CN112811997A - Production process for extracting and purifying phloretin from apple flowers - Google Patents
Production process for extracting and purifying phloretin from apple flowers Download PDFInfo
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- CN112811997A CN112811997A CN202110229944.6A CN202110229944A CN112811997A CN 112811997 A CN112811997 A CN 112811997A CN 202110229944 A CN202110229944 A CN 202110229944A CN 112811997 A CN112811997 A CN 112811997A
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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
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a production process for extracting and purifying phloretin from apple flowers, which comprises the following steps: pretreating raw materials, pulverizing apple flower raw materials into coarse powder raw materials, bagging for later use, extracting, dynamically extracting the coarse powder raw materials twice at normal temperature by using a mixed solvent to obtain a raw material extracting solution, concentrating the raw material extracting solution at normal pressure, reducing the volume and the weight, and crystallizing. The invention has the beneficial effects that: the invention provides a new safe source mode of pure natural phloretin. In the invention, the mixed solvent is used for extraction, so that the extraction of polar components is reduced, and the subsequent separation and purification is facilitated; the method extracts, concentrates and crystallizes the apple powder raw material, so that the content of phloretin can reach about 85%, and the content of phloretin can reach more than 98% through decoloring and crystallization.
Description
Technical Field
The invention relates to a production process for extracting and purifying phloretin from apple flowers, in particular to a production process for extracting and purifying phloretin from apple flowers, and belongs to the technical field of production process application of phloretin from dried apple flowers.
Background
The apple flower is flower of perennial deciduous tree of Rosaceae, and is white trumpet-shaped. Phloretin, also known as trishydroxyphenylacetone 2,4, 6-trihydroxy-3- (4-hydroxyphenyl) propiophenone. Is a novel natural skin whitening agent, and is mainly distributed in pericarp and root bark of succulent fruits such as apple, pear, etc. The phloretin can be applied in facial mask, skin cream, lotion and essence. Is pearl white crystal powder, can be dissolved in ethanol and acetone, and is almost insoluble in water.
The existing production process for extracting the phloretin from the apple flowers is easy to extract excessive polar components during implementation, is not beneficial to the subsequent separation and purification of the phloretin, and has lower purity and incomplete extraction.
Disclosure of Invention
The invention aims to solve the problems that the existing production process for extracting phloretin from apple flowers is easy to extract excessive polar components during implementation and is not beneficial to subsequent separation and purification of the phloretin; the invention provides a novel and safe source mode of pure natural phloretin, and the invention uses mixed solvent extraction to reduce extraction of polar components and is beneficial to subsequent separation and purification. The method extracts, concentrates and crystallizes the apple powder raw material, so that the content of phloretin can reach about 85%, and the content of phloretin can reach more than 98% through decoloring and crystallization.
The purpose of the invention can be realized by the following technical scheme: a production process for extracting and purifying phloretin from apple flowers specifically comprises the following steps:
the method comprises the following steps: pretreating raw materials, namely crushing the apple flower raw materials into coarse powder raw materials, and bagging for later use;
step two: extracting, namely dynamically extracting the coarse powder raw material twice by using a mixed solvent at normal temperature to obtain a raw material extracting solution;
step three: concentrating, namely concentrating the raw material extracting solution under normal pressure to reduce the volume and the weight;
step four: and (3) crystallization: crystallizing the concentrated raw material extract at normal temperature, and performing suction filtration to obtain yellow green or off-white powder coarse crystals;
step five: recrystallizing, heating and dissolving the powder crude crystals with ethanol to obtain a solution, adding activated carbon into the solution for decoloring, and cooling and crystallizing to obtain white powder crystals;
step six: and (5) performing suction filtration and drying, performing suction filtration on the white powder crystals obtained in the step five, and performing crystal drying to obtain a 98% phloretin product.
Preferably, the mixed solvent in the second step is prepared from ethyl acetate and acetone, and the volume ratio of the ethyl acetate to the acetone is 1: 1-4: 1.
Preferably, the apple flower raw material is crushed in the step one, and the granularity is less than 3 mm.
Preferably, in the second step, the extraction time of the coarse powder raw material dynamically extracted twice by the mixed solvent at normal temperature is 2 hours and 1.5 hours respectively, and the dosage of the mixed solvent extracted twice is respectively the weight of the raw material: the volume of the mixed solvent (M: V) is 6 times and 5 times.
Preferably, the concentration degree in the step three is 0.3 to 0.2 times of the raw material extracting solution.
Preferably, the concentration of the ethanol used in the fifth step is 95%, the dosage of the ethanol is 8 times of the crude crystals of the powder, and the dosage of the ethanol added is 2% of the solution.
Preferably, the volume ratio of the ethyl acetate to the acetone in the mixed solvent in the second step is 2: 1.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention aims to provide a simple and practical production process for extracting and purifying phloretin from apple flowers. Thereby fully utilizing the fallen flowers of the apples and providing a new and safe source mode of the pure natural phloretin. In the invention, the mixed solvent is used for extraction, so that the extraction of polar components is reduced, and the subsequent separation and purification are facilitated.
2. The method extracts, concentrates and crystallizes the apple powder raw material, so that the content of phloretin can reach about 85%, and the content of phloretin can reach more than 98% through decoloring and crystallization.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A production process for extracting and purifying phloretin from apple flowers specifically comprises the following steps:
the method comprises the following steps: feeding 400 kg of apple flower raw material after pretreatment, crushing the apple flower raw material into coarse powder raw material, and bagging for later use;
step two: extracting, namely dynamically extracting the coarse powder raw material twice at normal temperature by using a mixed solvent with the volume ratio of ethyl acetate to acetone being 2:1, wherein the two extraction times are respectively 2 hours and 1.5 hours, and the dosage of the two extraction solvents is respectively the weight of the raw materials: 6 times and 5 times of solvent volume (M: V) to obtain raw material extractive solution;
step three: concentrating, namely concentrating the raw material extracting solution to 120L volume under normal pressure;
step four: and (3) crystallization: crystallizing the concentrated raw material extract at normal temperature, and performing suction filtration to obtain yellow green or off-white powder coarse crystals;
step five: recrystallizing, volatilizing solvent, adding 50L95% ethanol into the powder crude crystal, heating and dissolving to obtain solution, adding 1 kg activated carbon into the solution for decolorization, filtering after 3 hours, and cooling and crystallizing to obtain white powder crystal;
step six: and (5) performing suction filtration and drying, performing suction filtration on the white powder crystals obtained in the step five, and performing crystal drying to obtain 4.5 kg of white crystal powder, wherein the product yield is 1.13%, and the phloretin product with the content of 99.2% is obtained.
Example 2
A production process for extracting and purifying phloretin from apple flowers specifically comprises the following steps:
the method comprises the following steps: feeding 1000 kg of apple flower raw material after pretreatment, crushing the apple flower raw material into coarse powder raw material, and bagging for later use;
step two: extracting, namely dynamically extracting the coarse powder raw material twice at normal temperature by using a mixed solvent with the volume ratio of ethyl acetate to acetone being 3:1, wherein the two extraction times are respectively 2 hours and 1.5 hours, and the dosage of the two extraction solvents is respectively the weight of the raw materials: 6 times and 5 times of solvent volume (M: V) to obtain raw material extractive solution;
step three: concentrating, namely concentrating the raw material extracting solution to 100L volume under normal pressure;
step four: and (3) crystallization: crystallizing the concentrated raw material extract at normal temperature, and performing suction filtration to obtain yellow green or off-white powder coarse crystals;
step five: recrystallizing, volatilizing solvent, adding 50L95% ethanol into the powder crude crystal, heating and dissolving to obtain solution, adding 1 kg activated carbon into the solution for decolorization, filtering after 3 hours, and cooling and crystallizing to obtain white powder crystal;
step six: and (5) performing suction filtration and drying, performing suction filtration on the white powder crystals obtained in the step five, and performing crystal drying to obtain 4.8 kg of white crystal powder, wherein the product yield is 1.2%, and the phloretin content is 98.3%.
The comparison of the content of phloretin extracted and purified in examples 1-2 with the content of phloretin extracted in the existing production process for extracting phloretin from apple flowers shows the following comparison results in table 1:
TABLE 1
And (4) conclusion:
the invention can fully utilize the fallen flowers of the apples and provide a new safe source mode of the pure natural phloretin, and in the invention, the extraction of polar components is reduced by using a mixed solvent for extraction, thereby being beneficial to the subsequent separation and purification;
the method extracts, concentrates and crystallizes the apple powder raw material, so that the content of phloretin can reach about 85%, and the content of phloretin can reach more than 98% through decoloring and crystallization.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A production process for extracting and purifying phloretin from apple flowers is characterized by comprising the following steps: the production process specifically comprises the following steps:
the method comprises the following steps: pretreating raw materials, namely crushing the apple flower raw materials into coarse powder raw materials, and bagging for later use;
step two: extracting, namely dynamically extracting the coarse powder raw material twice by using a mixed solvent at normal temperature to obtain a raw material extracting solution;
step three: concentrating, namely concentrating the raw material extracting solution under normal pressure to reduce the volume and the weight;
step four: and (3) crystallization: crystallizing the concentrated raw material extract at normal temperature, and performing suction filtration to obtain yellow green or off-white powder coarse crystals;
step five: recrystallizing, heating and dissolving the powder crude crystals with ethanol to obtain a solution, adding activated carbon into the solution for decoloring, and cooling and crystallizing to obtain white powder crystals;
step six: and (5) performing suction filtration and drying, performing suction filtration on the white powder crystals obtained in the step five, and performing crystal drying to obtain a phloretin product with the concentration of more than 98%.
2. The production process for extracting and purifying phloretin from apple flowers according to claim 1, wherein the mixed solvent in the second step is prepared from ethyl acetate and acetone, and the volume ratio of the ethyl acetate to the acetone is 1: 1-4: 1.
3. The process of claim 1, wherein the raw material of apple flower is pulverized to a particle size of less than 3 mm.
4. The process for producing phloretin from apple flower according to claim 2, wherein the two dynamic extractions of the coarse powder material with the mixed solvent at room temperature in step two are carried out for 2 hours and 1.5 hours, respectively, and the amounts of the mixed solvent used for the two extractions are the following raw materials by weight: the volume of the mixed solvent (M: V) is 6 times and 5 times.
5. The process for extracting purified phloretin from apple flowers according to claim 1, wherein the concentration degree in the third step is 0.3 to 0.2 times of that of the raw material extract.
6. The process for producing phloretin from apple flower according to claim 1, wherein the concentration of ethanol used in step five is 95%, the amount of ethanol is 8 times of the amount of crude crystals of the powder, and the amount of activated carbon added is 2% of the solution.
7. The production process for extracting and purifying phloretin from apple flowers according to claim 2, wherein the volume ratio of ethyl acetate to acetone in the mixed solvent in the second step is 2: 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110229944.6A CN112811997B (en) | 2021-03-02 | 2021-03-02 | Production process for extracting and purifying phlorizin from apple flowers |
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| CN202110229944.6A CN112811997B (en) | 2021-03-02 | 2021-03-02 | Production process for extracting and purifying phlorizin from apple flowers |
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| CN112811997B CN112811997B (en) | 2024-03-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117447318A (en) * | 2023-10-26 | 2024-01-26 | 南京林业大学 | Deep eutectic solvent for co-production of phloretin and fermented woody protein feed using pruned branches of apple trees and its fermentation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643315A (en) * | 2012-04-17 | 2012-08-22 | 陕西嘉禾植物化工有限责任公司 | Method for purifying phlorizin from apple velamen |
| CN102701938A (en) * | 2012-06-11 | 2012-10-03 | 成都中医药大学 | Method for extracting and purifying phloretin from Malus toringoides(Rehd.) Hughes. and Malus tiansitoria(Batal.)Schneid. |
| CN104292094A (en) * | 2014-09-29 | 2015-01-21 | 桂林莱茵生物科技股份有限公司 | Extracting method of high-purity phloretin |
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- 2021-03-02 CN CN202110229944.6A patent/CN112811997B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643315A (en) * | 2012-04-17 | 2012-08-22 | 陕西嘉禾植物化工有限责任公司 | Method for purifying phlorizin from apple velamen |
| CN102701938A (en) * | 2012-06-11 | 2012-10-03 | 成都中医药大学 | Method for extracting and purifying phloretin from Malus toringoides(Rehd.) Hughes. and Malus tiansitoria(Batal.)Schneid. |
| CN104292094A (en) * | 2014-09-29 | 2015-01-21 | 桂林莱茵生物科技股份有限公司 | Extracting method of high-purity phloretin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117447318A (en) * | 2023-10-26 | 2024-01-26 | 南京林业大学 | Deep eutectic solvent for co-production of phloretin and fermented woody protein feed using pruned branches of apple trees and its fermentation method and application |
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