CN107602638A - The method that phloridzin is prepared using apple branches and leaves, root skin - Google Patents
The method that phloridzin is prepared using apple branches and leaves, root skin Download PDFInfo
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- CN107602638A CN107602638A CN201710889369.6A CN201710889369A CN107602638A CN 107602638 A CN107602638 A CN 107602638A CN 201710889369 A CN201710889369 A CN 201710889369A CN 107602638 A CN107602638 A CN 107602638A
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Abstract
The invention belongs to chemical composition extraction and separation technology field, and in particular to a kind of method that phloridzin is prepared using apple branches and leaves, root skin.This method includes extraction, purifying, condensing crystallizing and the steps such as recrystallization of decolourizing.The method technological process of the invention for utilizing apple branches and leaves, root skin to prepare phloridzin is simple, cost is low, pollution is small, safe and efficient, is adapted to industrialized production.
Description
Technical field
The invention belongs to chemical composition extraction and separation technology field, and in particular to one kind is prepared using apple branches and leaves, root skin
The method of phloridzin.
Background technology
Phloridzin, also known as Phloridzin, 4,6- dihydroxy -2- (6- gluconic acids glycosides) -6- (para hydroxybenzene) propiophenone, its
Molecular formula is C21H24O10, molecular weight 436.41, slightly yellow acicular crystals, hot water, methanol, ethanol, acetone, second can be dissolved in
Acetoacetic ester etc., insoluble in chloroform and benzene.Phloridzin have hypoglycemic, whitening, it is anti-oxidant, enhancing memory, prevention sclerotin it is loose,
The multiple biological activities such as antitumor.Phloridzin has inhibitory action to the unordered hyperplasia of cell, available for cutaneum carcinoma and other tumours
Auxiliary treatment；Phloridzin has significant decompression lipid-lowering effect, is described as natural depressor, while can suppress melanocyte work
Property, there is desalination effect to various skin splash.China's cultivated area of the apple is big, every year due to tree body trimming, orchard seeds more
It is new etc., substantial amounts of apple branches and leaves and tree root are produced, these may serve to extraction and prepare phloridzin, produce huge social benefit
And economic benefit.
At present, the extraction on phloridzin, purification technique mainly have organic solvent extractionprocess, macroporous resin purification method, gathered
Acid amides column chromatography etc., but these methods all there is it is more or less the defects of, production process is cumbersome, loss is big；Using organic
Solvent is excessive, and toxicity is big；Therefore technology of preparing that is safe efficient, being simple to operate and friendly to environment is found curing for phloridzin
Extensive use important in inhibiting in medicine, food industries.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides one kind using apple branches and leaves, root skin
The method for preparing phloridzin.
The present invention technical solution be：A kind of method that phloridzin is prepared using apple branches and leaves, root skin, its it is special it
It is in comprising the following steps：
1) extract：Raw material is obtained after apple branches and leaves and root skin are crushed, the carbon that mass fraction is 1-3% is added into raw material
Acid sodium aqueous solution, the quality of the aqueous sodium carbonate of addition are 6-8 times of material quality；2 are extracted at a temperature of 60-90 DEG C
Secondary, each extraction time is 2 hours；Merge and extract obtained extract solution twice and be cooled to 30-35 DEG C；
2) purify：Using ion exchange resin to after cooling extract solution carry out ion exchange, with deionized water clean to
Efflux is clarified, and the sodium-chloride water solution for being then 5-10% with mass fraction is replaced collection from ion exchange resin and solved
Analyse liquid；
3) condensing crystallizing：It is 1.08-1.1 that desorbed solution is concentrated into proportion, and adjusting pH value to standing after 2-3 with watery hydrochloric acid ties
It is brilliant；Centrifugation, obtain phloridzin crude product after drying；
4) decolourize recrystallization：80-90 DEG C is heated to after adding deionized water and activated carbon into obtained phloridzin crude product,
The quality of the deionized water of addition is 5-8 times of phloridzin crude product quality, and the quality of the activated carbon of addition is phloridzin crude product matter
The 3-5% of amount；Insulated and stirred was filtered and stood still for crystals after 1-1.5 hours, is centrifuged, is dried to obtain phloridzin.
Further, ion exchange resin used in step 2) is 201 × 7 type ion exchange resin.
Further, the quality of the aqueous sodium carbonate added in step 1) into raw material is 7 times of material quality, carbonic acid
The mass fraction of sodium water solution is 2%.
Further, the Extracting temperature extracted twice in step 1) is 75 DEG C, and 32 DEG C are cooled to after merging extract solution.
Further, the mass fraction of the sodium-chloride water solution used in step 2) is 8%.
Further, the proportion for the desorbed solution being concentrated to give in step 3) is 1.09.
Further, the desorbed solution after being concentrated in step 3) adjusts pH value to 2.5 with watery hydrochloric acid.
Further, the quality of the deionized water added in step 4) is 6.5 times of phloridzin crude product quality, the work of addition
Property charcoal quality be phloridzin crude product quality 4%.
Further, the temperature of heating and thermal insulation is 85 DEG C in step 4).
Further, the time of insulated and stirred is 75 minutes in step 4).
The beneficial effects of the present invention are：The present invention prepares the method technological process of phloridzin using apple branches and leaves, root skin
Simply, cost is low, pollution is small, safe and efficient, is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the chemical structural formula of phloridzin.
Embodiment
Embodiment one
The present embodiment is a kind of method that phloridzin is prepared using apple branches and leaves, root skin, is comprised the following steps：
1) extract：Raw material is obtained after apple branches and leaves and root skin are crushed, the carbonic acid that mass fraction is 1% is added into raw material
Sodium water solution, the quality of the aqueous sodium carbonate of addition are 6 times of material quality；Extract 2 times at a temperature of 60 DEG C, carry every time
It is 2 hours to take the time；Merge the extract solution for extracting to obtain twice and be cooled to 30 DEG C using heat exchanger；
2) purify：Ion exchange is carried out to the extract solution after cooling using 201 × 7 type ion exchange resin, uses deionization
Water is cleaned to efflux and clarified, and collection is then replaced from ion exchange resin with the sodium-chloride water solution that mass fraction is 5%
Obtain desorbed solution；
3) condensing crystallizing：Desorbed solution is concentrated into proportion as 1.08, pH value is adjusted to standing still for crystals after 2 with watery hydrochloric acid；From
The heart, obtain phloridzin crude product after drying；
4) decolourize recrystallization：80 DEG C are heated to after adding deionized water and activated carbon into obtained phloridzin crude product, is added
The quality of the deionized water entered is 5 times of phloridzin crude product quality, and the quality of the activated carbon of addition is phloridzin crude product quality
3%；Insulated and stirred was filtered and stood still for crystals after 1 hour, centrifuged, is dried to obtain the phloridzin product of purity more than 95%.
Embodiment two
The present embodiment is a kind of method that phloridzin is prepared using apple branches and leaves, root skin, is comprised the following steps：
1) extract：Raw material is obtained after apple branches and leaves and root skin are crushed, the carbonic acid that mass fraction is 2% is added into raw material
Sodium water solution, the quality of the aqueous sodium carbonate of addition are 7 times of material quality；Extract 2 times at a temperature of 75 DEG C, carry every time
It is 2 hours to take the time；Merge and extract obtained extract solution twice and be cooled to 32 DEG C；
2) purify：Ion exchange is carried out to the extract solution after cooling using 201 × 7 type ion exchange resin, uses deionization
Water is cleaned to efflux and clarified, and collection is then replaced from ion exchange resin with the sodium-chloride water solution that mass fraction is 8%
Obtain desorbed solution；
3) condensing crystallizing：Desorbed solution is concentrated into proportion as 1.09, pH value is adjusted to standing still for crystals after 2.5 with watery hydrochloric acid；
Centrifugation, obtain phloridzin crude product after drying；
4) decolourize recrystallization：85 DEG C are heated to after adding deionized water and activated carbon into obtained phloridzin crude product, is added
The quality of the deionized water entered is 6.5 times of phloridzin crude product quality, and the quality of the activated carbon of addition is phloridzin crude product quality
4%；Insulated and stirred was filtered and stood still for crystals after 75 minutes, centrifuged, is dried to obtain the phloridzin of purity more than 95%.
Embodiment three
The present embodiment is a kind of method that phloridzin is prepared using apple branches and leaves, root skin, is comprised the following steps：
1) extract：Raw material is obtained after apple branches and leaves and root skin are crushed, the carbonic acid that mass fraction is 3% is added into raw material
Sodium water solution, the quality of the aqueous sodium carbonate of addition are 8 times of material quality；Extract 2 times at a temperature of 90 DEG C, carry every time
It is 2 hours to take the time；Merge and extract obtained extract solution twice and be cooled to 35 DEG C；
2) purify：Ion exchange is carried out to the extract solution after cooling using 201 × 7 type ion exchange resin, uses deionization
Water is cleaned to efflux and clarified, and collection is then replaced from ion exchange resin with the sodium-chloride water solution that mass fraction is 10%
Obtain desorbed solution；
3) condensing crystallizing：Desorbed solution is concentrated into proportion as 1.1, pH value is adjusted to standing still for crystals after 3 with watery hydrochloric acid；From
The heart, obtain phloridzin crude product after drying；
4) decolourize recrystallization：90 DEG C are heated to after adding deionized water and activated carbon into obtained phloridzin crude product, is added
The quality of the deionized water entered is 8 times of phloridzin crude product quality, and the quality of the activated carbon of addition is phloridzin crude product quality
5%；Insulated and stirred was filtered and stood still for crystals after 1.5 hours, centrifuged, is dried to obtain the phloridzin of purity more than 95%.
Claims (10)
- A kind of 1. method that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that comprise the following steps：1) extract：Raw material is obtained after apple branches and leaves and root skin are crushed, the sodium carbonate that mass fraction is 1-3% is added into raw material The aqueous solution, the quality of the aqueous sodium carbonate of addition are 6-8 times of material quality；Extract 2 times at a temperature of 60-90 DEG C, often Secondary extraction time is 2 hours；Merge and extract obtained extract solution twice and be cooled to 30-35 DEG C；2) purify：Ion exchange is carried out to the extract solution after cooling using ion exchange resin, cleaned with deionized water to outflow Liquid is clarified, and the sodium-chloride water solution for being then 5-10% with mass fraction is replaced collection from ion exchange resin and parsed Liquid；3) condensing crystallizing：It is 1.08-1.1 that desorbed solution is concentrated into proportion, and pH value is adjusted to standing still for crystals after 2-3 with watery hydrochloric acid； Centrifugation, obtain phloridzin crude product after drying；4) decolourize recrystallization：80-90 DEG C is heated to after deionized water and activated carbon are added into obtained phloridzin crude product, is added The quality of deionized water be 5-8 times of phloridzin crude product quality, the quality of the activated carbon of addition is phloridzin crude product quality 3-5%；Insulated and stirred was filtered and stood still for crystals after 1-1.5 hours, is centrifuged, is dried to obtain phloridzin.
- 2. the method according to claim 1 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 2) In used ion exchange resin be 201 × 7 type ion exchange resin.
- 3. the method according to claim 1 or 2 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 1) quality of the aqueous sodium carbonate added in into raw material is 7 times of material quality, and the mass fraction of aqueous sodium carbonate is 2%.
- 4. the method according to claim 3 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 1) In the Extracting temperature that extracts twice be 75 DEG C, be cooled to 32 DEG C after merging extract solution.
- 5. the method according to claim 1 or 2 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 2) mass fraction of the sodium-chloride water solution used in is 8%.
- 6. the method according to claim 1 or 2 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 3) proportion for the desorbed solution being concentrated to give in is 1.09.
- 7. the method according to claim 6 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 3) Desorbed solution after middle concentration adjusts pH value to 2.5 with watery hydrochloric acid.
- 8. the method according to claim 1 or 2 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 4) quality of the deionized water added in is 6.5 times of phloridzin crude product quality, and the quality of the activated carbon of addition is thick for phloridzin The 4% of quality.
- 9. the method according to claim 8 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 4) The temperature of middle heating and thermal insulation is 85 DEG C.
- 10. the method according to claim 9 that phloridzin is prepared using apple branches and leaves, root skin, it is characterised in that：Step 4) The time of middle insulated and stirred is 75 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710889369.6A CN107602638B (en) | 2017-09-27 | 2017-09-27 | Method for preparing phlorizin by using apple branches, leaves and root barks |
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| CN201710889369.6A CN107602638B (en) | 2017-09-27 | 2017-09-27 | Method for preparing phlorizin by using apple branches, leaves and root barks |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392008A (en) * | 2007-09-18 | 2009-03-25 | 兴化格林生物制品有限公司 | Extraction technique of high-purity phlorizin |
| CN102286037A (en) * | 2011-08-02 | 2011-12-21 | 桂林三宝药业有限公司 | Process for extracting phlorhizin from litchi rind |
| 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 |
| CN103864864A (en) * | 2014-03-27 | 2014-06-18 | 江苏斯威森生物医药工程研究中心有限公司 | Method for efficiently extracting phlorizin from plants |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
-
2017
- 2017-09-27 CN CN201710889369.6A patent/CN107602638B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392008A (en) * | 2007-09-18 | 2009-03-25 | 兴化格林生物制品有限公司 | Extraction technique of high-purity phlorizin |
| CN102286037A (en) * | 2011-08-02 | 2011-12-21 | 桂林三宝药业有限公司 | Process for extracting phlorhizin from litchi rind |
| 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 |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN103864864A (en) * | 2014-03-27 | 2014-06-18 | 江苏斯威森生物医药工程研究中心有限公司 | Method for efficiently extracting phlorizin from plants |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
Non-Patent Citations (1)
| Title |
|---|
| 刘引烽编著: "《特种高分子材料》", 31 December 2001, 上海大学出版社 * |
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