CN114605427A - Method for extracting and preparing raspberry ellagic acid - Google Patents
Method for extracting and preparing raspberry ellagic acid Download PDFInfo
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- 235000011034 Rubus glaucus Nutrition 0.000 title claims abstract description 81
- 235000009122 Rubus idaeus Nutrition 0.000 title claims abstract description 81
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 title claims abstract description 79
- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 title claims abstract description 79
- 229920002079 Ellagic acid Polymers 0.000 title claims abstract description 79
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- 238000000034 method Methods 0.000 title claims abstract description 30
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- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/06—Peri-condensed systems
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Abstract
The invention provides a method for extracting and preparing raspberry ellagic acid. The extraction reagent is mainly sodium bicarbonate aqueous solution, so that the use of an organic reagent is avoided, and the problems of sample residue and environmental pollution of the organic reagent are reduced. The extraction process adopts a sodium bicarbonate aqueous solution extraction method, improves the extraction efficiency through heating treatment, and achieves the optimal extraction efficiency by optimizing the concentration of the sodium bicarbonate aqueous solution, the solid-liquid extraction proportion, the extraction temperature and the extraction time. The ellagic acid extracted by the method has good biological activity such as oxidation resistance and the like, and is a good production material for nutritional health products. The extraction process is simple, efficient and less in pollution, and is a raspberry ellagic acid extraction method with industrial advantages.
Description
Technical Field
The invention relates to an ellagic acid extraction technology, in particular to a method for extracting and preparing raspberry ellagic acid.
Background
The raspberry is perennial deciduous shrub type fruit tree of Rubus of Rosaceae, also named raspberry and raspberry, etc. The raspberry is rich in ellagic acid, raspberry ketone, salicylic acid, etc. Wherein ellagic acid has effects of protecting and repairing DNA, resisting oxidation, diminishing inflammation, resisting mutation, and resisting cancer. The content of ellagic acid in raspberry seeds is rich, and raspberry residues after wine making or juice squeezing contain more raspberry seeds, so that the ellagic acid extracting and preparing material is good. The material cost can be saved by extracting the ellagic acid from the raspberry vinasse or the juicing residue. However, the traditional extraction method generally uses organic reagents such as acetone, methanol, ethanol, acetic acid and the like, and the use of the organic reagents has the problems of high cost and easy environmental pollution.
An extraction method with low cost and less pollution is urgently needed while the extraction effect is ensured.
Disclosure of Invention
The invention aims to provide a method for extracting and preparing raspberry ellagic acid aiming at the problems of high cost and environmental pollution of the existing organic reagent for extracting ellagic acid.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for extracting and preparing raspberry ellagic acid comprises the following steps:
step (1), drying or baking the raspberry wine and/or the raspberry juicing residue to obtain dry raspberry residue rich in raspberry seeds;
step (2) preparing NaHCO30.1-3% aqueous solution, mixing the raspberry residue of step (1) with NaHCO3Mixing the water solutions according to the mass-volume ratio of 1:3-1:100, grinding the mixed solution for 3-20min by using a colloid mill, and stopping grinding when seeds are thoroughly crushed in the colloid mill to form a solid-liquid mixed slurry solution;
step (3) transferring all the slurry solution in the step (2) into a heating container, heating and leaching for 10min-5h at a constant temperature of 60-100 ℃, and then cooling to room temperature;
and (4) performing solid-liquid separation on the solution obtained in the step (3) by a centrifugal or sedimentation and filtration method, and recovering a clear liquid part to obtain the ellagic acid solution.
Further, the raspberry residue and NaHCO in step (2)3The aqueous solutions are mixed according to the mass-volume ratio of 1:5-1: 80.
Further, NaHCO in step (2)3The concentration of the aqueous solution is 0.5-1.5% wt, raspberry residue and NaHCO3The mixing ratio of the aqueous solution is 1:5-1: 50. The grinding time is 4-6 min.
Further, the step (3) is carried out for 20min-2h at the constant temperature of 70-95 ℃.
Further, the ellagic acid solution is concentrated by drying under reduced pressure or freeze drying to obtain ellagic acid solid extract.
The invention also discloses raspberry ellagic acid prepared by the method.
The invention also discloses an ellagic acid health-care beverage which comprises the raspberry ellagic acid.
The invention also discloses an ellagic acid medicament comprising the raspberry ellagic acid.
The basic principle of the extraction of the raspberry ellagic acid of the invention is that the raspberry ellagic acid is contained in a series of components of vegetable fat, polysaccharide and protein, NaHCO3The aqueous solution is heated to facilitate NaHCO3And saponifying with fat component to dissolve the fat component in water and release ellagic acid component wrapped therein, and heating for alkaline hydrolysis of raspberry tannin to generate more ellagic acid molecules.
As shown in FIG. 1, A is raspberry lees residue component for ellagic acid extraction, containing raspberry seeds. Panel B is NaHCO at 40 deg.C3Extracting the resulting raspberry solution. FIG. C is NaHCO at 100 deg.C3Extracting the resulting raspberry solution. In the diagram B, the upper, middle and lower three layers are water phase, emulsifying layer and solid phase layer, and the middle emulsifying layer is raspberry fatty acid without thorough saponification. In panel C, there are two layers, with little yellow intermediate layer, and the emulsion layer has essentially disappeared, indicating that the fatty acid saponification reaction is essentially complete and has dissolved in the aqueous environment due to NaHCO at 100 deg.C3Heating to promote fat component and NaHCO3Saponification occurs to produce sodium fatty acid, thereby dissolving the fat component in the aqueous environment and releasing the ellagic acid contained therein.
FIG. 2 is an analytically pure standard sample of raspberry ellagic acid, quantified by liquid chromatography. FIG. 3 shows the residue of raspberry wine brewing by NaHCO3Heating the aqueous solution at 100 deg.C for 20min to obtain liquid chromatogram of ellagic acid solution. The liquid chromatography retention time of the ellagic acid standard was 12.94min, and the retention time of the main peak in the extract coincided with this time, it was confirmed that the main component in the extract was ellagic acid, and further, the ellagic acid in the extract was quantified based on the integrated areas of the standard and the extract.
The invention discloses a method for extracting and preparing raspberry ellagic acid, and particularly relates to a method for extracting and preparing the ellagic acid from raspberry wine making or juicing residues by using sodium bicarbonate as an extraction reagent and a water-phase heating method as a main extraction means, which has the following advantages compared with the prior art:
1) the extraction method has the advantages of simple and convenient operation, safety, health, low cost, high efficiency and the like, does not use organic reagents, and has little environmental pollution
2) The purity and extraction efficiency of the extract are high, the purity of the ellagic acid can reach more than 85%, and the extraction rate of the ellagic acid can reach 6.30 +/-0.92 mg/g (calculated on the dry basis of raspberry residues). In terms of extraction efficiency, it corresponds to the extraction rate of raspberry ellagic acid of 2.66 ± 0.35mg/g if methanol/acetone/water (7: 7: 6) is used as the leaching agent, and the extraction rate of raspberry ellagic acid of 1.98 ± 0.12mg/g if acetone/acetic acid/water (70: 1: 29) is used as the leaching agent.
3) The obtained ellagic acid is rich in raspberry fruit flavor, has sour taste, and good antioxidant activity, and can be used for producing ellagic acid health beverage or medicament, and the reduction activity of ellagic acid extract is 79.0 + -0.96 μmol Trolox eq/g by DPPH method. Correspondingly, if methanol/acetone/water (7: 7: 6) is used as the leaching agent, the reducing activity of the obtained raspberry ellagic acid is 59.7 + -3.02 μmol Trolox eq/g, and if acetone/acetic acid/water (70: 1: 29) is used as the leaching agent, the reducing activity of the obtained raspberry ellagic acid is 24.1 + -0.06 μmol Trolox eq/g.
Drawings
FIG. 1 is NaHCO3Demonstration of the acceleration of saponification reactions to hydrolysis of fatty acids in the accompanying drawing, where A is the raspberry lees residue fraction used for ellagic acid extraction and B is NaHCO at 40 deg.C3Extracting with a raspberry solution C NaHCO at 100 deg.C3Extracting the resulting raspberry solution;
FIG. 2 is a liquid chromatography spectrum of an analytically pure standard sample of raspberry ellagic acid;
FIG. 3 shows the residue of raspberry wine making after grinding in NaHCO3Liquid chromatography of ellagic acid solution obtained by heat-treating in water solution at 100 deg.C for 20 min.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The embodiment discloses a method for extracting and preparing raspberry ellagic acid, which uses sodium bicarbonate as an extraction reagent and a water phase heating method as a main extraction means, and comprises the following specific steps:
and (1) drying or baking the raspberry wine making residue in the sun to obtain dry raspberry residue rich in raspberry seeds.
Step (2) preparing NaHCO30.1% aqueous solution, mixing the raspberry residue of step (1) with NaHCO3Mixing the water solutions according to the mass-volume ratio of 1:3, grinding the mixed solution for 3min by using a colloid mill, and stopping grinding when seeds are thoroughly ground in the colloid mill to form a solid-liquid mixed slurry solution.
And (3) transferring the slurry solution in the step (2) into a heating container, heating and leaching for 10min at a constant temperature of 60 ℃, and then cooling to room temperature.
And (4) performing solid-liquid separation on the solution obtained in the step (3) by a centrifugal or sedimentation and filtration method, and recovering a clear liquid part to obtain the ellagic acid solution. The ellagic acid component can be quantified by liquid chromatography. The ellagic acid solution can be concentrated or a solid ellagic acid extract can be obtained by drying under reduced pressure or freeze drying.
The method can obtain ellagic acid with extraction rate of 0.59mg/g (based on raspberry residue dry basis).
Example 2
The embodiment discloses a method for extracting and preparing raspberry ellagic acid, which uses sodium bicarbonate as an extraction reagent and a water phase heating method as a main extraction means, and comprises the following specific steps:
drying or baking the raspberry wine making or juicing residue in the sun to obtain dry raspberry residue rich in raspberry seeds.
Step (2) preparing NaHCO31% aqueous solution of Raspberry residue and NaHCO in step (1)3Mixing the water solutions according to the mass-volume ratio of 1:10, grinding the mixed solution for 5min by using a colloid mill, and stopping grinding when seeds are thoroughly ground in the colloid mill to form a solid-liquid mixed slurry solution.
And (3) transferring the slurry solution in the step (2) into a heating container, heating and leaching for 30min at a constant temperature of 80 ℃, and then cooling to room temperature.
And (4) performing solid-liquid separation on the solution obtained in the step (3) by a method of centrifugation or sedimentation plus filtration, and recovering a clear liquid part to obtain the ellagic acid solution. The ellagic acid component can be quantified by liquid chromatography. The ellagic acid solution can be concentrated or a solid ellagic acid extract can be obtained by drying under reduced pressure or freeze drying.
The method can obtain ellagic acid with extraction rate of 4.2mg/g (based on raspberry residue dry basis).
Example 3
The embodiment discloses a method for extracting and preparing raspberry ellagic acid, which uses sodium bicarbonate as an extraction reagent and a water phase heating method as a main extraction means, and comprises the following specific steps:
drying or baking the raspberry wine making or juicing residue in the sun to obtain dry raspberry residue rich in raspberry seeds.
Step (2) preparing NaHCO33% aqueous solution of raspberry residue and NaHCO of the step (1)3Mixing the water solutions according to the mass-volume ratio of 1:100, grinding the mixed solution for 20min by using a colloid mill, and stopping grinding when seeds are thoroughly ground in the colloid mill to form a solid-liquid mixed slurry solution.
Step (3) transferring the slurry solution in the step (2) into a heating container, heating and leaching for 5h at constant temperature under the condition of 100 ℃, and then cooling to room temperature.
And (4) performing solid-liquid separation on the solution obtained in the step (3) by a centrifugal or sedimentation and filtration method, and recovering a clear liquid part to obtain the ellagic acid solution. The ellagic acid component can be quantified by liquid chromatography. The ellagic acid solution can be concentrated or the ellagic acid solid extract can be obtained by drying under reduced pressure or freeze drying.
The method can obtain ellagic acid with extraction rate of 5.3mg/g (based on raspberry residue dry basis).
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for extracting and preparing raspberry ellagic acid is characterized by comprising the following steps:
sun-drying or oven-drying raspberry wine and/or raspberry juicing residue to obtain dry raspberry residue rich in raspberry seeds;
step (2) preparing NaHCO30.1-3% aqueous solution, mixing the raspberry residue of step (1) with NaHCO3Mixing the water solutions according to the mass-volume ratio of 1:3-1:100, grinding the mixed solution for 3-20min by using a colloid mill, and stopping grinding when seeds are thoroughly crushed in the colloid mill to form a solid-liquid mixed slurry solution;
step (3) transferring all the slurry solution in the step (2) into a heating container, heating and leaching for 10min-5h at a constant temperature of 60-100 ℃, and then cooling to room temperature;
and (4) performing solid-liquid separation on the solution obtained in the step (3) by a method of centrifugation or sedimentation plus filtration, and recovering a clear liquid part to obtain the ellagic acid solution.
2. The method for extracting and preparing raspberry ellagic acid according to claim 1, wherein in step (2), the raspberry residue is mixed with NaHCO3The aqueous solutions are mixed according to the mass-volume ratio of 1:5-1: 80.
3. The method for extracting and preparing raspberry ellagic acid according to claim 1, wherein NaHCO is used in step (2)3The concentration of the aqueous solution is 0.5-1.5% wt, raspberry residue and NaHCO3The mixing ratio of the aqueous solution is 1:5-1:50, and the grinding time is 4-6 min.
4. The method for extracting and preparing raspberry ellagic acid according to claim 1, wherein the leaching in step (3) is performed at a constant temperature of 70-95 ℃ for 20min-2 h.
5. The method for preparing the raspberry ellagic acid according to claim 1, wherein the ellagic acid solution is concentrated by a method of drying under reduced pressure or freeze drying to obtain an ellagic acid solid extract.
6. Raspberry ellagic acid prepared by the method of any one of claims 1 to 5.
7. An ellagic acid health drink comprising the raspberry ellagic acid of claim 6.
8. An ellagic acid agent comprising the raspberry ellagic acid of claim 6.
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| CN202210298015.5A CN114605427A (en) | 2022-03-25 | 2022-03-25 | Method for extracting and preparing raspberry ellagic acid |
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| CN202210298015.5A CN114605427A (en) | 2022-03-25 | 2022-03-25 | Method for extracting and preparing raspberry ellagic acid |
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| CN115785114A (en) * | 2022-12-02 | 2023-03-14 | 浙江理工大学 | Method for extracting ellagic acid |
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