CN112336665B - Sambucus williamsii extract and preparation method thereof - Google Patents
Sambucus williamsii extract and preparation method thereof Download PDFInfo
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- CN112336665B CN112336665B CN202011443883.5A CN202011443883A CN112336665B CN 112336665 B CN112336665 B CN 112336665B CN 202011443883 A CN202011443883 A CN 202011443883A CN 112336665 B CN112336665 B CN 112336665B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention discloses an elderberry extract and a preparation method thereof, wherein the preparation method comprises the following steps: (1) extracting: weighing elderberry raw materials, pulping, crushing, adding water, adjusting the pH of the solution to 3, and stirring and extracting at 45 ℃ for 3 times; (2) filtering: filtering with filter cloth, and collecting filtrate; (3) resin adsorption: adsorbing the filtrate with DM21 resin; (4) impurity washing: washing impurities with 2BV water until the liquid is colorless; and (5) desorption: desorbing with 55% ethanol; (6) concentrating: concentrating the desorption solution under reduced pressure to obtain a Baume degree of 20; and (7) drying: and (4) carrying out spray drying on the concentrated solution to obtain a finished product. The invention adopts the process of extracting by using the acidic softened water, and the extract is directly subjected to column-loading desorption after being filtered, thereby greatly improving the production efficiency and ensuring the process safety and no risk; in addition, the DM21 resin is adopted, so that the content of anthocyanin in the extract (more than or equal to 36 percent) can be effectively improved.
Description
Technical Field
The invention relates to the technical field of plant extraction, and particularly relates to an elderberry extract and a preparation method thereof.
Background
The elderberry extract is extracted from stems and branches of Sambucus williamsii Hance of Caprifoliaceae, contains phenolic acid, triterpene aglycone and other active ingredients, has pharmacological activities of resisting osteoporosis, promoting fracture healing, resisting inflammation, resisting virus, resisting oxidation, improving immunity and the like, is widely applied to cosmetics, has the effects of moistening skin and beautifying, has the functions of sterilizing, diminishing inflammation and relieving itching of elderberry glycoside, mucus and other ingredients, and can be used in daily products for washing hair and caring hair.
The prior extraction process of elderberry is a methanol extraction method: pulping fresh ramulus Sambuci Williamsii, crushing, leaching with 10BV 70% methanol twice, filtering with 200 mesh filter cloth, mixing extractive solutions, concentrating to Be 20 without alcohol smell, diluting with water, purifying with chromatography column LSA-10, and drying with high concentration ethanol.
The process for leaching elderberry by methanol has the defects of long time consumption, high energy consumption, high solvent cost, certain harm to human bodies in the using process of the solvent and the like. In addition, the LSA-10 resin used in the traditional process has general enrichment capacity on anthocyanin, the recycling frequency is low, and the phase change improves the production cost.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides an elderberry extract and a preparation method thereof. The invention improves the use of solvent in the traditional process, saves energy consumption and reduces potential safety hazard in production; the invention improves the process method, adopts the process of extracting by using the acidic softened water, directly carries out column-loading desorption after the extracting solution is filtered, greatly improves the production efficiency, and simultaneously ensures the process safety without risk; in addition, the DM21 resin is adopted, so that the content of anthocyanin in the extract (not less than 36%) can be effectively improved, and the number of recycling times is greatly increased.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of an elderberry extract comprises the following steps:
(1) Extraction: weighing elderberry raw materials, pulping, crushing, adding 10 times of water, adjusting the pH of the solution to 3, stirring and extracting for 3 times in a 45 ℃ water bath kettle, and each time for 2 hours;
(2) And (3) filtering: filtering with filter cloth, collecting filtrate, and squeezing the filtrate;
(3) Resin adsorption: adsorbing the filtrate obtained in the step (2) by using DM21 resin, wherein the adsorption flow rate is 2BV/h;
(4) Impurity washing: washing impurities with 2BV of water until the liquid is colorless;
(5) Desorbing 55 percent ethanol at the desorption flow rate of 1BV/h, and collecting the desorption solution at 1.5BV;
(6) And (3) concentrating: concentrating the desorption solution obtained in the step (5) under reduced pressure to obtain Baume degree of 20;
(7) And (3) drying: and (4) carrying out spray drying on the concentrated solution obtained in the step (6) to obtain a finished product.
Preferably, in the step (1), the pH of the solution is adjusted to 3 by using a 4% HCl solution.
Preferably, in the step (2), the mesh number of the filter cloth is 200 meshes.
Preferably, in the step (6), the concentration under reduced pressure is carried out under conditions of-0.07 to-0.1MPa and 40 to 60 ℃.
Preferably, in the step (7), the inlet temperature of the spray drying is 185-200 ℃, and the outlet temperature is 85-100 ℃.
An elderberry extract is prepared by the preparation method.
In the technical scheme, when fresh fruits are treated, pulping and crushing are needed, which is beneficial to full extraction, but the fresh fruits cannot be beaten to be too thin, and the net is easy to block during filtration.
In the technical scheme, the pH value of the acidic softened water in the extraction process needs to be controlled to be about 3, the extraction is insufficient when the pH value is higher than 3, the use amount of acid is increased when the pH value is lower than 3, and the cost is increased.
In the technical scheme, from the aspect of improving the content, the DM21 resin with stronger adsorption and purification capacity is selected after comparison, the outflow speed cannot be too fast during adsorption, otherwise, the material is easy to run out, and the desorption speed is not fast until no color flows out during impurity washing; in addition, the resin needs to be maintained regularly and can be treated by adopting an acid-base soaking method.
In the technical scheme, the percentage is the mass percentage.
Compared with the prior art, the invention has the beneficial effects that:
the traditional elderberry mostly adopts a methanol extraction process, so that the problems of multiple steps, high solvent cost and safety risk in the use of a solvent exist; in addition, the content of anthocyanin in the product prepared by the traditional process is low and is mostly between 20 and 25 percent; compared with the prior art, the production process has the advantages of low cost and simple extraction process steps; the method reduces the use risk of the solvent and effectively improves the content of the product anthocyanin at the same time.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
Example 1
A preparation method of an elderberry extract comprises the following steps:
(1) Extraction: weighing 1000g ramulus Sambuci Williamsii raw material, pulping, crushing, adding 10BV water, adjusting pH to 3 with 4% HCl, extracting under stirring for 2 hr at 45 deg.C for 3 times;
(2) And (3) filtering: filtering with 200 mesh filter cloth, collecting filtrate, and squeezing the filtrate for the last time;
(3) Resin adsorption: adsorbing the extracting solution obtained in the step (2) by using DM21 resin, wherein the adsorption flow rate is 2BV/h;
(4) Impurity washing: washing impurities with 2BV of water until the liquid is colorless;
(5) Desorbing: desorbing with 55% ethanol at a desorption flow rate of 1BV/h, and collecting a desorption solution at 1.5BV;
(6) And (3) concentrating: concentrating the desorption solution obtained in the step (5) under-0.080 Mpa at 50 ℃ under reduced pressure to obtain Baume degree 20;
(7) And (3) drying: spray drying the concentrated solution obtained in the step (6) at the inlet temperature of 185 ℃ and the outlet temperature of 85 ℃;
(8) And (3) detection: collecting the product, and inspecting, wherein the anthocyanin content is 36%.
Comparative example 1
A preparation method of an elderberry extract comprises the following steps:
(1) Extraction: weighing 1000g of ramulus Sambuci Williamsii raw material, pulping, crushing, adding 6BV of water, adjusting pH to 5 with 4% HCl, stirring and extracting for 3 times at 60 deg.C for 2 hr each time;
(2) And (3) filtering: filtering with 200 mesh filter cloth, collecting filtrate, and squeezing the filtrate;
(3) Resin adsorption: adsorbing the extract obtained in step (2) with LSA-10 resin at an adsorption flow rate of 2BV/h;
(4) Impurity washing: washing impurities with 2BV of water until the liquid is colorless;
(5) Desorbing: desorbing with 55% ethanol at a desorption flow rate of 2BV/h, and collecting a desorption solution at 1.5BV;
(6) Concentration: concentrating the desorption solution obtained in the step (5) under-0.080 Mpa at 50 ℃ under reduced pressure to obtain Baume degree 20;
(7) And (3) drying: spray drying the concentrated solution obtained in the step (6) at an inlet temperature of 185 ℃ and an outlet temperature of 85 ℃;
(8) And (3) detection: collecting the product, and inspecting, wherein the content of anthocyanin is 25%.
Comparative example 2
A preparation method of an elderberry extract comprises the following steps:
(1) Extraction: weighing 1000g of ramulus Sambuci Williamsii raw material, pulping, crushing, adding 8BV of water, adjusting pH to 4 with 4% HCl, stirring and extracting for 3 times at 55 deg.C for 2 hr each time;
(2) And (3) filtering: filtering with 200 mesh filter cloth, collecting filtrate, and squeezing the filtrate;
(3) Resin adsorption: adsorbing the extracting solution obtained in the step (2) by using DM21 resin, wherein the adsorption flow rate is 2BV/h;
(4) Impurity washing: washing impurities with 2BV of water until the liquid is colorless;
(5) Desorbing: desorbing with 55% ethanol at a desorption flow rate of 1.5BV/h, and collecting a desorption solution at a rate of 1.5BV;
(6) Concentration: concentrating the desorption solution obtained in the step (5) under-0.080 Mpa at 50 ℃ under reduced pressure to obtain Baume degree 20;
(7) And (3) drying: spray drying the concentrated solution obtained in the step (6) at the inlet temperature of 185 ℃ and the outlet temperature of 85 ℃;
(8) And (3) detection: collecting the product, and inspecting, wherein the content of anthocyanin is 30%.
The determination method of the anthocyanin content comprises the following steps:
1 chromatographic conditions:
1.1 column: gemini-C18,4.6 x 250mm
1.2 detection wavelength 535nm
1.3 detector: VWD
1.4 column temperature: 30 deg.C
1.5 flow rate: 1.0ml/min
1.6 mobile phase: phase A: formic acid-water solution (8.5; phase B: acetonitrile-methanol-formic acid-water solution (22.5.
2 preparation of control solutions:
a standard USP Cyanidin-3-O-glucoside chloride RS is precisely weighed to be about 15mg (accurate to be 0.01 mg), placed in a 50mL volumetric flask, added with 2% hydrochloric acid-methanol solution (V/V) and diluted to the mark, and shaken up. Accurately, 5mL of the above solution was transferred into a 25mL volumetric flask and the volume was determined by 10% phosphoric acid aqueous solution (V/V). The concentration of Cyanidin-3-O-glucoside chloride in the prepared standard solution is 0.05mg/mL.
3, preparation of a test solution:
about 125mg (to the nearest 0.01 mg) of the sample was weighed out, and the volume was determined by 2% hydrochloric acid-methanol solution (V/V) in a 25mL volumetric flask, and 5mL of the above solution was transferred to a 25mL volumetric flask and the volume was determined by 10% phosphoric acid aqueous solution (V/V). Filtering with 0.45 μm microporous membrane to obtain test solution.
4, determination method:
precisely transferring 20 μ l of each of the reference solution and the sample solution, and measuring with liquid chromatograph.
Calculated as peak area by external standard method.
5 calculation of
A Sample (II) : the peak area of the test sample;
W sign : weighing (g) a reference substance;
V sample (A) : dilution times (ml) of the test sample;
A sign board : peak area of control;
W sample (A) : weighing (g) a sample;
V sign : control dilution (ml).
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (2)
1. The preparation method of the elderberry extract is characterized by comprising the following steps:
(1) Extraction: weighing elderberry raw materials, pulping, crushing, adding 10 times of water, adjusting the pH of the solution to 3, stirring and extracting at 45 ℃ for 3 times, and each time for 2 hours;
(2) And (3) filtering: filtering with filter cloth, and collecting filtrate;
(3) Resin adsorption: adsorbing the filtrate obtained in the step (2) by using DM21 resin, wherein the adsorption flow rate is 2BV/h;
(4) Impurity washing: washing impurities with 2BV of water until the liquid is colorless;
(5) Desorption: desorbing with 55% ethanol at a desorption flow rate of 1BV/h, and collecting a desorption solution at 1.5BV;
(6) Concentration: concentrating the desorption solution obtained in the step (5) under reduced pressure to obtain Baume degree of 20;
(7) And (3) drying: spray drying the concentrated solution obtained in the step (6) to obtain a finished product;
in the step (1), adjusting the pH value of the solution to 3 by using a 4% HCl solution;
in the step (2), the mesh number of the filter cloth is 200 meshes;
in the step (6), the reduced pressure concentration condition is-0.07 to-0.1MPa and 40 to 60 ℃;
in the step (7), the inlet temperature during spray drying is 185-200 ℃, and the outlet temperature is 85-100 ℃.
2. An elder extract characterized by being prepared by the method for preparing an elder extract according to claim 1.
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| CN101463027B (en) * | 2009-01-08 | 2012-05-02 | 陕西明锐天然产物有限责任公司 | Method for extracting and separating flavone and anthocyanidin from elder fruit |
| CN102119950B (en) * | 2011-02-23 | 2013-01-02 | 匡海学 | Compound elder composition for treating bone injury and preparation method and pharmaceutical application thereof |
| CN110433190B (en) * | 2019-08-28 | 2020-12-08 | 汤臣倍健股份有限公司 | Method for separating and extracting effective components from cowberry |
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