CN107602638B - Method for preparing phlorizin by using apple branches, leaves and root barks - Google Patents
Method for preparing phlorizin by using apple branches, leaves and root barks Download PDFInfo
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- CN107602638B CN107602638B CN201710889369.6A CN201710889369A CN107602638B CN 107602638 B CN107602638 B CN 107602638B CN 201710889369 A CN201710889369 A CN 201710889369A CN 107602638 B CN107602638 B CN 107602638B
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Abstract
The invention belongs to the technical field of extraction and separation of chemical components, and particularly relates to a method for preparing phlorizin by utilizing apple branches, leaves and root barks. The method comprises the steps of extraction, purification, concentration crystallization, decoloration recrystallization and the like. The method for preparing phlorizin by utilizing apple branches, leaves and root barks has the advantages of simple process flow, low cost, small pollution, safety and high efficiency, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of extraction and separation of chemical components, and particularly relates to a method for preparing phlorizin by utilizing apple branches, leaves and root barks.
Background
Phlorizin, also known as Floricin, 4, 6-dihydroxy-2- (6-glucuronide) -6- (p-hydroxyphenyl) propiophenone, has the molecular formula C21H24O10The molecular weight is 436.41, and the product is yellowish needle-shaped crystal, soluble in hot water, methanol, ethanol, acetone, ethyl acetate, etc., and insoluble in chloroform and benzene. Phlorizin has various biological activities of reducing blood sugar, whitening skin, resisting oxidation, enhancing memory, preventing osteoporosis, resisting tumor and the like. Phlorizin has inhibitory effect on disordered cell proliferation, and can be used for adjuvant treatment of skin cancer and other tumors; phlorizin has obvious functions of reducing blood pressure and blood fat, is known as a natural antihypertensive drug, can inhibit activity of melanocytes and has a function of fading various skin color spots. The apple planting area in China is large, a large amount of apple branches and leaves and tree roots are generated every year due to tree pruning, orchard tree species updating and the like, and the apple branches and leaves and the tree roots can be used for extracting and preparing phlorizin, so that huge social benefits and economic benefits are generated.
At present, extraction and purification technologies of phlorizin mainly comprise an organic solvent extraction method, a macroporous resin purification method, a polyamide column chromatography method and the like, but the methods have more or less defects, and the production process is complicated and the loss is large; the use of excessive organic solvents has high toxicity; therefore, the search for safe, efficient, simple to operate and environment-friendly preparation technology has important significance for the wide application of phlorizin in the medicine and food industries.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for preparing phlorizin by using apple branches, leaves and root barks.
The technical solution of the invention is as follows: a method for preparing phlorizin by utilizing apple branches, leaves and root barks is characterized by comprising the following steps:
1) extraction: crushing branches, leaves and root barks of apples to obtain raw materials, adding a sodium carbonate aqueous solution with the mass fraction of 1-3% into the raw materials, wherein the mass of the added sodium carbonate aqueous solution is 6-8 times of that of the raw materials; extracting at 60-90 deg.C for 2 times, each for 2 hr; mixing the extractive solutions, and cooling to 30-35 deg.C;
2) and (3) purification: performing ion exchange on the cooled extracting solution by using ion exchange resin, washing the extracting solution by using deionized water until effluent is clear, and then replacing and collecting the effluent from the ion exchange resin by using a sodium chloride aqueous solution with the mass fraction of 5-10% to obtain an analytic solution;
3) concentration and crystallization: concentrating the desorption solution until the specific gravity is 1.08-1.1, adjusting the pH value to 2-3 by using dilute hydrochloric acid, and standing for crystallization; centrifuging and drying to obtain crude phlorizin;
4) decoloring and recrystallizing: adding deionized water and active carbon into the obtained crude phlorizin product, heating to 80-90 ℃, wherein the mass of the added deionized water is 5-8 times of that of the crude phlorizin product, and the mass of the added active carbon is 3-5% of that of the crude phlorizin product; stirring for 1-1.5 hr, filtering, standing for crystallization, centrifuging, and drying to obtain phlorizin.
Further, the ion exchange resin used in step 2) is a 201 × 7 type ion exchange resin.
Further, the mass of the sodium carbonate aqueous solution added to the raw material in the step 1) is 7 times of the mass of the raw material, and the mass fraction of the sodium carbonate aqueous solution is 2%.
Further, the extraction temperature of the two times of extraction in the step 1) is 75 ℃, and the temperature is reduced to 32 ℃ after the extracting solutions are combined.
Further, the mass fraction of the sodium chloride aqueous solution used in step 2) was 8%.
Further, the specific gravity of the analysis liquid obtained by concentration in step 3) was 1.09.
Further, the pH value of the desorption solution concentrated in the step 3) is adjusted to 2.5 by using dilute hydrochloric acid.
Further, the mass of the deionized water added in the step 4) is 6.5 times of the mass of the crude phlorizin product, and the mass of the added active carbon is 4% of the mass of the crude phlorizin product.
Further, the temperature of the heating and heat preservation in the step 4) is 85 ℃.
Further, the time for keeping warm and stirring in the step 4) is 75 minutes.
The invention has the beneficial effects that: the method for preparing phlorizin by utilizing apple branches, leaves and root barks has the advantages of simple process flow, low cost, small pollution, safety and high efficiency, and is suitable for industrial production.
Drawings
FIG. 1 shows the chemical structure of phlorizin.
Detailed Description
Example one
The embodiment is a method for preparing phlorizin by utilizing apple branches, leaves and root barks, which comprises the following steps:
1) extraction: crushing branches, leaves and root barks of apples to obtain raw materials, adding a sodium carbonate aqueous solution with the mass fraction of 1% into the raw materials, wherein the mass of the added sodium carbonate aqueous solution is 6 times of that of the raw materials; extracting at 60 deg.C for 2 times, each time for 2 hr; mixing the extractive solutions obtained by two times, and cooling to 30 deg.C with heat exchanger;
2) and (3) purification: performing ion exchange on the cooled extracting solution by using 201 x 7 type ion exchange resin, washing the extracting solution by using deionized water until effluent liquid is clear, and then replacing and collecting sodium chloride aqueous solution with the mass fraction of 5% from the ion exchange resin to obtain analysis solution;
3) concentration and crystallization: concentrating the desorption solution until the specific gravity is 1.08, adjusting the pH value to 2 by using dilute hydrochloric acid, and standing for crystallization; centrifuging and drying to obtain crude phlorizin;
4) decoloring and recrystallizing: adding deionized water and activated carbon into the obtained crude phlorizin product, heating to 80 ℃, wherein the mass of the added deionized water is 5 times of that of the crude phlorizin product, and the mass of the added activated carbon is 3 percent of that of the crude phlorizin product; stirring for 1 hr, filtering, standing for crystallization, centrifuging, and drying to obtain phlorizin product with purity over 95%.
Example two
The embodiment is a method for preparing phlorizin by utilizing apple branches, leaves and root barks, which comprises the following steps:
1) extraction: crushing branches, leaves and root barks of apples to obtain raw materials, adding a sodium carbonate aqueous solution with the mass fraction of 2% into the raw materials, wherein the mass of the added sodium carbonate aqueous solution is 7 times of that of the raw materials; extracting at 75 deg.C for 2 times, each for 2 hr; mixing the extractive solutions obtained by two times, and cooling to 32 deg.C;
2) and (3) purification: performing ion exchange on the cooled extracting solution by using 201 x 7 type ion exchange resin, washing the extracting solution by using deionized water until effluent liquid is clear, and then replacing and collecting sodium chloride aqueous solution with the mass fraction of 8% from the ion exchange resin to obtain analysis solution;
3) concentration and crystallization: concentrating the desorption solution until the specific gravity is 1.09, adjusting the pH value to 2.5 by using dilute hydrochloric acid, and standing for crystallization; centrifuging and drying to obtain crude phlorizin;
4) decoloring and recrystallizing: adding deionized water and activated carbon into the obtained crude phlorizin product, heating to 85 ℃, wherein the mass of the added deionized water is 6.5 times of that of the crude phlorizin product, and the mass of the added activated carbon is 4% of that of the crude phlorizin product; stirring for 75 min, filtering, standing for crystallization, centrifuging, and drying to obtain phlorizin with purity over 95%.
EXAMPLE III
The embodiment is a method for preparing phlorizin by utilizing apple branches, leaves and root barks, which comprises the following steps:
1) extraction: crushing branches, leaves and root barks of apples to obtain raw materials, adding a sodium carbonate aqueous solution with the mass fraction of 3% into the raw materials, wherein the mass of the added sodium carbonate aqueous solution is 8 times of that of the raw materials; extracting at 90 deg.C for 2 times, each for 2 hr; mixing the extractive solutions obtained by two times, and cooling to 35 deg.C;
2) and (3) purification: performing ion exchange on the cooled extracting solution by using 201 x 7 type ion exchange resin, washing the extracting solution by using deionized water until effluent liquid is clear, and then replacing and collecting sodium chloride aqueous solution with the mass fraction of 10% from the ion exchange resin to obtain analysis solution;
3) concentration and crystallization: concentrating the desorption solution until the specific gravity is 1.1, adjusting the pH value to 3 by using dilute hydrochloric acid, and standing for crystallization; centrifuging and drying to obtain crude phlorizin;
4) decoloring and recrystallizing: adding deionized water and activated carbon into the obtained crude phlorizin product, heating to 90 ℃, wherein the mass of the added deionized water is 8 times of that of the crude phlorizin product, and the mass of the added activated carbon is 5% of that of the crude phlorizin product; stirring for 1.5 hr, filtering, standing for crystallization, centrifuging, and drying to obtain phlorizin with purity over 95%.
Claims (8)
1. A method for preparing phlorizin by utilizing apple branches, leaves and root barks is characterized by comprising the following steps:
1) extraction: crushing branches, leaves and root barks of apples to obtain raw materials, adding a sodium carbonate aqueous solution with the mass fraction of 1-3% into the raw materials, wherein the mass of the added sodium carbonate aqueous solution is 6-8 times of that of the raw materials; extracting at 75 deg.C for 2 times, each for 2 hr; mixing the extractive solutions obtained by two times, and cooling to 32 deg.C;
2) and (3) purification: performing ion exchange on the cooled extracting solution by using ion exchange resin, washing the extracting solution by using deionized water until effluent is clear, and then replacing and collecting the effluent from the ion exchange resin by using a sodium chloride aqueous solution with the mass fraction of 5-10% to obtain an analytic solution; the ion exchange resin is 201 multiplied by 7 type ion exchange resin;
3) concentration and crystallization: concentrating the desorption solution until the specific gravity is 1.08-1.1, adjusting the pH value to 2-3 by using dilute hydrochloric acid, and standing for crystallization; centrifuging and drying to obtain crude phlorizin;
4) decoloring and recrystallizing: adding deionized water and active carbon into the obtained crude phlorizin product, heating to 80-90 ℃, wherein the mass of the added deionized water is 5-8 times of that of the crude phlorizin product, and the mass of the added active carbon is 3-5% of that of the crude phlorizin product; stirring for 1-1.5 hr, filtering, standing for crystallization, centrifuging, and drying to obtain phlorizin.
2. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 1, wherein: the mass of the sodium carbonate aqueous solution added into the raw materials in the step 1) is 7 times of that of the raw materials, and the mass fraction of the sodium carbonate aqueous solution is 2%.
3. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 1, wherein: the mass fraction of the sodium chloride aqueous solution used in step 2) was 8%.
4. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 1, wherein: the specific gravity of the analysis liquid obtained by concentration in the step 3) was 1.09.
5. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 4, wherein: adjusting the pH value of the concentrated analysis solution in the step 3) to 2.5 by using dilute hydrochloric acid.
6. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 1, wherein: the mass of the deionized water added in the step 4) is 6.5 times of the mass of the crude phlorizin product, and the mass of the added active carbon is 4 percent of the mass of the crude phlorizin product.
7. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 6, wherein: the temperature for heating and heat preservation in the step 4) is 85 ℃.
8. The method for preparing phlorizin by using apple branches, leaves and root barks as claimed in claim 7, wherein: the time for keeping warm and stirring in the step 4) is 75 minutes.
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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 |
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