CN107383113A - A kind of preparation method of coproduction apple polyphenol - Google Patents
A kind of preparation method of coproduction apple polyphenol Download PDFInfo
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- CN107383113A CN107383113A CN201710520084.5A CN201710520084A CN107383113A CN 107383113 A CN107383113 A CN 107383113A CN 201710520084 A CN201710520084 A CN 201710520084A CN 107383113 A CN107383113 A CN 107383113A
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- apple
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
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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
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- 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
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
Abstract
The invention discloses a kind of preparation method of coproduction apple polyphenol, it is characterised in that comprises the following steps：1. using apple as raw material squeezing, extraction, separation, apple extract solution is obtained；2. apple extract solution carries out adsorbing separation using macroreticular resin, water-soluble, fat-soluble two parts are separated into；3. water-soluble portion the apple extract product of high polyphenolic content, highly-water-soluble is obtained into；Fatty contents are obtained to 3 chlorogenic acid, phloridzin, phloretin Phytochemistry monomer components successively.A kind of preparation method of coproduction apple polyphenol of the present invention, overcomes the defects of current extraction process extract is single, solves the existing mass defect of apple polyphenol product, improves raw material resources utilization rate, reduces comprehensive production cost.
Description
Technical field
The invention belongs to field of biological extraction, more particularly to a kind of preparation method of coproduction apple polyphenol.
Background technology
Apple polyphenol is favored using its superior performance by people.Current apple extract manufacturing enterprise master large-scale in the world
To obtain 75% apple polyphenol extract using macroporous resin adsorption separating-purifying, but its product poorly water-soluble, extract product
Single, resource utilization is low.Domestic apple polyphenol is because starting late in market, and extraction process more falls behind, and apple polyphenol product contains
Amount is between 50%-75%.Simultaneously because the reason for raw material and process aspect, the residual content of agriculture of existing product is left in 100ppm
It is right.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of coproduction apple polyphenol, overcome current extraction process and carry
The defects of taking thing single, solve the existing mass defect of apple polyphenol product, improve raw material resources utilization rate, reduce synthesis
Production cost.
Technical scheme：A kind of preparation method of coproduction apple polyphenol, it is characterised in that comprise the following steps：
1. being squeezed by raw material of apple, the skin slag after squeezing is extracted with warm water, obtains the Aqueous extracts in waste residue, then by entering
One step separates, and obtains apple extract solution；
2. carrying out adsorbing separation using macroreticular resin to above-mentioned apple extract solution, apple extract solution is separated into water-soluble, liposoluble
Property two parts；
3. above-mentioned water-soluble portion is separated using nanofiltration membrane, wherein condensed tannin and large biological molecule material are removed, is obtained
The apple extract product of high polyphenolic content, highly-water-soluble is arrived；Above-mentioned fatty contents are used into simulated moving bed technology, led to
To cross and more root chromatogram columns are cascaded, fatty contents circulate direction exchange-column shift along organic solvent mobile phase,
So as to the inlet and outlet position of periodically-varied material, the adverse current movement between stationary phase and mobile phase is realized, is realized between component
Continuous separation, obtain 3 chlorogenic acid, phloridzin, phloretin Phytochemistry monomer components successively.
A kind of preparation method of foregoing coproduction apple polyphenol, step 1. in, the apple is wild for non agricultural chemical residuum
Apple.
A kind of preparation method of foregoing coproduction apple polyphenol, step 1. in, inert gas is used in the expressing process
Protection.
A kind of preparation method of foregoing coproduction apple polyphenol, the inert gas are nitrogen.
A kind of preparation method of foregoing coproduction apple polyphenol, step 2. in, the macroreticular resin is about for average pore size
40-90 angstroms, than the polystyrene backbone or polystyrene framework material that surface is 400-760 ㎡/g
A kind of preparation method of foregoing coproduction apple polyphenol, step 3. in, the water-soluble portion by using retention molecule
2000-2200Da NF membrane is measured, is separated by filtration under 3-5MPa hyperosmosis, obtains the apple that polyphenol content is higher than 80%
Extract product.
Compared with prior art, after the present invention squeezes the juice wilding, by macroporous resin adsorption, further using nanofiltration
Membrane separation technique, separating-purifying apple polyphenol, and work chromatographic technique is introduced, the fatty contents extraction point that UF membrane is discarded
From obtaining 3 kinds of phloridzin, phloretin, chlorogenic acid high added value apple source Phytochemistry monomer components.
It it is about 40-90 angstroms using average pore size, than the polystyrene backbone or polystyrene bone that surface is 400-760 ㎡/g
Frame material macroreticular resin carries out adsorbing separation, and apple extract solution is separated into water-soluble, fat-soluble two parts.By water-soluble portion
Point, continue to separate using nanofiltration membrane, remove wherein condensed tannin and large biological molecule material, obtained high polyphenolic content,
The apple extract product of highly-water-soluble.Apple polyphenol class molecular weight of material is general all below 1000, by the present invention in that with
The NF membrane of molecular cut off more than 2000, under 5MPa hyperosmosis, by things such as the pectin of macromolecular, polysaccharide, amino acid
Matter is trapped in outside NF membrane, has obtained the apple extract product that polyphenol content is higher than 80%, and by this Project Product polyphenol
Water solubility greatly improve；Also, on the basis of apple polyphenol is apple extract unique Product, introduce Simulation moving bed color
Spectral technology, 3 phloridzin, phloretin, chlorogenic acid plants are obtained using the fatty contents discarded object of macroreticular resin chromatography
Thing chemistry monomer component, the defects of overcoming current extraction process extract single, improve raw material resources utilization rate, carry significantly
The high added value of unit raw material, reduces comprehensive production cost.
Present invention employs the method for water seal and inert gas shielding, that is, avoids the brown stain of apple polyphenol, reduce again
SO2 addition.Detailed process is：After the cleaning of apple raw material, increase a nitrogen cylinder on broken disintegrating machine so that broken
During the gas that contacts be nitrogen, crush the apple fine grained to get off and be directly entered in water（By negative pressure, low latitude gas residual
Water）, apple raw material and air contact are avoided, in a nitrogen environment using screw pump, product pump is pressed into squash type squeezer
Squeeze.Pomace is discharged into the water of extraction after squeezing, is carried out water seal extraction, extract solution filtering and concentrating, is carried out next step separation.
Using this kind of technology, the quinoneization for avoiding follow-up process-scale chromatography separation root skin glycoside material turns pink process, obtained list
Body compound is pure white.
Apple polyphenol product good water solubility, the inoxidizability of the present invention is strong, alternative external import product and traditional
Industrial antioxidant（BHT）For food antioxidant.
Embodiment
The present invention is further illustrated for example below, but is not intended as the foundation limited the present invention.
Embodiment：
A kind of preparation method of coproduction apple polyphenol, comprises the following steps：
1. being squeezed by raw material of apple, the skin slag after squeezing is extracted with warm water, obtains the Aqueous extracts in waste residue, then by entering
One step separates, and obtains apple extract solution；
2. carrying out adsorbing separation using macroreticular resin to above-mentioned apple extract solution, apple extract solution is separated into water-soluble, liposoluble
Property two parts；
3. above-mentioned water-soluble portion is separated using nanofiltration membrane, wherein condensed tannin and large biological molecule material are removed, is obtained
The apple extract product of high polyphenolic content, highly-water-soluble is arrived；Above-mentioned fatty contents are used into simulated moving bed technology, led to
To cross and more root chromatogram columns are cascaded, fatty contents circulate direction exchange-column shift along organic solvent mobile phase,
So as to the inlet and outlet position of periodically-varied material, the adverse current movement between stationary phase and mobile phase is realized, is realized between component
Continuous separation, obtain 3 chlorogenic acid, phloridzin, phloretin Phytochemistry monomer components successively.
Further, step 1. in, the apple be non agricultural chemical residuum wilding.
Further, step 1. in, inert gas shielding is used in the expressing process.
Further, step 1. in, the inert gas is nitrogen.
Further, step 2. in, the macroreticular resin be average pore size be about 40-90 angstroms, be 400-760 than surface
㎡/g polystyrene backbone or polystyrene framework material
Further, step 3. in, the water-soluble portion by using molecular cut off 2000-2200Da NF membrane,
It is separated by filtration under 3-5MPa hyperosmosis, obtains the apple extract product that polyphenol content is higher than 80%.
The present invention has following innovation：
1st, the plant monomer component in four kinds of apple sources such as apple polyphenol is extracted using joint production process, overcomes current extraction process to carry
The defects of taking thing single, solve the existing mass defect of apple polyphenol product, improve raw material resources utilization rate, reduce synthesis
Production cost；
2nd, recycling has been carried out to wilding resource and squeezing skin slag, has improved product yield and quality, reduces list
Position production cost, improves competitive power of product；
3rd, this project uses water seal and inert gas shielding method first, instead of the SO2 protection techniques of Japanese ASAHI companies, has
Effect prevents the oxidizing process in production process, obtained light Polyphenols product and pure white monomeric compound；
4th, this project apple polyphenol product good water solubility, inoxidizability are strong, alternative external import product and traditional industry
Antioxidant（BHT）For food antioxidant.
Claims (6)
1. a kind of preparation method of coproduction apple polyphenol, it is characterised in that comprise the following steps：
1. being squeezed by raw material of apple, the skin slag after squeezing is extracted with warm water, obtains the Aqueous extracts in waste residue, then by entering
One step separates, and obtains apple extract solution；
2. carrying out adsorbing separation using macroreticular resin to above-mentioned apple extract solution, apple extract solution is separated into water-soluble, liposoluble
Property two parts；
3. above-mentioned water-soluble portion is separated using nanofiltration membrane, wherein condensed tannin and large biological molecule material are removed, is obtained
The apple extract product of high polyphenolic content, highly-water-soluble is arrived；Above-mentioned fatty contents are used into simulated moving bed technology, led to
To cross and more root chromatogram columns are cascaded, fatty contents circulate direction exchange-column shift along organic solvent mobile phase,
So as to the inlet and outlet position of periodically-varied material, the adverse current movement between stationary phase and mobile phase is realized, is realized between component
Continuous separation, obtain 3 chlorogenic acid, phloridzin, phloretin Phytochemistry monomer components successively.
A kind of 2. preparation method of coproduction apple polyphenol according to claim 1, it is characterised in that step 1. in, it is described
Apple is the wilding of non agricultural chemical residuum.
A kind of 3. preparation method of coproduction apple polyphenol according to claim 1, it is characterised in that step 1. in, it is described
Inert gas shielding is used in expressing process.
4. the preparation method of a kind of coproduction apple polyphenol according to claim 2, it is characterised in that the inert gas is
Nitrogen.
A kind of 5. preparation method of coproduction apple polyphenol according to claim 1, it is characterised in that step 2. in, it is described
Macroreticular resin is that average pore size is about 40-90 angstroms, than the polystyrene backbone or polystyrene skeleton that surface is 400-760 ㎡/g
Material.
A kind of 6. preparation method of coproduction apple polyphenol according to claim 1, it is characterised in that step 3. in, it is described
Water-soluble portion is separated by filtration under 3-5MPa hyperosmosis by using molecular cut off 2000-2200Da NF membrane,
Obtain the apple extract product that polyphenol content is higher than 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710520084.5A CN107383113A (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method of coproduction apple polyphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710520084.5A CN107383113A (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method of coproduction apple polyphenol |
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| Publication Number | Publication Date |
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| CN107383113A true CN107383113A (en) | 2017-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710520084.5A Withdrawn CN107383113A (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method of coproduction apple polyphenol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512082A (en) * | 2021-08-10 | 2021-10-19 | 湖南绿蔓生物科技股份有限公司 | Method for extracting phlorizin and phloretin in apple root bark and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2935096A1 (en) * | 2008-08-21 | 2010-02-26 | Cooperative Agricole D Elle Et | Composition of fruit extract of Rosaceae family seeds, useful to prepare e.g. food composition, comprises polyphenols, chlorogenic acid and combination of flavonols (quercetin), dihydrochalcone (phloridzin), and flavanols (catechins) |
| CN102697895A (en) * | 2012-06-11 | 2012-10-03 | 陕西师范大学 | Method for continuously extracting total polyphenol, chlorogenic acid and phlorizin from green apples |
| CN104721301A (en) * | 2015-01-12 | 2015-06-24 | 中国人民武装警察部队后勤学院 | Apple polyphenol ethanol extract as well as preparation method and application thereof |
| CN105111256A (en) * | 2015-08-16 | 2015-12-02 | 李玉山 | Integrated extracting and purifying method for active ingredients of apple pomace |
-
2017
- 2017-06-30 CN CN201710520084.5A patent/CN107383113A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2935096A1 (en) * | 2008-08-21 | 2010-02-26 | Cooperative Agricole D Elle Et | Composition of fruit extract of Rosaceae family seeds, useful to prepare e.g. food composition, comprises polyphenols, chlorogenic acid and combination of flavonols (quercetin), dihydrochalcone (phloridzin), and flavanols (catechins) |
| CN102697895A (en) * | 2012-06-11 | 2012-10-03 | 陕西师范大学 | Method for continuously extracting total polyphenol, chlorogenic acid and phlorizin from green apples |
| CN104721301A (en) * | 2015-01-12 | 2015-06-24 | 中国人民武装警察部队后勤学院 | Apple polyphenol ethanol extract as well as preparation method and application thereof |
| CN105111256A (en) * | 2015-08-16 | 2015-12-02 | 李玉山 | Integrated extracting and purifying method for active ingredients of apple pomace |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512082A (en) * | 2021-08-10 | 2021-10-19 | 湖南绿蔓生物科技股份有限公司 | Method for extracting phlorizin and phloretin in apple root bark and application thereof |
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Application publication date: 20171124 |
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