CN113512082B - Method for extracting phlorizin and phloretin in apple root bark and application thereof - Google Patents
Method for extracting phlorizin and phloretin in apple root bark and application thereof Download PDFInfo
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Abstract
The invention discloses a method for extracting phlorizin and phloretin from apple root bark and application thereof, wherein the method comprises the following steps: extracting apple root bark with boiling water after ethanol elution, cooling the obtained extract, adding a flocculating agent, carrying out solid-liquid separation after reaction, and extracting phlorizin and phloretin from the filtrate and the filter residue respectively. The invention selects the apple root bark as a raw material, adopts an internal boiling method, firstly permeates into the material through a small amount of desorption solvent, and then adds a large amount of hot solvent to ensure that the desorption solvent boils and vaporizes to generate internal convection so as to strengthen the diffusion of effective components; a vacuum freeze drying method is adopted to form a spongy porous structure, so that many heat-sensitive substances are not denatured or inactivated, the growth of microorganisms and the action of enzymes cannot be carried out, and the original properties can be maintained; the vacuum freeze drying and the internal boiling method are combined, so that the effective components are fully diffused, and the extraction rate is obviously improved.
Description
Technical Field
The invention belongs to the technical field of extraction of plant active ingredients, and particularly relates to a method for extracting phlorizin and phloretin from apple root bark and application of the method.
Background
Phlorizin belongs to polyphenol substances and is dihydrochalcone glycoside in plant flavonoids in the polyphenol substances; phlorizin is mainly present in the root bark, stem, tender leaves of apple trees and apple fruits, has various biological activities such as regulating blood pressure and blood sugar, protecting heart, scavenging free radicals in vivo, whitening and the like, and also has the characteristic of low toxicity.
Phloretin is dihydrochalcone compound, is a natural active substance existing in fruits such as apples and pears and various vegetables, has been used as a natural skin whitening agent, can inhibit tyrosinase activity and melanin activity, whitens skin and has a fading effect on various skin stains. According to the latest research, the compound also has the effects of resisting inflammation, suppressing immunity, protecting cardiovascular and the like, and has potential great market demand.
At present, the preparation methods of phlorizin and phloretin researched at home and abroad generally comprise an organic solvent extraction method, a microwave-assisted extraction method, a hot water extraction method and the like.
Wherein: ethanol is mostly used in the organic solvent extraction method, the method can reduce the leaching of water-soluble impurities in materials to a higher degree and reduce the cost of later separation and purification, but the method consumes more ethanol and takes longer time, and if the temperature is raised, more dissolved impurities are easily caused, although the solvent extraction method only uses relatively safe solvents such as ethanol, ethyl acetate and the like in the extraction process, the selectivity is poor, the purity of the extract is low, and the effect can be achieved by extracting for many times; in the microwave-assisted extraction method, different substances with different microwave absorbing capacities are utilized to selectively heat part of components in a solution, so that a target product to be extracted can be dissolved out of a matrix and dissolved in a solvent with low solubility, but at present, microwave equipment and technology need to be improved, and phlorizin has poor thermal stability and is difficult to apply; the hot water extraction method has low cost, simple equipment, safety and no toxicity, but the phlorizin has lower solubility in water, more extracted impurities and low yield, thereby causing difficulty in the subsequent purification steps.
The unique functional value of phlorizin determines that phlorizin will play an important role in the fields of food and medicine, so that the search for a safe, efficient and environment-friendly phlorizin extraction technology is very necessary for the wide application of phlorizin in the medicine and food industries.
In the prior art, only a method for preparing single high-purity phlorizin by using apples or extracts thereof or a method for preparing single phloretin does not have a preparation method for simultaneously obtaining two high-purity components, so that waste and loss of the other component are caused while one component is prepared, and great resource waste is caused during industrial mass production.
Disclosure of Invention
In view of the above, the invention provides a method for extracting phlorizin and phloretin from apple root bark and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for extracting phlorizin and phloretin from apple root bark comprises the following steps:
extracting apple root bark with boiling water after ethanol elution, cooling the obtained extract, adding a flocculating agent, carrying out solid-liquid separation after reaction, and extracting phlorizin and phloretin from the filtrate and the filter residue respectively.
In the above technical scheme, the method for extracting phlorizin and phloretin from apple root bark further comprises drying the apple root bark until the water content is lower than 15 wt% before ethanol resolution.
Further, in the above technical solution, the drying is vacuum freeze drying.
Preferably, in the above technical solution, the drying is to dry the apple root bark to a moisture content of 5-12 wt%.
Still further, in the above technical scheme, in the resolving process, the concentration of the ethanol is 30-60 wt%, the material-liquid ratio is 1: 5-8, the resolving temperature is 0-40 ℃, and the resolving time is 10-20 min.
Further, in the technical scheme, in the extraction process, the material-liquid ratio is 1: 15-20, the extraction temperature is 82-100 ℃, and the extraction time is 1-2 h.
Still further, in the above technical scheme, the flocculant is polyacrylamide, and the addition amount thereof is 0.5-2% of the mass of the apple root bark.
Still further, in the above technical scheme, the solid-liquid separation is centrifugation at 2000-5000rpm for 5-15 min.
Still further, in the above technical solution, the process of extracting phloretin includes:
and drying the filter residue, dissolving the filter residue by using an organic solvent, purifying by using a purification resin, concentrating and drying, cooling and crystallizing, and recrystallizing by using an ethanol water solution to obtain the phloretin.
In a preferred embodiment of the present invention, the organic solvent is 70 to 80 wt% ethanol aqueous solution.
In a preferred embodiment of the present invention, the effective component of the purified resin is one or more of attapulgite, hydrotalcite, bentonite and perlite.
In a preferred embodiment of the present invention, the concentration of the ethanol aqueous solution is 15 to 30 wt% during the recrystallization.
Still further, in the above technical solution, the process of extracting phlorizin includes:
subjecting the filtrate to resin adsorption chromatography, eluting impurities with water and an alcohol aqueous solution with the concentration lower than 40 wt%, and then resolving with an alcohol aqueous solution with the concentration higher than 50 wt% to obtain a phlorizin resolving solution; concentrating the phlorizin analytic solution, pouring into a distillation still, heating and recovering residual alcohols to obtain a phlorizin concentrated solution; adding active carbon into the phlorizin concentrated solution for decolorization, filtering while hot, then standing at 0-4 ℃ for crystallization and precipitation, and drying to obtain phlorizin.
In one embodiment of the invention, the method for extracting phlorizin and phloretin from apple root bark further comprises filtering the filtrate through a ceramic membrane with the pore diameter of 100-800nm before the filtrate is subjected to resin adsorption chromatography.
In a preferred embodiment of the invention, the resin for adsorption chromatography is one or more of AB-8, HPD-400, ADS-7 and D-101.
In a preferred embodiment of the present invention, the elution impurities are, specifically, eluted with water at a pH of 3 to 5 at a flow rate of 1 to 2BV and an aqueous ethanol solution at a flow rate of 10 to 40 wt% at a flow rate of 1 to 3 BV.
In a preferred embodiment of the present invention, in the resolving step, the alcohol aqueous solution is a 50 to 80 wt% ethanol aqueous solution.
In a preferred embodiment of the invention, the concentration is normal pressure filtration through a polyethersulfone composite nanofiltration membrane, the heating temperature in the distillation kettle is 70-80 ℃, and the concentration of the phlorizin concentrated solution is 25-35 wt%.
In a preferred embodiment of the invention, the adding amount of the activated carbon is 0.01-0.03 times of the mass of the phlorizin concentrated solution, and the temperature and the time for decoloring are 60-70 ℃ and 30-60min respectively.
The invention also provides application of the method in extracting phlorizin and phloretin in apple root bark.
Compared with the prior art, the invention has the following advantages:
(1) according to the method for extracting phlorizin and phloretin in apple root bark, the apple root bark with rich resources and high phlorizin content is selected as a raw material, an internal boiling method is adopted, a small amount of desorption solvent is firstly permeated into the material, and a large amount of hot solvent is added to ensure that the desorption solvent is boiled and vaporized, so that internal convection is generated, and the diffusion of effective components is enhanced;
(2) the method for extracting phlorizin and phloretin in the apple root bark adopts a vacuum freeze drying method, water vapor is left in an ice shelf during freezing after being directly sublimated out to form a spongy porous framework, a plurality of heat-sensitive substances cannot be denatured or inactivated, some volatile components in the substances are slightly lost, and the growth of microorganisms and the action of enzymes cannot be carried out during the freeze drying process, so that the original properties can be maintained;
(3) according to the method for extracting phlorizin and phloretin in apple root bark, provided by the invention, vacuum freeze drying and an internal boiling method are combined, a loose porous structure similar to a spongy structure is formed, and then the porous structure is fully permeated by ethanol, so that effective components are fully diffused by a large amount of hot solvent, and the extraction rate is obviously improved;
(4) the method for extracting phlorizin and phloretin in apple root bark provided by the invention comprises the steps of dissolving low-content phloretin in an ethanol water solution, dissolving impurities with strong water solubility and large polarity by using the low-concentration ethanol water solution, removing the impurities, eluting by using a high-concentration ethanol water solution to remove compounds with small polarity in a chromatographic column, concentrating to remove the impurities, recovering ethanol, and dissolving phloretin by using the ethanol water solution, so that high-purity phloretin is extracted, and impurities containing impurity colors are removed from the extracted phloretin.
Drawings
FIG. 1 is a process flow diagram of a method for extracting phlorizin and phloretin from apple root bark in the embodiment of the invention;
FIG. 2 is an HPLC chart of phlorizin extracted in example 1 of the present invention;
FIG. 3 is an HPLC chart of phloretin extracted in example 1 of the present invention;
FIG. 4 is an HPLC chart of phlorizin extracted in example 2 of the present invention;
FIG. 5 is an HPLC chart of phloretin extracted in example 2 of the present invention;
FIG. 6 is an HPLC chart of phlorizin extracted in example 3 of the present invention;
FIG. 7 is an HPLC chart of phloretin extracted in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments.
It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In the examples, the means used are conventional in the art unless otherwise specified.
The terms "comprises," "comprising," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The apple root bark used in the examples of the present invention is a commercially available product.
Example 1
The embodiment of the invention provides a method for extracting phlorizin and phloretin from apple root bark, which specifically comprises the following steps:
(1) drying and extracting: carrying out vacuum freeze drying treatment on 1kg of apple root bark until the water content is less than or equal to 15%, carrying out freeze drying, desorbing the apple root bark with 30% ethanol at a feed-liquid ratio of 1: 5 for 10min, then rapidly adding 1: 15 boiling water for extraction at the extraction temperature of 82-100 ℃ for 1 h;
(2) and (3) purification: cooling the extractive solution, adding 0.5% flocculant (polyacrylamide), centrifuging to obtain clarified centrifugate, and filtering with ceramic membrane (600 nm).
(3) Separating phloretin: drying the centrifugal precipitate, dissolving with ethanol, purifying with resin, concentrating, drying, cooling with 20% ethanol, crystallizing, and recrystallizing to obtain phloretin.
(4) Adsorption and desorption: adsorbing the filtrate with resin, eluting with 1BV of water and 30% ethanol to remove impurities, and eluting with 2BV of 50% ethanol at a flow rate of 2BV/h to obtain phlorizin eluate.
(5) Concentration: and carrying out nanofiltration and concentration on the phlorizin analytic solution to obtain a phlorizin concentrated solution.
(6) And (3) distillation: pouring the phlorizin concentrated solution into a distillation kettle, heating, and recovering residual ethanol after nanofiltration to obtain the phlorizin concentrated solution with the solid content of 25%.
(7) And (3) decoloring: adding 1% active carbon, decolorizing for 30min at 60 deg.C.
(8) And (3) crystallization: the decolored solution is placed at 0-4 ℃ to separate out crystals, and the phlorizin finished product is obtained after drying.
Example 2
The embodiment of the invention provides a method for extracting phlorizin and phloretin from apple root bark, which specifically comprises the following steps:
(1) drying and extracting: carrying out vacuum freeze drying treatment on 1kg of apple root bark until the water content is less than or equal to 15%, carrying out freeze drying, desorbing the apple root bark with 30% ethanol at a feed-liquid ratio of 1: 5 for 10min, then rapidly adding 1: 15 boiling water for extraction at the extraction temperature of 82-100 ℃ for 1 h.
(2) And (3) purification: cooling the extractive solution, adding 0.5% flocculant (polyacrylamide), centrifuging to obtain clarified centrifugate, and filtering with ceramic membrane (600 nm).
(3) Separating phloretin: drying the centrifugal precipitate, dissolving with ethanol, purifying with resin, concentrating, drying, cooling with 20% ethanol, crystallizing, and recrystallizing to obtain phloretin.
(4) Adsorption and desorption: adsorbing the filtrate with resin, eluting with 1BV of water and 30% ethanol to remove impurities, and eluting with 2BV of 50% ethanol at a flow rate of 2BV/h to obtain phlorizin eluate.
(5) And (3) concentrating: and carrying out nanofiltration and concentration on the phlorizin analytic solution to obtain a phlorizin concentrated solution.
(6) And (3) distillation: pouring the phlorizin concentrated solution into a distillation kettle, heating, and recovering residual ethanol after nanofiltration to obtain the phlorizin concentrated solution with the solid content of 25%.
(7) And (3) decoloring: adding 3% active carbon, decolorizing for 30min at 70 deg.C.
(8) And (3) crystallization: the decolored solution is placed at 0-4 ℃ to separate out crystals, and the phlorizin finished product is obtained after drying.
Example 3
The embodiment of the invention provides a method for extracting phlorizin and phloretin from apple root bark, which specifically comprises the following steps:
(1) drying and extracting: carrying out vacuum freeze drying treatment on 2kg of apple root bark, drying until the water content is less than or equal to 15%, freeze drying, desorbing the apple root bark by using 30% ethanol at a feed-liquid ratio of 1: 8 for 20min, then rapidly adding 1: 20 boiling water for extraction, wherein the extraction temperature is 82-100 ℃, and the extraction time is 1 h.
(2) And (3) purification: cooling the extractive solution, adding 0.5% flocculant (polyacrylamide), centrifuging to obtain clarified centrifugate, and filtering with ceramic membrane (600 nm).
(3) Separating phloretin: drying the centrifugal precipitate, dissolving with ethanol, purifying with resin, concentrating, drying, cooling with 20% ethanol for crystallization, and recrystallizing to obtain phloretin.
(4) Adsorption and desorption: adsorbing the filtrate with resin, eluting with 1BV of water and 30% ethanol to remove impurities, and eluting with 2BV of 60% ethanol at a flow rate of 2BV/h to obtain phlorizin eluate.
(5) Concentration: and carrying out nanofiltration and concentration on the phlorizin analytic solution to obtain a phlorizin concentrated solution.
(6) And (3) distillation: pouring the phlorizin concentrated solution into a distillation still, heating, recovering ethanol remained after nanofiltration, and obtaining the phlorizin concentrated solution with the solid content of 35 percent.
(7) And (3) decoloring: adding 2% active carbon, decolorizing for 30min at 60 deg.C.
(8) And (3) crystallization: the decolored solution is placed at 0-4 ℃ to separate out crystals, and the phlorizin finished product is obtained after drying.
Example 4
The embodiment of the invention provides a method for extracting phlorizin and phloretin from apple root bark, which specifically comprises the following steps:
(1) drying and extracting: carrying out vacuum freeze drying treatment on 2kg of apple root bark, drying until the water content is less than or equal to 15%, freeze drying, desorbing the apple root bark by using 40% ethanol at a feed-liquid ratio of 1: 8 for 20min, then rapidly adding 1: 20 boiling water for extraction, wherein the extraction temperature is 82-100 ℃, and the extraction time is 2 h.
(2) And (3) purification: cooling the extractive solution, adding 0.5% flocculant (polyacrylamide), centrifuging to obtain clarified centrifugate, and filtering with ceramic membrane (600 nm).
(3) Separating phloretin: drying the centrifugal precipitate, dissolving with ethanol, purifying with resin, concentrating, drying, cooling with 20% ethanol for crystallization, and recrystallizing to obtain phloretin.
(4) Adsorption and desorption: adsorbing the filtrate with resin, eluting with 1BV of water and 30% ethanol to remove impurities, and eluting with 2BV of 60% ethanol at a flow rate of 2BV/h to obtain phlorizin eluate.
(5) Concentration: and carrying out nanofiltration and concentration on the phlorizin analytic solution to obtain a phlorizin concentrated solution.
(6) And (3) distillation: pouring the phlorizin concentrated solution into a distillation still, heating, recovering ethanol remained after nanofiltration, and obtaining the phlorizin concentrated solution with the solid content of 35 percent.
(7) And (3) decoloring: adding 1% active carbon, decolorizing for 40min at 60 deg.C.
(8) And (3) crystallization: the decolored solution is placed at 0-4 ℃ to separate out crystals, and the phlorizin finished product is obtained after drying.
Comparative example 1
The comparative example of the present invention provides a method for extracting phlorizin and phloretin from apple root bark, which has steps and process parameters similar to those of example 1, except that in the drying extraction process of step (1), 30% ethanol is not added for desorption before extraction with boiling water, and the subsequent steps and parameters are all consistent with those of example 1.
Comparative example 2
The invention provides a method for extracting phlorizin and phloretin from apple root bark, which has the steps and process parameters similar to those of example 1, and is only different in that the traditional microwave-assisted extraction method is adopted in the extraction process of the step (1), namely 30% ethanol is added according to the ratio of material to liquid of 1: 5, the extraction is carried out for 1 hour under the assistance of 500W of microwave, and the subsequent steps and parameters are all consistent with those of example 1.
The purity of the prepared phlorizin and phloretin was determined by High Performance Liquid Chromatography (HPLC), the chromatographic column was a Phe-nomenex Gemini C18 column (250 mm. times.4.6 mm, 5 μm), the detection wavelength was 280nm, the mobile phase was acetonitrile-water (0.1% phosphoric acid), the gradient elution (elution conditions are shown in Table 1 below) was performed at a flow rate of 1.0 mL/min.
Table 1 mobile phase gradient elution table (%)
FIGS. 2 to 3 are HPLC charts of phlorizin and phloretin, respectively, extracted in example 1 of the present invention; FIGS. 4 to 5 are HPLC charts of phlorizin and phloretin, respectively, extracted in example 2 of the present invention; FIGS. 6 to 7 are HPLC charts of phlorizin and phloretin, respectively, extracted in example 3 of the present invention.
Meanwhile, the extracted products were weighed, and the purity and extraction rate of phloretin and phlorizin of examples 1 to 4 and comparative examples 1 to 2 were statistically calculated, with the results shown in table 2 below.
TABLE 2 product purity and extraction statistics
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention.
It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A method for extracting phlorizin and phloretin in apple root bark is characterized in that,
the method comprises the following steps:
drying the apple root and peel by vacuum freeze drying until the water content is 5-15 wt%;
and (3) resolving the dried apple root and peel by using ethanol, wherein in the resolving process, the concentration of the ethanol is 30-60 wt%, and the material-liquid ratio is 1: 5-8, the resolving temperature is 0-40 ℃, and the resolving time is 10-20 min;
immediately adding boiling water into the analyzed apple root bark for extraction, cooling the obtained extracting solution, adding a flocculating agent, carrying out solid-liquid separation after reaction, respectively extracting phlorizin and phloretin from filtrate and filter residue, wherein the flocculating agent is polyacrylamide, the adding amount of the flocculating agent is 0.5-2% of the mass of the apple root bark, and the solid-liquid separation is carried out for 5-15min at 2000-5000 rpm;
drying the filter residue, dissolving the filter residue by using an organic solvent, purifying by using a purification resin, concentrating, drying, cooling, crystallizing, and recrystallizing by using an ethanol water solution to obtain phloretin; the organic solvent is 70-80 wt% of ethanol water solution, the effective component of the purified resin is one or more of attapulgite, hydrotalcite, bentonite and perlite, and the concentration of the ethanol water solution is 15-30 wt% in the recrystallization process;
performing resin adsorption chromatography on the filtrate, eluting impurities by using water and an alcohol aqueous solution with the concentration of less than 40 wt%, and then analyzing by using an alcohol aqueous solution with the concentration of more than 50 wt% to obtain a phlorizin analytical solution; concentrating the phlorizin analytic solution, pouring into a distillation still, heating and recovering residual alcohols to obtain a phlorizin concentrated solution; adding active carbon into the phlorizin concentrated solution for decoloring, filtering while hot, then standing at 0-4 ℃ for crystallization and separation, and drying to obtain phlorizin; filtering the filtrate by a ceramic membrane with the aperture of 100-800nm before the filtrate is subjected to resin adsorption chromatography.
2. The method of claim 1, wherein the phlorizin and phloretin in the apple root bark are extracted from the apple root bark,
in the boiling water extraction process, the ratio of material to liquid is 1: 15-20 deg.C, extraction temperature of 82-100 deg.C, and extraction time of 1-2 h.
3. The method of claim 2, wherein the phlorizin and phloretin in the apple root bark are extracted from the apple root bark,
the resin for adsorption chromatography is one or more of AB-8, HPD-400, ADS-7 and D-101.
4. The method for extracting phlorizin and phloretin from apple root bark as claimed in claim 3,
specifically, the impurities are eluted by washing with water of pH 3-5 and flow rate 1-2BV and ethanol aqueous solution of 10-40 wt% and flow rate 1-3 BV.
5. The method of claim 4, wherein the phlorizin and phloretin in the apple root bark are extracted from the apple root bark,
the alcohol aqueous solution with the concentration higher than 50 wt% is an ethanol aqueous solution with the concentration of 50-80 wt%.
6. The method of claim 5, wherein the phlorizin and phloretin in the apple root bark are extracted from the apple root bark,
concentrating, and filtering with polyethersulfone composite nanofiltration membrane at normal pressure, wherein the heating temperature in the distillation still is 70-80 deg.C, and the concentration of the phlorizin concentrated solution is 25-35 wt%.
7. The method for extracting phlorizin and phloretin from apple root bark as claimed in claim 6,
the addition amount of active carbon is 0.01-0.03 times of the phlorizin concentrated solution, and the decoloring temperature and time are 60-70 ℃ and 30-60min respectively.
8. Use of the method of any one of claims 1 to 7 for extracting phlorizin and phloretin from apple root bark.
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| CN102701938B (en) * | 2012-06-11 | 2014-04-23 | 成都中医药大学 | Method for extracting and purifying phloretin from Malus toringoides(Rehd.) Hughes. and Malus tiansitoria(Batal.)Schneid. |
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| 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 |
| CN107383113A (en) * | 2017-06-30 | 2017-11-24 | 湖州知维技术服务有限公司 | A kind of preparation method of coproduction apple polyphenol |
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