanidin.
In order to achieve the goal above, the present invention provides following technical schemes：
The method extracted from acorn cup, purify anthocyanidin, includes the following steps：
Acorn cup is extracted with acidic aqueous solution, obtains leaching liquor；The temperature of the extraction is 70~80 DEG C, described
The pH value of acidic aqueous solution is less than 1.3；
The leaching liquor is purified, obtains anthocyanidin.
In the prior art, acorn cup is mainly used to extract acorn nut shell brown pigment, is not used for also directly extracting anthocyanidin.Acorn nut
The complicated component of shell brown pigment, it is considered that the mixture for catechol, xanthin and procyanidine composition.
Anthocyanidin in acorn cup is mainly dissolved out by the present invention using acidic aqueous solution, and procyanidine therein is turned
Become anthocyanidin, improve the purity of anthocyanidin by purifying again later, it is final to realize that recovery rate is high, purity is high, production efficiency is high
Deng extraction purpose.
The present invention can reach more than 2% to the recovery rate of anthocyanidin, and anthocyanidin purity after purification is up to more than 90%.
Acidic aqueous solution in the present invention refers to arbitrary acidic aqueous solution, as long as pH value is less than 1.3, such as pH
1.3rd, pH 1.2, pH 1.1, pH 1.0, pH 0.9, pH 0.8 etc..
The Extracting temperature of the present invention can be 70 DEG C, 72 DEG C, 74 DEG C, 75 DEG C, 76 DEG C, 78 DEG C, 80 DEG C etc..
Above method can also be further improved from the following aspect.
Preferably, the method for the purifying is：
The leaching liquor is adsorbed with macroporous absorbent resin, is then eluted with water to efflux and clarifies, then mixed with alcohol-water
It closes liquid to be eluted, collects eluent.
Macroporous absorbent resin purifies anthocyanidin using principle of polarity, with cost of material is low, operating condition is mild, can expand
The advantages that metaplasia is produced.When adsorbing the leaching liquor with macroporous absorbent resin, it is limited with adsorption saturation, generally when collected outflow
During summation of the liquid for upper prop liquid and resin column volume, adsorption saturation stops upper prop, and for a period of time, the time is staticaccelerator adsorption at this time
1h, 2h, 3h, 4h, depending on comprehensive benefit.
Preferably, the volume ratio of ethyl alcohol is 40%~70%, preferably 60%~70% in the ethanol-water mixture.
During present invention elution anthocyanidin with ethanol-water mixture, due to 40%~70% ethanol-water mixture
Elution speed is fast and anthocyanidin discharge rate is high, therefore, it is suggested that using the ratio, when concrete application can be used 40%, 45%,
50%th, 55%, 60%, 65%, 70% ethanol-water mixture, more than ratio refer both to the volume ratio of ethyl alcohol in solution.Utilize with
The purity for the anthocyanidin that upper solution elutes can reach more than 90%.
Preferably, the macroporous absorbent resin is cross-linked polystyrene resin.
Cross-linked polystyrene resin be low pole resin, the anthocyanidin purity higher of extraction, purity can reach 95% with
On.
Preferably, the aperture of the macroporous absorbent resin is 8~14nm.
Preferably, the macroporous absorbent resin for AB-8 resins, CAD-40 resins, CAD-45 resins, BS-30 resins,
DM130 resins or D860021 resins, preferably DM130 resins.
Preferably, elution speed when being eluted with water is 3~4BV/H.
The elution speed can achieve the purpose that good separating effect and solvent dosage is few.Specific elution speed can be used 3
The arbitrary value in~4BV/H sections, such as 3BV/H, 3.2BV/H, 3.4BV/H, 3.5BV/H, 3.7BV/H or 4BV/H etc..
Preferably, elution speed when being eluted with ethanol-water mixture is 2~3BV/H.
The elution speed can achieve the purpose that anthocyanidin purity is high and solvent dosage is few, and specific elution speed can be used
The arbitrary value in 2~3BV/H sections, such as 2BV/H, 2.2BV/H, 2.4BV/H, 2.5BV/H, 2.7BV/H or 3BV/H etc..
Preferably, the concentration leaching liquor is further included after the extraction and before the purifying：At 60~80 DEG C
It is concentrated into paste.
Moisture is removed by concentration, reduces the workload of purifying, improves production efficiency.
Preferably, the acidic aqueous solution is aqueous hydrochloric acid solution, aqueous citric acid solution or acetic acid aqueous solution.
Preferably, the method for the extraction is decocting method, circumfluence method or ultrasonic extraction, preferably decocting method.
Preferably, the decocting method is multiple to repeat to decoct, and feed liquid mass ratio when decocting every time is 1:20~25.
Preferably, acorn cup is pre-processed before extraction, such as selects, clears up, crushes, is sieved.
To sum up, compared with prior art, invention achieves following technique effects：
(1) a kind of new anthocyanidin extraction source --- acorn cup is provided；
(2) recovery rate is high：The recovery rate of the present invention is up to more than 2%；
(3) anthocyanidin purity is high：Cyanine is improved by the process conditions such as the method and solvent of optimized purification, elution speed
The purity of element, the purity of anthocyanidin is up to more than 90%；
(4) extracting method is simple, suitable for industrialized production.
Specific embodiment
Technical scheme of the present invention is clearly and completely described below in conjunction with specific embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, instead of all the embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiments obtained without making creative work belong to the model that the present invention protects
It encloses.The person that is not specified actual conditions in embodiment, the condition suggested according to normal condition or manufacturer carry out.Agents useful for same or instrument
Production firm person is not specified, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
The method that anthocyanidin is extracted from acorn cup：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions (being adjusted with hydrochloric acid) are added in, it is 1 to adjust pH, and lower processing 3h is carried out at 75 DEG C, repeats 3
It is secondary, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h.
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second.
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 90% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.3%.
Embodiment 2
It is that the concentration of alcohol that macroporous absorbent resin is detached used in elution is different from the main distinction of embodiment 1, specifically such as
Under：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, adjusting pH is 1 (being adjusted with hydrochloric acid), and lower processing 3h is carried out at 75 DEG C, repeats 3
It is secondary, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 40% ethanol-eluting resin column, elution speed controls in 3BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 95% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.25%.
Embodiment 3
It is that the concentration of alcohol that macroporous absorbent resin is detached used in elution is different from the main distinction of embodiment 1, specifically such as
Under：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, adjusting pH is 1 (being adjusted with hydrochloric acid), and lower processing 3h is carried out at 75 DEG C, repeats 3
It is secondary, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 70% ethanol-eluting resin column, elution speed controls in 2.5BV/H, resin column is adsorbed to obtain
Anthocyanidin be eluted out, obtain the acorn cup anthocyanidin of 96% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.31%.
Embodiment 4
It is that macroporous absorbent resin type used is different from the main distinction of embodiment 1, it is specific as follows：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, adjusting pH is 1 (being adjusted with hydrochloric acid), and lower processing 3h is carried out at 75 DEG C, repeats 3
It is secondary, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the AB-8 resins of activation process, upper prop speed is
5BV/H when collected efflux is the summation of upper prop liquid and resin column volume, stops upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 4BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 92% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.11%.
Embodiment 5
PH value when being to extract from the main distinction of embodiment 1 is different, specific as follows：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, adjusting pH is 1.3 (being adjusted with citric acid), and lower processing 3h is carried out at 75 DEG C, weight
It is 3 times multiple, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 94% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.45%.
Embodiment 6
Temperature when being to extract from the main distinction of embodiment 1 is different, specific as follows：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of acidic aqueous solutions are added in, adjusting pH is 1 (being adjusted with hydrochloric acid), and lower processing 3h is carried out at 75 DEG C, weight
It is 3 times multiple, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 90 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 91% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.2%.
Embodiment 7
It is specific as follows from embodiment 1 difference lies in the temperature of concentration is different：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, adjusting pH is 1 (being adjusted with hydrochloric acid), and lower processing 3h is carried out at 75 DEG C, repeats 3
It is secondary, merge the extracting solution of each time, filtering obtains filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 80 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 91% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 2.3%.
Comparative example 1
It is different from the pH value for differing only in acidic aqueous solution of embodiment 1, it is specific as follows：
1st, pre-treatment is extracted：Select without go mouldy, without rotten acorn cup, remove peel, after dries pulverizing, sieve with 100 mesh sieve
Son.
2nd, it extracts：20 times of aqueous solutions are added in, it is 1.5 to adjust pH, and lower processing 3h is carried out at 75 DEG C, is repeated 3 times, and is merged each time
Extracting solution, filtering, obtain filtrate.
3rd, it is concentrated under reduced pressure：Filtrate at 70 DEG C is evaporated under reduced pressure and is concentrated into paste.
4th, macroreticular resin detaches：Ointment addition is had already passed through in the DM-130 resins of activation process, upper prop speed
For 6BV/H, when collected efflux is the summation of upper prop liquid and resin column volume, stop upper prop, staticaccelerator adsorption 3h；
5th, washed with impurities：With pure water rinsing resin column, elution speed 3BV/H, when efflux becomes clarification from muddiness,
Stop washing, washing can remove water-soluble substances of the absorption in the resin table second；
6th, alcohol is washed：With 60% ethanol-eluting resin column, elution speed controls in 2BV/H, resin column is adsorbed
Anthocyanidin is eluted out, and obtains the acorn cup anthocyanidin of 88% purity.
Through weighing, calculating, the recovery rate of anthocyanidin is 1.4%.
By the result of above-described embodiment and comparative example it is found that pH value when extracting has important shadow to the recovery rate of anthocyanidin
It rings, if condition is not suitable for, even if there is minute differences, recovery rate also differs greatly.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe is described in detail the present invention with reference to foregoing embodiments, it will be understood by those of ordinary skill in the art that：Its according to
Can so modify to the technical solution recorded in foregoing embodiments either to which part or all technical features into
Row equivalent replacement；And these modifications or replacement, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. the method extracted from acorn cup, purify anthocyanidin, which is characterized in that include the following steps：
Acorn cup is extracted with acidic aqueous solution, obtains leaching liquor；The temperature of the extraction is 70-80 DEG C, the acidity
The pH value of aqueous solution is less than 1.3；
The leaching liquor is purified, obtains anthocyanidin.
2. according to the method described in claim 1, it is characterized in that, the method for the purifying is：
The leaching liquor is adsorbed with macroporous absorbent resin, is then eluted with water to efflux and clarifies, then use ethanol-water mixture
It is eluted, collects eluent.
3. according to the method described in claim 2, it is characterized in that, the volume ratio of ethyl alcohol is in the ethanol-water mixture
40%~70%, preferably 60%~70%.
4. according to the method described in claim 2, it is characterized in that, the macroporous absorbent resin is cross-linked polystyrene resin；
Preferably, the aperture of the macroporous absorbent resin is 8~14nm；
Preferably, the macroporous absorbent resin is AB-8 resins, CAD-40 resins, CAD-45 resins, BS-30 resins, DM130 trees
Fat or D860021 resins, preferably DM130 resins.
5. according to the method described in claim 2, it is characterized in that, elution speed when being eluted with water is 3~4BV/H.
6. according to the method described in claim 2, it is characterized in that, elution when being eluted with ethanol-water mixture
Speed is 2~3BV/H.
7. it according to the method described in claim 1, it is characterized in that, is further included after the extraction and before the purifying dense
Contract the leaching liquor：Paste is concentrated at 60~80 DEG C.
8. according to the method described in claim 1, it is characterized in that, the acidic aqueous solution is aqueous hydrochloric acid solution, citric acid water
Solution or acetic acid aqueous solution.
9. according to the method described in claim 1, it is characterized in that, the method for the extraction is decocting method, circumfluence method or ultrasound
Wave extraction method, preferably decocting method.
10. according to the method described in claim 9, it is characterized in that, the decocting method is multiple to repeat to decoct, when decocting every time
Feed liquid mass ratio be 1:20~25.
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