CN114031587B - Method for extracting dihydromyricetin from vine tea - Google Patents
Method for extracting dihydromyricetin from vine tea Download PDFInfo
- Publication number
- CN114031587B CN114031587B CN202111403173.4A CN202111403173A CN114031587B CN 114031587 B CN114031587 B CN 114031587B CN 202111403173 A CN202111403173 A CN 202111403173A CN 114031587 B CN114031587 B CN 114031587B
- Authority
- CN
- China
- Prior art keywords
- dihydromyricetin
- extraction
- des
- vine tea
- hydrogen bond
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/32—2,3-Dihydro derivatives, e.g. flavanones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
Abstract
The invention discloses a method for extracting dihydromyricetin from vine tea, which specifically comprises the following steps: 1) Eutectic bonding of the hydrogen bond acceptor and the hydrogen bond donor to obtain DES, and standing overnight; 2) Preparing DES and water into an extraction solvent, uniformly mixing vine tea powder and the extraction solvent, and carrying out shake extraction to obtain an extract of dihydromyricetin; 3) Loading the extract of dihydromyricetin onto macroporous resin, sequentially eluting with distilled water, 80% ethanol and 95% ethanol, collecting 80% ethanol eluate A, and concentrating the eluate A to obtain concentrate B, which is dihydromyricetin monomer component. The invention can simply and efficiently obtain the dihydromyricetin compound from vine tea, has high yield of extracted dihydromyricetin which is 10-20% higher than that of the traditional organic solvent, has the advantages of simple and safe extraction procedure, high extraction efficiency, short analysis time and no byproduct in the extraction process, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of natural product extraction and separation, and particularly relates to a method for obtaining dihydromyricetin from vine tea by utilizing a deep eutectic solvent combined macroporous resin chromatographic column technology.
Background
Ampelopsis grossedentata is Ampelopsis wild wood deciduous vine Ampelopsis Ampelopsis grossedentata (Hand-Mazz) W.T. native to mountain areas in Jiangnan province of China, and has been approved as a new resource food raw material by the third party in 2013 as a drinking history of tea beverage in hundreds of years in the folk. Recent researches show that the vine tea is rich in flavonoid functional active ingredients, including dihydromyricetin, myricetin and the like, wherein the content of the dihydromyricetin in the vine tea can be up to 30-40%; it has various biological activities such as anti-tumor, anti-inflammatory, antiviral, and anti-Alzheimer's disease. Therefore, the development of the extraction method of the dihydromyricetin in the vine tea has great practical value.
The traditional extraction method of dihydromyricetin mainly comprises an organic solvent extraction method, an alkaline extraction method, an enzyme extraction method and a water extraction method, wherein the organic solvent extraction is most commonly used at present, however, the organic solvent has a plurality of defects such as environmental protection, flammability, limitation of the use of certain foods and the like. Therefore, an attempt to replace the organic solvent with a novel green solvent to extract dihydromyricetin from vine tea is a problem to be solved.
Deep eutectic solvents (Deep Eutectic Solvents, DES), which were first proposed in 2001, mix two solid materials with higher melting points and heat them for a period of time to synthesize a homogeneous mixed solution, and find that the physical state changes from solid to liquid, and the melting point of the mixture is far lower than that of the two solid compositions used for synthesis. It also has the remarkable advantages of low toxicity and difficult volatilization as a novel solvent. The invention patent of Chinese patent application No. 201610209945.3 discloses a method for extracting anthocyanin by using deep eutectic solvent with hydrogen bond acceptor as quaternary ammonium salt, wherein the molar ratio of the quaternary ammonium salt to the hydrogen donor is 1:5. The invention patent of China patent application No. 202010351893.X discloses a method for extracting total flavonoids of moringa oleifera by deep eutectic solvent, wherein a hydrogen bond acceptor is choline chloride, and a donor is glycerol, urea and lactic acid. Although there are many reports on deep eutectic solvents applied to extraction of natural active substances, the extraction and preparation of dihydromyricetin with abundant content in vine tea are not reported at present.
In addition, the macroporous adsorption resin is a material commonly used for separating natural products, and has the advantages of good adsorption selection, low cost, simple and convenient operation and the like. The invention patent of Chinese patent application No. CN201811393143.8 discloses a method for adsorbing and separating dihydromyricetin from vine tea water extract by using macroporous resin. In chinese patent application No. cn200710026288.X, a method for extracting dihydromyricetin from hovenia dulcis thunb is disclosed. Therefore, the macroporous resin has feasibility in enriching dihydromyricetin after DES extraction and recovering DES.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to design a technical scheme of a method for extracting high-purity dihydromyricetin from vine tea by using DES and macroporous resin. The method comprises the steps of optimizing the optimized deep eutectic solvent and the extraction condition to obtain the dihydromyricetin efficiently; then, macroporous resin is adopted for adsorption separation, and the high-purity dihydromyricetin is separated from the dihydromyricetin extract. The method fully exerts the characteristics of DES and macroporous resin, and can effectively obtain dihydromyricetin.
The invention is realized by the following technical scheme:
the method for extracting dihydromyricetin from vine tea is characterized by comprising the following steps of:
1) Preparation of DES: eutectic bonding of the hydrogen bond acceptor and the hydrogen bond donor to obtain DES, and standing overnight;
2) DES extraction: preparing an extraction solvent from the DES obtained in the step 1) and water, uniformly mixing vine tea powder and the extraction solvent, and performing shake extraction to obtain an extraction solution of dihydromyricetin;
3) And (3) macroporous resin adsorption separation: loading the extract of dihydromyricetin obtained in the step 2) on macroporous resin, eluting with distilled water, 80% ethanol and 95% ethanol in sequence, collecting 80% ethanol eluate A, and concentrating the eluate A to obtain concentrate B, which is dihydromyricetin monomer component.
Further, the hydrogen bond acceptor in the step 1) is tetrabutylammonium bromide; the hydrogen bond donor is pyruvic acid; the molar ratio of tetrabutylammonium bromide to pyruvic acid is 1:2.
Further, the conditions of the eutectic processing in the step 1) are as follows: shaking at 200rpm in a shaker at 80℃for 3-4 hours.
Further, the DES and water in the step 2) are prepared into an extraction solvent with the volume concentration of 60-80%.
Further, the particle size of the vine tea powder in the step 2) is smaller than 1mm, and the water content of the vine tea powder is 10% -12%.
Further, the ratio of vine tea powder to extraction solvent in the step 2) is 10-40g/mL.
Further, the oscillation extraction conditions in the step 2) are as follows: shaking in a shaking table at 35-55deg.C and rotation speed of 150-230rpm for 2-3 hr.
Further, the macroporous adsorbent resin in the step 3) is AB-8, DM301 or XAD-7HP.
Further, the macroporous resin adsorption separation conditions in the step 3) are as follows: the solid-liquid ratio is 1-2g/mL, the initial loading concentration is 25-100 mu g/mL, and the adsorption temperature is 20-30 ℃.
The invention can simply and efficiently obtain the dihydromyricetin compound from vine tea, and the extraction yield of the dihydromyricetin is high and is 10-20% higher than that of the traditional organic solvent. The extraction method provided by the invention utilizes DES which is a mixed salt solution formed by combining two or more cheap and safe compounds through hydrogen bonding interaction. The DES has larger polarity, physical and chemical properties close to those of the ionic liquid, but is cheaper, safer and easier to prepare than the ionic liquid, and has simple extraction procedure, high extraction efficiency and short analysis time. Compared with the traditional organic solvent, the DES has the advantages of low raw material cost, good biocompatibility, difficult volatilization, simple process operation and no byproduct in the extraction process, and fully reflects the characteristics of green chemistry. And secondly, the macroporous resin adopted in the invention can be repeatedly utilized for at least 6 times, and the operation process is simple and convenient, is suitable for small-scale or industrialized application, and has good application prospect.
Drawings
FIG. 1 is an HPLC profile of ampelopsin control;
FIG. 2 is an HPLC diagram of a Deep Eutectic Solvent (DES) extracted vine tea sample;
FIG. 3 shows the effect of Deep Eutectic Solvent (DES) water content (a), liquid-to-material ratio (b), extraction temperature (c) and extraction time (d) on ampelopsis grossedentata dihydromyricetin extraction yield;
FIG. 4 is a graph showing the effect of response surface optimization interactions on the efficiency of dihydromyricetin extraction from Ampelopsis grossedentata;
FIG. 5 shows the recovery rate of dihydromyricetin by different macroporous resins;
FIG. 6 is a graph showing the effect of DM301 macroporous resin on the adsorption rate of dihydromyricetin in the feed-to-liquid ratio (a), the initial concentration of the upper sample (b) and the adsorption temperature (c);
FIG. 7 is an HPLC chart of a DES extraction sample recovered by DM301 macroporous resin in example 3.
Detailed Description
The invention is further illustrated below in conjunction with specific examples.
The HPLC conditions for analyzing dihydromyricetin in the vine tea extract solution adopted in the embodiment are as follows: octadecylsilane chemically bonded silica (C18) column (Shimadzu WondaCract ODS-2.6mm.times.250mm, 5 μm) is used as filler, and methanol-0.1% formic acid (30:70) is used as mobile phase; the detection wavelength was 292nm. The flow rate was 1.0 mL/min, the column temperature was 35℃and the sample injection amount was 10. Mu.l. The HPLC detection spectrum of the dihydromyricetin standard substance is shown in figure 1.
Example 1: selection of DES and selection of DES extraction conditions
(1) Preparing deep eutectic solvent: the hydrogen bond acceptor and the hydrogen bond donor are uniformly mixed according to a certain molar ratio, the specific adopted molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is shown in table 1, the mixture is put into a sealed glass bottle, and the mixture is vibrated for 3 hours in a shaking table at 200rpm and 80 ℃ to obtain pure and uniform liquid, and then the pure and uniform liquid is stood at 30 ℃ overnight. In this example, 32 deep eutectic solvent trials were prepared.
(2) Deep eutectic solvent extraction: preparing the solution obtained in the step (1) and water into an extraction solvent A with the volume ratio of 30%, uniformly mixing vine tea powder and the extraction solvent A according to the feed liquid ratio of 1:20g/mL, vibrating for 2 hours in a shaking table with the rotating speed of 200rpm at the temperature of 45 ℃ to obtain an extraction solution of the dihydromyricetin, and detecting the yield of the dihydromyricetin in the extraction solution through a liquid phase; the yield of the dihydromyricetin obtained by extracting 32 DES extraction solvents is shown in table 1, and the DES extraction efficiency obtained by taking tetrabutylammonium bromide as a hydrogen bond acceptor is found to be higher, wherein the No. 12 tetrabutylammonium bromide is used: the highest yield of pyruvic acid (1:2) is 388.481 (mg/g vine tea dry weight), and the HPLC detection chart is shown in figure 2. Thus, DES No. 12 was chosen as the extractant in the present invention.
TABLE 1 different DES compositions and extraction rates of dihydromyricetin
(a) Selection of Deep Eutectic Solvent (DES) moisture content
According to the extraction conditions described above, other experiments were carried out in the same manner to examine the effect of DES water contents of 10, 20, 30, 40, 50,60,70,80,90% on the extraction efficiency of the target compound, respectively. As shown in fig. 3 (a), when the water content is 70%, the extraction efficiency reaches the maximum value, and the extraction efficiency decreases instead by continuing to increase the water content. Comprehensively, the DES water content is selected to be 60-80%.
(b) Selection of liquid-to-material ratio
According to the extraction conditions, other experiments are the same, and the influence of different liquid-to-material ratios of 5, 10, 20, 30 and 40mL/g on the extraction efficiency of the target compound is examined. As shown in fig. 3 (b), when the liquid-to-liquid ratio reaches 20mL/g, the extraction efficiency reaches the maximum value, and the solid-to-liquid ratio continues to increase, and the extraction efficiency decreases instead. This may be due to DES itself results and physical characteristics. In combination, the liquid-to-material ratio is selected to be 10-40mL/g.
(c) Selection of extraction temperature
According to the extraction conditions, other experiments are the same, and the influence of different extraction temperatures of 20 ℃,35 ℃,40 ℃,45 ℃,50 ℃,55 ℃,60 ℃ on the extraction efficiency of the target compound is examined respectively. As shown in fig. 3 (c), the extraction efficiency of dihydromyricetin gradually increases when the extraction temperature increases from 30 ℃ to 50 ℃, whereas the extraction efficiency of dihydromyricetin decreases slightly when the temperature further increases, probably due to degradation of the compound at high temperature. In combination, the extraction temperature is selected to be 35-55 ℃.
(d) Selection of extraction time
According to the extraction conditions, other experiments are the same, and the influence of different extraction times of 0.5,1,1.5,2,2.5,3 and 3.5 hours on the extraction efficiency of the target compound is examined respectively. As shown in fig. 3 (d), when the extraction time was 2.5h, the extraction efficiency of the target compound was maximized, and after further extending the extraction time, the change in the extraction efficiency of the target compound was insignificant, suggesting that the extraction process had reached equilibrium. Comprehensive, the extraction time is selected to be 2-3h.
(e) Optimizing optimal extraction conditions by response surface experiments
According to the center combination experimental design principle of Box-Behnken, the extraction efficiency of dihydromyricetin is taken as a response value (Y), the fixed liquid-to-material ratio is 20mL/g, DES water content (A), extraction temperature (B) and time (C) are selected as optimization factors, and a three-factor three-level response surface analysis method is adopted. The experimental factors and horizontal designs are shown in table 2.
TABLE 2 response surface factor design level table
In order to examine the influence of each factor and interaction thereof on the extraction efficiency, the invention utilizes Design-Expert software to carry out multiple regression fitting on three levels of four factors in table 2 to obtain a calculation equation Y= 2.960A-0.482B+6.531C+0.014AB-0.060AC+0.294BC-0.024A of the total extraction efficiency 2 -0.014B 2 -2.837C 2 -63.463. The analysis of variance of the fitted quadratic polynomial model is shown in Table 3, model P<0.0001 (extremely significant), indicating that the model can be used to make predictions of response values. The model mismatch term is not obvious, which indicates that the fitting degree of the regression equation in the whole regression space is good.
TABLE 3 model analysis of variance
The response surface graph obtained according to the regression equation is shown in fig. 4, which shows the effects of the factors and the relationship between the interaction and the extraction efficiency. The optimal extraction conditions of the dihydromyricetin in the vine tea are obtained through analysis: the water content is 71.18%, the extraction time is 2.80h, and the extraction temperature is 46.40 ℃. The yield of the dihydromyricetin measured by the condition is 40.1%, which is similar to the calculated value 39.82% of the model, and the optimal extraction condition obtained by the response surface method is accurate and reliable and has practical application value.
Example 2: selection of macroporous resin and selection of loading conditions
Separating by macroporous resin: taking 1mL of dihydromyricetin extracting solution obtained by taking No. 12 DES as an extracting agent in the embodiment 1, loading the dihydromyricetin extracting solution on macroporous resin, eluting the dihydromyricetin extracting solution with a large amount of distilled water and 80% ethanol (10 mL) in sequence, collecting an ethanol eluting part after loading the sample to obtain an eluent A, concentrating the eluent to obtain a concentrate B, and measuring the purity yield.
(a) Screening of macroporous resins
Nine macroporous resins of XAD1600N, XAD16, XAD1180, XAD7HP, D101, S-8, AB-8, DM301 and X-5 were selected for carrying out the adsorption recovery experiment of the dihydromyricetin extract, and the results of AB-8, DM301 or XAD-7HP show that the effect on the dihydromyricetin is better (figure 5 a). The DM301 was reused 6 times and the recovery was good (fig. 5 b).
(b) Influence study of sample conditions
Specifically, according to the above adsorption elution procedure, the effect of the solid-to-liquid ratio (2, 1,0.5, 0.33,0.25,0.2 g/mL), the loading concentration (306.52, 234.19, 98.11, 47.58, 25.93. Mu.g/mL), and the adsorption temperature (20, 30, 40, 50,60 ℃) on the adsorption rate of dihydromyricetin was examined under the same conditions, and as shown in FIG. 6, the adsorption rate was decreased with the increase of the solid-to-liquid ratio and the adsorption temperature, and the adsorption rate was increased with the decrease of the adsorption initial concentration. Therefore, the recovery rate of dihydromyricetin can be increased by selecting proper solid-to-liquid ratio, adsorption concentration and adsorption temperature.
Example 3: method for extracting dihydromyricetin from vine tea
1) Preparation of DES: the tetrabutyl ammonium bromide serving as a hydrogen bond acceptor and pyruvic acid serving as a hydrogen bond donor are subjected to eutectic melting according to the mol ratio of 1:2, and the eutectic melting condition is that: shaking at 200rpm in a shaking table at 80 ℃ for 3.5 hours to obtain DES, and standing overnight;
2) DES extraction: preparing the DES obtained in the step 1) and water into an extraction solvent with the concentration of 70%, uniformly mixing the vine tea powder and the extraction solvent according to the liquid-to-material ratio of 20mL/g, wherein the grain size of the vine tea powder is less than 1mm, the water content of the vine tea powder is 11%, and the vine tea powder is vibrated in a shaking table at 45 ℃ and the rotating speed of 200rpm for 2.5 hours to obtain an extraction liquid of dihydromyricetin; HPLC detection shows that the yield of dihydromyricetin in the extract reaches 40.09%;
3) And (3) macroporous resin adsorption separation: taking 1ml of the dihydromyricetin extract obtained in the step 2), loading the extract on macroporous resin, wherein the model of the macroporous resin is DM301, and the macroporous resin adsorption and separation conditions are as follows: the solid-to-liquid ratio is 2g/mL, the initial loading concentration is 25.93 mug/mL, the adsorption temperature is 20 ℃, distilled water, 80% ethanol and 95% ethanol are sequentially used for eluting, 80% ethanol eluent A is collected and obtained, the eluent A is concentrated to obtain concentrate B, namely the dihydromyricetin monomer component, and 23.34mg of dihydromyricetin with the purity of 92.1% is obtained (figure 7).
Example 4: method for extracting dihydromyricetin from vine tea
1) Preparation of DES: the tetrabutyl ammonium bromide serving as a hydrogen bond acceptor and pyruvic acid serving as a hydrogen bond donor are subjected to eutectic melting according to the mol ratio of 1:2, and the eutectic melting condition is that: shaking for 3 hours at 200rpm in a shaking table at 80 ℃ to obtain DES, and standing overnight;
2) DES extraction: preparing the DES obtained in the step 1) and water into an extraction solvent with the concentration of 60%, uniformly mixing the vine tea powder and the extraction solvent according to the liquid-material ratio of 40mL/g, wherein the grain diameter of the vine tea powder is less than 1mm, the water content of the vine tea powder is 10.5%, the temperature is 55 ℃, and the shaking is carried out in a shaking table with the rotating speed of 230rpm for 3 hours, so as to obtain the extract of the dihydromyricetin; HPLC detection shows that the yield of dihydromyricetin in the extract reaches 39.64%;
3) And (3) macroporous resin adsorption separation: taking 2ml of the dihydromyricetin extract obtained in the step 2), loading the dihydromyricetin extract on macroporous resin, wherein the type of the macroporous resin is AB-8, and the macroporous resin adsorption and separation conditions are as follows: the solid-to-liquid ratio is 1.5g/mL, the initial loading concentration is 40 mu g/mL, the adsorption temperature is 30 ℃, distilled water, 80% ethanol and 95% ethanol are sequentially used for eluting, 80% ethanol eluent A is collected and obtained, the eluent A is concentrated to obtain concentrate B, namely the dihydromyricetin monomer component, and 21.24mg of dihydromyricetin with the purity of 91.6% is obtained.
Example 5: method for extracting dihydromyricetin from vine tea
1) Preparation of DES: the tetrabutyl ammonium bromide serving as a hydrogen bond acceptor and pyruvic acid serving as a hydrogen bond donor are subjected to eutectic melting according to the mol ratio of 1:2, and the eutectic melting condition is that: shaking for 4 hours at 200rpm in a shaking table at 80 ℃ to obtain DES, and standing overnight;
2) DES extraction: preparing 80% concentration extraction solvent from DES obtained in the step 1) and water, uniformly mixing vine tea powder and the extraction solvent according to a liquid-material ratio of 10mL/g, wherein the grain size of the vine tea powder is less than 1mm, the water content of the vine tea powder is 11.5%, and shaking for 2 hours in a shaking table at 35 ℃ and a rotating speed of 150rpm to obtain dihydromyricetin extraction liquid; HPLC detection shows that the yield of dihydromyricetin in the extract reaches 39.40%;
3) And (3) macroporous resin adsorption separation: taking 1ml of the dihydromyricetin extract obtained in the step 2), loading the extract on macroporous resin, wherein the type of the macroporous resin is XAD-7HP, and the macroporous resin adsorption and separation conditions are as follows: the solid-to-liquid ratio is 1.5g/mL, the initial loading concentration is 40 mu g/mL, the adsorption temperature is 30 ℃, distilled water, 80% ethanol and 95% ethanol are sequentially used for eluting, 80% ethanol eluent A is collected and obtained, the eluent A is concentrated to obtain concentrate B, namely the dihydromyricetin monomer component, and 44.62mg of dihydromyricetin with the purity of 90.9% is obtained.
Claims (3)
1. A method for extracting dihydromyricetin from vine tea, which is characterized by comprising the following steps:
1) Preparation of DES: eutectic bonding of the hydrogen bond acceptor and the hydrogen bond donor to obtain DES, and standing overnight; the hydrogen bond acceptor is tetrabutylammonium bromide; the hydrogen bond donor is pyruvic acid; the molar ratio of tetrabutylammonium bromide to pyruvic acid is 1:2;
2) DES extraction: preparing an extraction solvent from the DES obtained in the step 1) and water, uniformly mixing vine tea powder and the extraction solvent, and performing shake extraction to obtain an extraction solution of dihydromyricetin; the DES and water are prepared into an extraction solvent with the volume concentration of 60-80 percent; the liquid-material ratio of vine tea powder to extraction solvent is 10-40 mL/g; the oscillation extraction conditions are as follows: shaking in a shaking table at 35-55deg.C and rotation speed of 150-230rpm for 2-3 hr;
3) And (3) macroporous resin adsorption separation: loading the extract of the dihydromyricetin obtained in the step 2) on macroporous resin, eluting with distilled water, 80% ethanol and 95% ethanol in sequence, collecting the 80% ethanol eluent A, concentrating the eluent A to obtain a concentrate B, namely the dihydromyricetin monomer component, wherein the macroporous resin has the model of AB-8, DM301 or XAD-7HP, and the macroporous resin has the following adsorption separation conditions: the solid-liquid ratio is 1-2g/mL, the initial loading concentration is 25-100 mu g/mL, and the adsorption temperature is 20-30 ℃.
2. A method for extracting dihydromyricetin from tenuifolia tea according to claim 1, wherein the conditions of the co-melting treatment in step 1) are: shaking at 200rpm in a shaker at 80℃for 3-4 hours.
3. The method for extracting dihydromyricetin from vine tea according to claim 1, wherein the grain size of vine tea powder in the step 2) is smaller than 1mm, and the water content of vine tea powder is 10% -12%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111403173.4A CN114031587B (en) | 2021-11-24 | 2021-11-24 | Method for extracting dihydromyricetin from vine tea |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111403173.4A CN114031587B (en) | 2021-11-24 | 2021-11-24 | Method for extracting dihydromyricetin from vine tea |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114031587A CN114031587A (en) | 2022-02-11 |
| CN114031587B true CN114031587B (en) | 2023-08-08 |
Family
ID=80145325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111403173.4A Active CN114031587B (en) | 2021-11-24 | 2021-11-24 | Method for extracting dihydromyricetin from vine tea |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114031587B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115960066A (en) * | 2022-12-26 | 2023-04-14 | 湖北省农业科学院中药材研究所 | Method for extracting dihydromyricetin from vine tea |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777696A (en) * | 2016-04-06 | 2016-07-20 | 华南理工大学 | Method for extracting anthocyanin by utilizing deep eutectic solvent (DES) |
| CN109305954A (en) * | 2018-11-21 | 2019-02-05 | 中南民族大学 | A method of isolating and purifying dihydromyricetin from vine tea |
| CN112028865A (en) * | 2020-09-23 | 2020-12-04 | 劲牌持正堂药业有限公司 | Method for extracting and preparing high-content dihydromyricetin from vine tea |
-
2021
- 2021-11-24 CN CN202111403173.4A patent/CN114031587B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777696A (en) * | 2016-04-06 | 2016-07-20 | 华南理工大学 | Method for extracting anthocyanin by utilizing deep eutectic solvent (DES) |
| CN109305954A (en) * | 2018-11-21 | 2019-02-05 | 中南民族大学 | A method of isolating and purifying dihydromyricetin from vine tea |
| CN112028865A (en) * | 2020-09-23 | 2020-12-04 | 劲牌持正堂药业有限公司 | Method for extracting and preparing high-content dihydromyricetin from vine tea |
Non-Patent Citations (1)
| Title |
|---|
| 低共熔溶剂中天然产物分离方法研究;田海圆;《硕士学位论文电子期刊》;20210315(第3期);第11-29页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114031587A (en) | 2022-02-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114031587B (en) | Method for extracting dihydromyricetin from vine tea | |
| CN102835713B (en) | A kind of Acerola cherry fruit powder and manufacture method thereof | |
| CN101824018B (en) | Method for purifying dihydromyricetin | |
| CN103665059B (en) | A kind of natural crocin extraction separation method and the preparation of blood lipid-lowering medicine thereof | |
| CN102875514A (en) | Method for extracting and purifying anthocyanins from blueberry red leaves | |
| CN107936079B (en) | Method for preparing high-purity mogroside V | |
| CN102030733B (en) | The preparation method of a kind of high purity costuslactone and dehydro-α-curcumene | |
| CN104231097A (en) | Preparation method of lyceum barbarum polysaccharide | |
| CN110882357A (en) | High-purity bamboo leaf flavonoid powder and preparation method thereof | |
| CN101985440B (en) | Method for producing piperine | |
| CN107573255A (en) | A kind of method that capsaicine and dihydrocapsaicin are isolated and purified from pepper fruit | |
| CN105712896B (en) | A kind of method that macamide monomer is efficiently prepared from maca | |
| CN102648750B (en) | Refined Chinese date cane sugar, Chinese date high fructose syrup and preparation method thereof | |
| CN101941936B (en) | Process for extracting 5-hydroxytryptamine as bioactive substance from sea buckthorns | |
| CN112125948B (en) | Method for synchronously extracting plant polyphenol and plant protein from plant leaves and preparing plant protein hydrolysis peptide | |
| CN112450420A (en) | Seasoning salt and preparation method thereof | |
| CN102078400B (en) | Preparation method of extract of total triterpene acid of loquat leaf | |
| CN105646429A (en) | Method for preparing high-purity catechin gallate CG | |
| CN105820142B (en) | A kind of pre-treating method for extracting fucoxanthin brown alga sample | |
| CN112300233B (en) | Method for separating and preparing paeoniflorin-3-O- (6-O-p-coumaroyl) glucoside-5-glucoside | |
| CN109956873B (en) | Pentanediamine melt crystallization process | |
| CN106674326A (en) | Method for separating hordein fractions by using zeolite | |
| CN115057900B (en) | Method for extracting anthocyanin from Aronia melanocarpa | |
| CN109574976B (en) | Method for industrially extracting dihydroquercetin from larch roots | |
| CN108329374B (en) | Method for separating high-purity tea seed saponin monomer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |