CN109705127A - A kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin - Google Patents
A kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin Download PDFInfo
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Abstract
The invention discloses a kind of emulsion resistance preparation methods of plant source sodium copper chlorophyllin, using ginkgo leaf as raw material, alcohol extracting obtains black medicinal extract, positive, back extraction is carried out using the alcohol solvent and petroleum ether solvent of difference concentration, the phenomenon that substantially reducing emulsification layering, ginkgo acid content is less than 1ppm, absorbance >=600 E405nm in the chlorophyll cupric acid sodium of acquisition.
Description
Technical field
The present invention relates to plant extracts and chemical field, relate in particular to a kind of anti-cream of plant source sodium copper chlorophyllin
Change preparation method.
Background technique
Sodium copper chlorophyllin is a kind of natural pigment product, including animal origin (such as silkworm excrement) and plant origin
(such as leaf of clover, bamboo, ginkgo plant) converts chlorophyllin salt, then acid for chlorophyll by saponification when production
Change copper for chlorophyll cupric acid is obtained, to obtain chlorophillins copper acid sodium with chlorophyll cupric acid in sodium hydroxide.GB 26406-2011
It discloses and extracts silkworm excrement using organic solvent, standard of the sodium copper chlorophyllin obtained through saponification, copper generation as food additives,
It is required that production when strict control free copper content, absorbance E405nm >=568.As people recognize sodium copper chlorophyllin
Be gradually increased, more and more people select plant extract mode obtain sodium copper chlorophyllin, to preparation process require very
It is high.
Ginkgo biloba p.e (Ginko Biloba Extract, GBE) is to be with the leaf of ginkgo Ginkgo biloba L.
Raw material, using extraction, a kind of product that column chromatography enriching and purifying obtains, the content of active constituent be GINKGO BILOBA EXTRACT >=
24 wt%, ginkgolides >=26 wt%.Since ginkgo biloba p.e has expansion blood vessel, improvement microcirculation, thrombus etc.
Effect can be made various preparations using it as raw material, for treating various cardiovascular and cerebrovascular diseases, thus be widely used in medicine
The fields such as object, health care product, food additives, functional beverage, cosmetics.Sodium copper chlorophyllin is prepared not using ginkgo leaf
The content of free copper is only controlled, Ginkgolic Acid in Extract of Ginkgo biloba Leaves is the objectionable impurities being primarily present in product, it is not easy to quilt
Separation greatly affects product preparation and purification.
Chinese patent CN 108451988A discloses a kind of preparation that sodium copper chlorophyllin is obtained using enzyme hydrolysis ginkgo leaf
Method, this method are needed using a large amount of protease and cellulase, and the ginkgo acid content that cannot be effectively reduced in product, are made
It is excessive to obtain product impurity, is in muddy shape after water-soluble.
Chinese patent CN 104725387A, which is disclosed, extracts ginkgo leaf using ethyl alcohol, isopropanol and No. 6 solvent naphtha mixing
The method of extract Determination of Chlorophyll copper sodium, the method use a large amount of No. 6 solvent naphthas, alcohol phase increases containing there are many in system
The step of post-processing, can obtain the emulsion layer of suitable thickness after the step saponification, and magazine content is higher in product, be dissolved in
Precipitating is formed after water.And the ginkgoic acid (20-50ppm) in system cannot be effectively reduced in this method.
Summary of the invention
Goal of the invention: the object of the present invention is to provide one kind by optimization purifying technique, eliminates emulsion layer to substantially subtract
The plant source chlorophyll copper sodium salt production process of few ginkgo acid content, for obtaining the transparent copper chlorophyll of high yield, aqueous solution
Sodium salt.
Technical solution: in order to achieve the above-mentioned object of the invention, a kind of emulsion resistance of plant source sodium copper chlorophyllin of the invention
Preparation method includes the following steps:
(1) ginkgo leaf is crushed, alcoholic solution extraction, filtering concentrates the filtrate to no alcohol, obtains black medicinal extract；
(2) the black medicinal extract is added in the alcoholic solution of petroleum ether, stirring, stratification；It isolates petroleum ether phase and is added
First alcoholic solvent stirring alcohol is washed, stratification；
(3) the second alcoholic solvent and diluted alkaline is added in the petroleum ether solution finally obtained suddenly one step up, isolates transparent petroleum ether
Phase；
(4) strong alkali alcosol is added into transparent petroleum ether phase and carries out saponification, stratification；It is added after isolating alcohol phase
Petroleum ether and stirring extraction；
(5) sulfuric acid acidification is added in the alcohol phase solution finally obtained suddenly one step up, petroleum ether and stirring extraction is then added；
(6) copper sulphate thermal reflow is added to color greening in the alcohol phase that rapid extraction obtains one step up, cooling is concentrated into nothing
Alcohol, washing, then be concentrated, dry, obtain chlorophyll cupric acid；
(7) chlorophyll ketonic acid is redissolved, equivalent sodium hydroxide is added to neutralize, drying obtains chlorophillins copper sodium.
Method of the invention is: the ginkgo leaf black medicinal extract obtained to extraction is pure using pure and mild petroleum ether progress separating for several times
Change, isolates the impurity in petroleum ether phase first with solvent partition, after saponification, active constituent is mutually transferred to alcohol from petroleum ether
Then phase, then isolate the impurity in alcohol phase with petroleum ether extraction is acidified, petroleum ether extraction and copper Dai Fanying again.Due to
Emulsion before saponification will have a direct impact on saponification, product purity, thus how to select suitable extraction agent, how
It is separated, so that minimizing emulsion layer is the main problem that the present invention solves.Since emulsion layer problem is effectively solved,
So that the purity of sodium copper chlorophyllin of the present invention improves, product coloration and transparency are outstanding, and are conducive to further decrease body
The content of ginkgoic acid in system.
This method while producing ginkgo biloba p.e, using the black generated in extraction process discard stickies as
Raw material prepares sodium copper chlorophyllin, not only realizes the comprehensive utilization of ginkgo leaf, reduces production cost, while alleviating ring
Border pollution.
The reflux extraction of 85% -95% (V/V) ethanol solution, water-bath are added to smashed ginkgo leaf in the step (1)
Temperature is 85-90 DEG C, merging filtrate after extraction filtering.Preferably, reflux extraction, the filtering in step (1) to ginkgo leaf is crushed
Step repeats 1-2 times.It is highly preferred that utilizing the reflux extraction of 90% (V/V) ethanol solution, return time in the step (1)
It is no more than 3 hours every time.
In the step (2), the first alcoholic solvent is the ethanol solution of 60%-95% (V/V), and alcohol is washed total progress 2-3 times, closed
And petroleum ether phase.It is preferred that with the ethanol solution of 65%-80% (V/V), it is highly preferred that first alcoholic solvent selects 70% (V/V)
Ethanol solution.In the step (3), the second alcoholic solvent is the ethanol solution of 45%-85% (V/V), which carries out 1-3 altogether
It is secondary.Preferably, second alcoholic solvent selects the ethanol solution of 50%-65% (V/V).
It is worth noting that, generally passing through to the conventional demulsification processing of emulsion and heating being added, be added in chemical field
Methanol, acetone, inorganic salts, acid etc. reagent promote to be layered.But in the present invention, due to being extracted using two kinds of organic phases,
A variety of organic solvents, which are added, will affect effect of extracting and is unfavorable for increasing the recovery difficult of solvent when producing, and inorganic salts and acid is added
The effect for abolishing emulsification completely can not be played.In step (2) and step (3), the present invention distinguishes the concentration of alcohol solvent
It comes and is first post-processed, substantially reduce the thickness of emulsion layer in the case where not adding additional solvent or demulsifier, when extraction
Alcoholic solvent concentration must be paid special attention to, if excessive concentration, be layered unobvious；Concentration is too low, and emulsification is serious, and impurity-eliminating effect is poor.Step
Suddenly by addition diluted alkaline in (3), and due to the concentration of control ethyl alcohol, unexpected complete demulsification is obtained.
Diluted alkaline in the step (3) is ammonium hydroxide, sodium hydroxide, potassium hydroxide, any one in sodium carbonate liquor.It is excellent
It is selected as sodium hydroxide solution.
Further, the diluted alkaline additional amount is 0.05-5 % (m/V) of the second alcoholic solvent, and the amount of being preferably added to is
0.05-1 % (m/V), it is highly preferred that being 0.1-0.2% (m/V).
Highly basic in the step (4) is any one of NaOH, KOH, preferably potassium hydroxide.The alcohol that highly basic is added is molten
Liquid after saponification reacts 3-5 hours.Highly basic additional amount is the 1.0-5.0% (m/V) of alcoholic solution, and petroleum ether room temperature is added and extracts 1-3
It is secondary.
The step (5) adjusts pH to pH to 1-4 after sulfuric acid is added, then petroleum ether is added in preferably pH to 1.5-2.5
Room temperature extracts 1-3 times.
Copper generation reaction is to be heated up to 40-60 DEG C after copper-bath is added in the step (6), reflux 10 minutes to solution
Gradually greening, after 1 hour, reflux stops, cooling.In step (6), methyl acetate, ethyl acetate, propyl acetate are selected in washing
Any one is extracted, and is preferably extracted with ethyl acetate.Extraction Shi Jiashui discards lower layer's water phase, repeats washing 1-2 times.
It is mixed when the present invention is mutually extracted using ethyl alcohol and petroleum ether according to ethyl alcohol, petroleum ether volume ratio 1:3 ~ 1:5,
Preferred volume ratio is 1:4, for example, being directed to 100g ginkgo leaf extract, is extracted using 100ml ethyl alcohol and 400ml petroleum ether.
The utility model has the advantages that the present invention is only purified with the two kinds of solvent extractions of ethyl alcohol and petroleum ether, avoid in system that there are a variety of
Organic solvent influence is to extracting and demixing；Ginkgo leaf crushes extraction using multi-reflow in short-term, merges the mode of leaching liquor, improves
Product yield；It successively cleans in petroleum ether phase and alcohol phase, the cream of saponification front and back is significantly reduced by control solvent strength
Change lamination, ensure that the yield and purity of product, is effectively stripped of 90% or more ginkgoic acid, the leaf that this method obtains
Green element absorbance>=600 copper acid sodium E405nm, absorbance ratio 3.1 ~ 3.58, complex copper>=6.2%, ginkgoic acid<1.0ppm produce
Product yield is up to 0.4%.
Specific embodiment
Specific embodiments of the present invention are further described below, in the case where no additional description, alcoholic solvent
It is indicated using percent by volume (V/V).
Embodiment 1
1)The preparation of ginkgo leaf medicinal extract
100 grams of ginkgo leaves are taken to crush, first extraction is extracted 3 hours using 90% alcohol reflux, and bath temperature is 90 DEG C, gauze mistake
Filter；Then it extracts 3 hours again, filtered through gauze, merging filtrate, heating is stirred evenly, is cooled to room temperature, and filtering is stand-by.It is concentrated under reduced pressure
It to medicinal extract shape, is dissolved in water, is centrifuged, obtains dark viscous object.
2)Petroleum ether phase abstraction impurity removal
95% ethyl alcohol 100ml, petroleum ether 400ml is added in aforementioned medicinal extract, stirs 0.5-1.5 hours, is filtered under diminished pressure, and is transferred to liquid separation leakage
Bucket is stood, it is seen that obvious boundary layer throws aside lower layer's alcohol phase.Then 70% ethyl alcohol stirring alcohol is added to wash 30 minutes, stratification is abandoned
Set lower layer's alcohol phase.Alcohol washes total carry out 2 times.
Then the sodium hydroxide of 62% ethyl alcohol and 0.15% (m/V), stirring 30 are added in the petroleum ether phase after washing to aforementioned alcohol
Minute, lower layer's alcohol phase is thrown aside, alcohol phase pH is 9-10, the sodium hydroxide of 62% ethyl alcohol and 0.15% (m/V) is then added again, then
Secondary stirring, stratification, alcohol phase pH is 11-12 at this time.Obtain transparent petroleum ether phase.
3)Saponification
95% alcoholic solution that naoh concentration is 4.0% (m/V) is added into transparent petroleum ether phase, it is ordinary-temp hydrolysis 4 hours, quiet
It sets and separates lower layer's alcohol phase.
4)Alcohol phase abstraction impurity removal
Alcohol phase after saponification adds petroleum ether extraction removal of impurities, is repeated twice.Petroleum ether 50ml is added in extraction, stirs 10 points
Clock, stratification.
5)Acidification
The acidification of 9M sulfuric acid is added in the alcohol phase solution finally obtained suddenly one step up, pH is adjusted to 2-3, stirs 10 minutes, filtrate
Petroleum ether extraction is added three times, retains alcohol phase.
6)Copper Dai Fanying
20% (m/V) copper-bath is added in the alcohol phase that rapid extraction obtains one step up, 55 DEG C are flowed back 60 minutes, at this time alcohol phase
Gradually greening cools down after the reaction was completed, is concentrated into no alcohol.
7)Finished product preparation
After concentration three times using ethyl acetate washing, lower layer's water phase is discarded.Ethyl acetate phase is concentrated, 95% ethyl alcohol is added, water-bath is steamed
Wherein moisture and alcohol are sent out, obtains dry product 0.41g after drying is dry.
It is that 600, E630nm absorbance is that the chlorophyll cupric acid sodium yield that this method obtains, which is 0.41%, E405nm absorbance,
191, absorbance ratio 3.14, ginkgo acid content is less than 1ppm.
Embodiment 2
1)The preparation of ginkgo leaf medicinal extract
100 grams of ginkgo leaves are taken to crush, first extraction is extracted 3 hours using 90% alcohol reflux, and bath temperature is 90 DEG C, gauze mistake
Filter；Then it extracts 3 hours again, filtered through gauze, merging filtrate, heating is stirred evenly, is cooled to room temperature, and filtering is stand-by.It is concentrated under reduced pressure
It to medicinal extract shape, is dissolved in water, is centrifuged, obtains dark viscous object.
2)Petroleum ether phase abstraction impurity removal
95% ethyl alcohol 100ml, petroleum ether 400ml is added in aforementioned medicinal extract, stirs 0.5-1.5 hours, is filtered under diminished pressure, and is transferred to liquid separation leakage
Bucket is stood, it is seen that obvious boundary layer throws aside lower layer's alcohol phase.Then 60% ethyl alcohol stirring alcohol is added to wash 30 minutes, stratification is abandoned
Set lower layer's alcohol phase.Alcohol washes total carry out 2 times.
Then the sodium hydroxide of 60% ethyl alcohol and 0.10% (m/V), stirring 30 are added in the petroleum ether phase after washing to aforementioned alcohol
Minute, lower layer's alcohol phase is thrown aside, petroleum ether phase pH is 12-13, and the hydroxide of 60% ethyl alcohol and 0.10% (m/V) is then added again
Sodium is again stirring for, stratification.Obtain transparent petroleum ether phase.
3)Saponification
95% alcoholic solution that naoh concentration is 3.0% (m/V) is added into transparent petroleum ether phase, it is ordinary-temp hydrolysis 5 hours, quiet
It sets and separates lower layer's alcohol phase.
4)Alcohol phase abstraction impurity removal
Alcohol phase after saponification adds petroleum ether extraction removal of impurities, and petroleum ether 50ml is added in extraction, stirs 10 minutes, standing point
Layer.
5)Acidification
The acidification of 9M sulfuric acid is added in the alcohol phase solution finally obtained suddenly one step up, pH is adjusted to 2-3, stirs 10 minutes, it filters,
Petroleum ether extraction is added three times in filtrate, retains alcohol phase.
6)Copper Dai Fanying
20% (m/V) copper-bath is added in the alcohol phase that rapid extraction obtains one step up, 55 DEG C are flowed back 60 minutes, at this time alcohol phase
Gradually greening cools down after the reaction was completed, is concentrated into no alcohol.
7)Finished product preparation
After concentration three times using ethyl acetate washing, lower layer's water phase is discarded.Ethyl acetate phase is concentrated, ethyl alcohol, water-bath evaporation is added
Wherein moisture and alcohol obtain dry product 0.39g after drying is dry.
It is that 630, E630nm absorbance is that the chlorophyll cupric acid sodium yield that this method obtains, which is 0.39%, E405nm absorbance,
190；Absorbance ratio is 3.31, and ginkgo acid content is less than 1ppm.
Embodiment 3
1)The preparation of ginkgo leaf medicinal extract
100 grams of ginkgo leaves are taken to crush, first extraction is extracted 3 hours using 90% alcohol reflux, and bath temperature is 90 DEG C, gauze mistake
Filter；Then it extracts 3 hours again, filtered through gauze, merging filtrate, heating is stirred evenly, is cooled to room temperature, and filtering is stand-by.It is concentrated under reduced pressure
It to medicinal extract shape, is dissolved in water, is centrifuged, obtains dark viscous object.
2)Petroleum ether phase abstraction impurity removal
95% ethyl alcohol 100ml, petroleum ether 300ml is added in aforementioned medicinal extract, stirs 0.5-1.5 hours, is filtered under diminished pressure, and is transferred to liquid separation leakage
Bucket is stood, it is seen that obvious boundary layer throws aside lower layer's alcohol phase.Then 95% ethyl alcohol stirring alcohol is added to wash 30 minutes, stratification is abandoned
Set lower layer's alcohol phase.Alcohol washes total carry out 2 times.
3)Saponification
95% alcoholic solution that naoh concentration is 4.0% (m/V) is added into transparent petroleum ether phase, it is ordinary-temp hydrolysis 4 hours, quiet
It sets and separates lower layer's alcohol phase.
4)Alcohol phase abstraction impurity removal
Alcohol phase after saponification adds petroleum ether extraction removal of impurities, is repeated twice.Petroleum ether 50ml is added in extraction, stirs 10 points
Clock, stratification.
5)Acidification
The acidification of 9M sulfuric acid is added in the alcohol phase solution finally obtained suddenly one step up, pH is adjusted to 2-3, stirs 10 minutes, it filters,
Petroleum ether extraction is added three times in filtrate, retains alcohol phase.
6)Copper Dai Fanying
20% (m/V) copper-bath is added in the alcohol phase that rapid extraction obtains one step up, 55 DEG C are flowed back 60 minutes, at this time alcohol phase
Gradually greening cools down after the reaction was completed, is concentrated into no alcohol.
7)Finished product preparation
After concentration three times using ethyl acetate washing, lower layer's water phase is discarded.Ethyl acetate phase is concentrated, ethyl alcohol, water-bath evaporation is added
Wherein moisture and alcohol obtain dry product 2.0g after drying is dry.
It is that 150, E630nm absorbance is that the chlorophyll cupric acid sodium yield that this method obtains, which is 2.0%, E405nm absorbance,
89, absorbance ratio 1.68, ginkgo acid content is greater than 10000ppm.Although the product high income that this method obtains, right product
Middle impurity is more, and product can not be dried, and to be thick, being added to the water has a large amount of precipitatings.
It is to be unable to reach from the embodiments above as can be seen that alcohol and extracting process using normal concentration are purified
The present invention such as technical effect of embodiment 1.
Claims (10)
1. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin, which comprises the steps of:
(1) ginkgo leaf is crushed, alcoholic solution extraction, filtering concentrates the filtrate to no alcohol, obtains black medicinal extract；
(2) the black medicinal extract is added in the alcoholic solution of petroleum ether, stirring, stratification；It isolates petroleum ether phase and is added
First alcoholic solvent stirring alcohol is washed, stratification；
(3) the second alcoholic solvent and diluted alkaline is added in the petroleum ether solution finally obtained suddenly one step up, isolates transparent petroleum ether
Phase；
(4) strong alkali alcosol is added into transparent petroleum ether phase and carries out saponification, stratification；It is added after isolating alcohol phase
Petroleum ether and stirring extraction；
(5) sulfuric acid acidification is added in the alcohol phase solution finally obtained suddenly one step up, petroleum ether and stirring extraction is then added；
(6) copper sulphate thermal reflow is added to color greening in the alcohol phase that rapid extraction obtains one step up, cooling is concentrated into nothing
Alcohol, washing, then be concentrated, dry, obtain chlorophyll cupric acid；
(7) chlorophyll ketonic acid is redissolved, equivalent sodium hydroxide is added to neutralize, drying obtains chlorophillins copper sodium.
2. a kind of emulsion resistance method for preparing sodium copper chlorophyllin from ginkgo leaf according to claim 1, it is characterised in that:
The reflux extraction of 85% -95% (V/V) ethanol solution is added to smashed ginkgo leaf in the step (1), bath temperature is
85-90 DEG C, merging filtrate after extraction filtering.
3. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 1, it is characterised in that: institute
The ethanol solution that the first alcoholic solvent is 60%-95% (V/V) is stated, the alcohol of step (2) washes total carry out 2-3 times.
4. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 1, it is characterised in that: institute
The ethanol solution that the second alcoholic solvent is 45%-85% (V/V) is stated, step (3) carries out 1-3 times altogether.
5. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 4, it is characterised in that: institute
The diluted alkaline in step (3) is stated as any one in ammonium hydroxide, sodium hydroxide, potassium hydroxide, sodium carbonate.
6. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 5, it is characterised in that:
The diluted alkaline additional amount is 0.05-5 % (m/V) of the second alcoholic solvent.
7. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 1, it is characterised in that: institute
Any one that the highly basic in step (4) is NaOH, KOH is stated, strong alkali alcosol after saponification is added and reacts 3-5 hours.
8. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 7, it is characterised in that: institute
The 1.0-5.0% (m/V) that highly basic additional amount in step (4) is alcoholic solution is stated, petroleum ether room temperature is added and extracts 1-3 times.
9. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 1, it is characterised in that: institute
It states after sulfuric acid is added in step (5) and adjusts pH to 1-4, petroleum ether room temperature is then added and extracts 1-3 times.
10. a kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin according to claim 1, it is characterised in that:
Any one of washing selection methyl acetate, ethyl acetate, propyl acetate are extracted in the step (6), and water is added to discard down
Layer water phase, repeats washing 1-2 times.
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| CN109705127B (en) | 2020-04-14 |
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Address after: 210000 building C, Shilin Industrial Park, No. 10, Wanshou Road, Jiangbei new area, Nanjing, Jiangsu Patentee after: Nanjing sbaike Biotechnology Co.,Ltd. Address before: 210000 floor 5, building C, Shilin Industrial Park, No. 10, Wanshou Road, Pukou District, Nanjing, Jiangsu Province Patentee before: SPEC-CHEM INDUSTRY Inc. |
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Denomination of invention: A Method for Preparing Plant Derived Sodium Copper Chlorophyll Salt for Anti emulsification Effective date of registration: 20230419 Granted publication date: 20200414 Pledgee: Nanjing Branch of Jiangsu Bank Co.,Ltd. Pledgor: Nanjing sbaike Biotechnology Co.,Ltd. Registration number: Y2023980038503 |