CN108147955A - A kind of method that curcumin is extracted from ginger - Google Patents
A kind of method that curcumin is extracted from ginger Download PDFInfo
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- CN108147955A CN108147955A CN201810154117.3A CN201810154117A CN108147955A CN 108147955 A CN108147955 A CN 108147955A CN 201810154117 A CN201810154117 A CN 201810154117A CN 108147955 A CN108147955 A CN 108147955A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
Abstract
The present invention relates to a kind of methods that curcumin is extracted from ginger, ginger raw material is not required to dry directly use, broken wall, complex enzyme zymohydrolysis, ultrasonic wave added sodium salicylate ethanol solution extraction method are carried out using flash extracter in extraction process, the technology that broken wall and complex enzyme zymohydrolysis combination are carried out using flash extracter substantially increases extraction efficiency;By crystallization, most impurity can be stayed in mother liquor in solution, then by filtering, and washing can obtain the higher crystal of purity, and with HPLC detection purity up to more than 90% after crystallization, purity is detected up to more than 97% with HPLC after recrystallization.
Description
Technical field
The present invention relates to a kind of extraction process, more particularly to a kind of method that curcumin is extracted from ginger.
Background technology
Turmeric be zingiberaceous plant turmeric (Curcumalonga L.) dry rhizome, have promoting qi circulation and relieving pain, promoting menstruation blood-breaking,
Numbness and other effects is treated in wind-dispelling.In recent years domestic and international pharmaceutical research finds that there is curcuma prevention and treatment cancer and cranial nerve to protect
A variety of effects such as shield, thus be concerned.
Curcumin is commonly referred to as curcumin, is mainly derived from the rhizome of Zingiber curcuma turmeric.Numerous studies are demonstrate,proved
Bright, there is curcumin anti-oxidant, anti-inflammatory, anticancer, removing free radical, antimicrobial and protection cardio-cerebrovascular, adjusting to disappear
Change many-sided pharmacological action such as system function.Turmeric is alternatively arranged as flavouring, natural pigment, natural dye, due to safe and non-toxic,
It is without side-effects, thus WHO and FDA approval curcumins are natural additive for foodstuff.
The extraction process report of curcumin is more, such as organic solvent extraction, extraction, SCF-CO 2
Method, sodium salicylate method etc., wherein organic solvent extraction with simple for process, easy to operate, reaction condition due to being relatively easy to control
The advantages that be a kind of current the most widely used extracting method.But organic solvent extraction accelerates to increase extraction efficiency
The dissolution of curcumin, it usually needs Extracting temperature is improved, so as to which the activity of curcumin, obtained ginger can be destroyed to a certain extent
Flavine medicinal extract is not easy drying, and the purity of curcumin can also be affected.
Application number 201310141337.X discloses a kind of technique of carbon dioxide supercritical extraction method extraction curcumin,
Extractant is done using supercritical carbon dioxide fluid, 95% ethyl alcohol is entrainer, and curcumin is extracted from ginger.The invention uses
Means of supercritical extraction, equipment requirement is high, of high cost, is not suitable for industrialized production.For example organic solvent carries disclosed in CN102603505
It follows the example of, supercritical CO_2 extraction method disclosed in CN103254050, enzyme process disclosed in CN105061168 pre-processes assisted extraction turmeric
The technique of element;Buck extracting method etc. disclosed in CN103570517;Common problem is organic molten in method made above
The constituent impurity content of agent extraction method extraction is more;Enzyme process is more demanding to environment and pH value can not large-scale application;Buck
Extraction reaction is violent, can be to destroying curcumin;And also there is the problems such as not easy purification for curcumin prepared by above method.Cause
This, seeks a kind of at low cost, and operability is strong, and the method for extraction curcumin with short production cycle is critically important.
Invention content
The purpose of the present invention is to provide a kind of methods that curcumin is extracted from ginger, and curcumin is extracted from ginger,
Extraction and the technology that is combined of enzymolysis are crushed using plant, has easy to operate, raw material is easy to get, at low cost, pollutes few reagent and returns
Receive the advantages that utilization rate is high.
In order to solve the above technical problem, the present invention provides it is a kind of from ginger extract curcumin method, step
It is as follows:
1)By ginger chopping, dilute alkaline soln leaching pretreatment is added in;Then broken wall treatment is carried out using flash extracter, obtains broken wall
Slurries.
2)The cellulase of shell-broken liquid weight 0.3%, the amylase and 1.0% of 0.1% turmeric are added in the broken wall slurries
Turmeric papain composition complex enzyme, in acid condition digest 2-3 hours after, high temperature destroy the enzyme treatment is digested
Liquid.
3)Enzymolysis liquid is added in into sodium salicylate alcoholic solution, homogenate, ultrasonic extraction obtains curcumin extracting solution twice.
4)Concentrated extracting solution to paste, upper macroreticular resin is eluted with acetone-glacial acetic acid, is collected eluent removing solvent and is obtained
Curcumin crude product;
5)Curcumin crude product is crystallized using alcohol-water method, obtains orange-yellow acicular crystal, by the orange-yellow acicular crystal
Freeze-drying obtains curcumin primary crystallization object;
6)Recrystallization, recrystallizes curcumin primary crystallization object using alcohol-water method, obtains orange red acicular crystal, will
The orange red acicular crystal is freeze-dried to obtain purifying curcumin.
Preferably, the step 1)Middle dilute alkaline soln for alkali metal hydride or carbonate aqueous solution, it is furthermore preferred that
The dilute alkaline soln is NaOH solution.
Preferably, the step 1)Middle homogenate extraction voltage be 220V, 1~3 minute extraction time.
Preferably, the step 2)Middle acid condition is that pH value is 3-4.
Preferably, the step 3)The concrete operations of middle homogenate are homogenized 3~10min under the conditions of being 3000~6000r/min.
Preferably, the step 4)Middle macroreticular resin is Diaion HP-10 types, SPD100, D-101 type or AB-
8 types.
Preferably, the step 6)Concrete operations are as follows:It is 1 by mass volume ratio:50~80 by curcumin primary crystallization
Object is dissolved in ethyl alcohol, and heating stirring makes curcumin primary crystallization powder fully dissolve, obtains peony clear transparent solutions;Then to institute
It obtains in solution and is slowly added to hot distilled water, until occurring muddy;The ethyl alcohol of 10~25% hot water volumes, solution are added in into solution again
Become peony clear transparent solutions again;By acquired solution under the conditions of 0~4 DEG C crystallisation by cooling, obtain orange red needle-shaped knot
It is brilliant.
Advantages of the present invention is as follows:
(1) technology being combined using flash extracter broken wall treatment with compound enzymatic treatment effectively destroys the cell of cell
Wall increases the mass transfer area that curcumin during subsequent extracted is spread to ethyl alcohol, significantly improves the recovery rate of curcumin;
(2) addition of amylase and papain can will influence the decomposition such as starch, protein that curcumin refines and remove, and carry
The clarity of high extraction system, and papain can increase intercellular dispersion degree, conducive to the progress of subsequent extracted technique
;
(3) homogenized is carried out after the turmeric after enzymolysis processing mixes with ethyl alcohol, it is ensured that turmeric cell and ethanol solution
It is sufficiently mixed, and under the action of high shear is homogenized, cell generation further crushes, and promotes effective ingredient curcumin
Extraction.
(4) sodium salicylate is added in when ethyl alcohol is used to extract as extraction accelerating agent, improves the extraction effect of curcumin
Rate.
(5) by crystallizing, most impurity can be stayed in mother liquor in solution, then by filtering, and washing can obtain
The higher crystal of purity, can with HPLC detection purity after recrystallization with HPLC detection purity up to more than 90% after crystallization
Up to more than 97%.
Specific embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiments obtained under the premise of creative work is not made belong to the model that the present invention protects
It encloses.
【Embodiment 1】
1)1kg ginger choppings are taken, add in 15 times of amount NaOH solution leaching pretreatments;Using flash extracter in the case where voltage is 220V
It carries out broken wall treatment 3 minutes, obtains broken wall slurries.
2)The cellulase of shell-broken liquid weight 0.3%, the amylase and 1.0% of 0.1% turmeric are added in the broken wall slurries
Turmeric papain composition complex enzyme and adjust pH as 3, for enzymolysis after 3 hours, high temperature destroy the enzyme treatment obtains enzymolysis liquid.
3)Enzymolysis liquid is added in into sodium salicylate alcoholic solution, 6min is homogenized under the conditions of 6000r/min, then ultrasonic extraction
Curcumin extracting solution is obtained twice.
4)Concentrated extracting solution to paste, upper Diaion HP-10 macroreticular resins is 30% acetone-ice vinegar with percentage by volume
Pickling takes off, and collects eluent removing solvent and obtains curcumin crude product;
5)Curcumin crude product is crystallized using mixed solvent second alcohol and water, obtains orange-yellow acicular crystal, this is orange-yellow
Acicular crystal is freeze-dried to obtain curcumin primary crystallization object, and purity is detected up to 90% with HPLC;
6)Recrystallization is 1 by mass volume ratio:Curcumin primary crystallization object is dissolved in ethyl alcohol by 50~80, and heating stirring makes turmeric
Plain primary crystallization powder fully dissolves, and obtains peony clear transparent solutions;Then hot distilled water is slowly added into acquired solution,
It is muddy to occurring;The ethyl alcohol of 25% hot water volume is added in into solution again, solution becomes peony clear transparent solutions again;It will
Acquired solution crystallisation by cooling under the conditions of 0~4 DEG C obtains the orange red acicular crystals of 180g, reachable with HPLC detections purity
More than 97%.
【Embodiment 2】
1)1kg ginger choppings are taken, add in 10 times of amount NaOH solution leaching pretreatments;Using flash extracter in the case where voltage is 220V
It carries out broken wall treatment 3 minutes, obtains broken wall slurries.
2)The cellulase of shell-broken liquid weight 0.3%, the amylase and 1.0% of 0.1% turmeric are added in the broken wall slurries
Turmeric papain composition complex enzyme and adjust pH as 3, for enzymolysis after 3 hours, high temperature destroy the enzyme treatment obtains enzymolysis liquid.
3)Enzymolysis liquid is added in into sodium salicylate alcoholic solution, 6min is homogenized under the conditions of 3000r/min, then ultrasonic extraction
Curcumin extracting solution is obtained twice.
4)Concentrated extracting solution to paste, upper Diaion HP-10 macroreticular resins is 30% acetone-ice vinegar with percentage by volume
Pickling takes off, and collects eluent removing solvent and obtains curcumin crude product;
5)Curcumin crude product is crystallized using mixed solvent second alcohol and water, obtains orange-yellow acicular crystal, this is orange-yellow
Acicular crystal is freeze-dried to obtain curcumin primary crystallization object, and purity is detected up to 90% with HPLC;
6)Recrystallization is 1 by mass volume ratio:Curcumin primary crystallization object is dissolved in ethyl alcohol by 50~80, and heating stirring makes turmeric
Plain primary crystallization powder fully dissolves, and obtains peony clear transparent solutions;Then hot distilled water is slowly added into acquired solution,
It is muddy to occurring;The ethyl alcohol of 25% hot water volume is added in into solution again, solution becomes peony clear transparent solutions again;It will
Acquired solution crystallisation by cooling under the conditions of 0~4 DEG C obtains the orange red acicular crystals of 176g, reachable with HPLC detections purity
More than 97%.
【Comparative example 1】
1)1kg ginger choppings are taken, add in 10 times of amount NaOH solution leaching pretreatments;Then add in weight 0.3% cellulase,
The complex enzyme of the amylase of 0.1% turmeric and the papain of 1.0% turmeric composition simultaneously adjusts pH as 3, and enzymolysis is after 3 hours,
High temperature destroy the enzyme treatment obtains enzymolysis liquid.
2)Enzymolysis liquid is added in into sodium salicylate alcoholic solution, 6min is homogenized under the conditions of 3000r/min, then ultrasonic extraction
Curcumin extracting solution is obtained twice.
3)Concentrated extracting solution to paste, upper Diaion HP-10 macroreticular resins is 30% acetone-ice vinegar with percentage by volume
Pickling takes off, and collects eluent removing solvent and obtains curcumin crude product;
4)Curcumin crude product is crystallized using mixed solvent second alcohol and water, obtains orange-yellow acicular crystal, this is orange-yellow
Acicular crystal is freeze-dried to obtain curcumin primary crystallization object, and purity is detected up to 90% with HPLC;
5)Recrystallization is 1 by mass volume ratio:Curcumin primary crystallization object is dissolved in ethyl alcohol by 50~80, and heating stirring makes turmeric
Plain primary crystallization powder fully dissolves, and obtains peony clear transparent solutions;Then hot distilled water is slowly added into acquired solution,
It is muddy to occurring;The ethyl alcohol of 25% hot water volume is added in into solution again, solution becomes peony clear transparent solutions again;It will
Acquired solution crystallisation by cooling under the conditions of 0~4 DEG C obtains the orange red acicular crystals of 135g, reachable with HPLC detections purity
More than 97%.
【Comparative example 2】
1)1kg ginger choppings are taken, add in 10 times of amount NaOH solution leaching pretreatments;Using flash extracter in the case where voltage is 220V
It carries out broken wall treatment 3 minutes, obtains broken wall slurries.
2)Broken wall slurries are added in into sodium salicylate alcoholic solution, 6min are homogenized under the conditions of 3000r/min, then ultrasound carries
It takes and obtains curcumin extracting solution twice.
3)Concentrated extracting solution to paste, upper Diaion HP-10 macroreticular resins is 30% acetone-ice vinegar with percentage by volume
Pickling takes off, and collects eluent removing solvent and obtains curcumin crude product;
4)Curcumin crude product is crystallized using mixed solvent second alcohol and water, obtains orange-yellow acicular crystal, this is orange-yellow
Acicular crystal is freeze-dried to obtain curcumin primary crystallization object, and purity is detected up to 90% with HPLC;
5)Recrystallization is 1 by mass volume ratio:Curcumin primary crystallization object is dissolved in ethyl alcohol by 50~80, and heating stirring makes turmeric
Plain primary crystallization powder fully dissolves, and obtains peony clear transparent solutions;Then hot distilled water is slowly added into acquired solution,
It is muddy to occurring;The ethyl alcohol of 25% hot water volume is added in into solution again, solution becomes peony clear transparent solutions again;It will
Acquired solution crystallisation by cooling under the conditions of 0~4 DEG C obtains the orange red acicular crystals of 123g, reachable with HPLC detections purity
More than 97%.
Beneficial effects of the present invention are as follows:
(1) technology being combined using flash extracter broken wall treatment with compound enzymatic treatment effectively destroys the cell of cell
Wall increases the mass transfer area that curcumin during subsequent extracted is spread to ethyl alcohol, significantly improves the recovery rate of curcumin;
(2) addition of amylase and papain can will influence the decomposition such as starch, protein that curcumin refines and remove, and carry
The clarity of high extraction system, and papain can increase intercellular dispersion degree, conducive to the progress of subsequent extracted technique
;
(3) homogenized is carried out after the turmeric after enzymolysis processing mixes with ethyl alcohol, it is ensured that turmeric cell and ethanol solution
It is sufficiently mixed, and under the action of high shear is homogenized, cell generation further crushes, and promotes effective ingredient curcumin
Extraction.
(4) sodium salicylate is added in when ethyl alcohol is used to extract as extraction accelerating agent, improves the extraction effect of curcumin
Rate.
(5) by crystallizing, most impurity can be stayed in mother liquor in solution, then by filtering, and washing can obtain
The higher crystal of purity, can with HPLC detection purity after recrystallization with HPLC detection purity up to more than 90% after crystallization
Up to more than 97%.
Above description has fully disclosed the specific embodiment of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change that the specific embodiment of the present invention is done all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (8)
1. a kind of method that curcumin is extracted from ginger, its step are as follows:
1)By ginger chopping, dilute alkaline soln leaching pretreatment is added in;Then broken wall treatment is carried out using flash extracter, obtains broken wall
Slurries;
2)The cellulase of shell-broken liquid weight 0.3%, the amylase of 0.1% turmeric and 1.0% ginger are added in the broken wall slurries
The complex enzyme of yellow papain composition, after digesting 2-3 hours in acid condition, high temperature destroy the enzyme treatment obtains enzymolysis liquid;
3)The enzymolysis liquid is added in into sodium salicylate alcoholic solution, homogenate, ultrasonic extraction obtains curcumin extracting solution twice;
4)The extracting solution is concentrated to paste, upper macroreticular resin is eluted with acetone-glacial acetic acid, is collected eluent removing solvent and is obtained
Curcumin crude product;
5)The curcumin crude product is crystallized using alcohol-water method, obtains orange-yellow acicular crystal, this is orange-yellow needle-shaped
Crystallization freezing is dried to obtain curcumin primary crystallization object;
6)Recrystallization, recrystallizes curcumin primary crystallization object using alcohol-water method, obtains orange red acicular crystal, will
The orange red acicular crystal is freeze-dried to obtain purifying curcumin.
2. the method according to claim 1 that curcumin is extracted from ginger, the step 1)In dilute alkaline soln be alkali
The hydride of metal or the aqueous solution of carbonate.
3. the method according to claim 2 that curcumin is extracted from ginger, the dilute alkaline soln is NaOH solution.
4. the method according to claim 1 that curcumin is extracted from ginger, homogenate extraction voltage is 220V, during extraction
Between 1~3 minute.
5. the method according to claim 1 that curcumin is extracted from ginger, the step 2)Middle acid condition is pH value
For 3-4.
6. the method according to claim 1 that curcumin is extracted from ginger, the step 3)The concrete operations of middle homogenate
To be homogenized 3~10min under the conditions of 3000~6000r/min.
7. the method according to claim 1 that curcumin is extracted from ginger, the step 4)Middle macroreticular resin is
Diaion HP-10 types, SPD100, D-101 type or AB-8 types.
8. the method according to claim 1 that curcumin is extracted from ginger, the step 6)Concrete operations are:By quality
Volume ratio is 1:Curcumin primary crystallization object is dissolved in ethyl alcohol by 50~80, and heating stirring makes curcumin primary crystallization powder fully molten
Solution, obtains peony clear transparent solutions;Then hot distilled water is slowly added into acquired solution, until occurring muddy;Again to solution
The middle ethyl alcohol for adding in 10~25% hot water volumes, solution become peony clear transparent solutions again;By acquired solution 0~4
Crystallisation by cooling under the conditions of DEG C obtains orange red acicular crystal.
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Cited By (4)
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CN111995509A (en) * | 2020-07-31 | 2020-11-27 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
CN112772776A (en) * | 2021-01-08 | 2021-05-11 | 江西嘉博生物工程有限公司 | Preparation method and application of turmeric extract |
CN114031489A (en) * | 2021-11-08 | 2022-02-11 | 福建省农业科学院农业质量标准与检测技术研究所 | Ionic liquid BMIM]PF6Method for extracting curcumin by synergistic enzyme |
CN115448992A (en) * | 2022-10-10 | 2022-12-09 | 江西省科学院应用化学研究所 | Extraction method and application of camellia oleifera shell polysaccharide |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111995509A (en) * | 2020-07-31 | 2020-11-27 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
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CN114031489A (en) * | 2021-11-08 | 2022-02-11 | 福建省农业科学院农业质量标准与检测技术研究所 | Ionic liquid BMIM]PF6Method for extracting curcumin by synergistic enzyme |
CN115448992A (en) * | 2022-10-10 | 2022-12-09 | 江西省科学院应用化学研究所 | Extraction method and application of camellia oleifera shell polysaccharide |
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Application publication date: 20180612 |