CN114699468A - Preparation method of vine tea extract - Google Patents
Preparation method of vine tea extract Download PDFInfo
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- CN114699468A CN114699468A CN202210324000.1A CN202210324000A CN114699468A CN 114699468 A CN114699468 A CN 114699468A CN 202210324000 A CN202210324000 A CN 202210324000A CN 114699468 A CN114699468 A CN 114699468A
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- filtrate
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- ampelopsis grossedentata
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
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- A61K36/87—Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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Abstract
The invention discloses a preparation method of vine tea extract, which comprises the steps of preliminarily extracting vine tea through enzymolysis, simultaneously destroying intercellular layers and cell walls between vine tea cells, further destroying the inner cell layers, simulating the environment of transportation and absorption of oral drugs through gastrointestinal tracts, and carrying out acid-base digestion treatment on vine tea filter residues, thus being very beneficial to leaching out active ingredients in the vine tea, then adopting an ultrasonic auxiliary technology, leading the cell walls of raw materials to be destroyed through mechanical action, cavity action and thermal effect generated by ultrasonic waves, fully extracting the active ingredients in the vine tea in a short time under the condition of low temperature, and finally adding high-concentration alcohol for extraction for a certain time, removing negative active ingredients such as protein, pectin and the like in the extract, and greatly improving the yield of the active ingredients such as vine tea flavone, polysaccharide and the like. The Ampelopsis grossedentata extract prepared by the method is bright in color, palatable in sour and sweet taste and good in product stability.
Description
Technical Field
The invention relates to the technical field of vine tea extraction, and particularly relates to a preparation method of a vine tea extract.
Background
Ampelopsis grossedentata (Ampelopsis grossedentata) is a wild vine of the genus Ampelopsis of the family Vitaceae, commonly known as nectarine, white tea, white monkey, etc. Is a perennial vine plant which is widely distributed in the south of the Yangtze river in China, is an ancient medicine and food dual-purpose plant and is widely used as a tea plant and a Chinese herbal medicine in folks for a long time. The tea is a wild natural tea plant substitutional tea with unique health care efficacy and drinking value, the whole plant has medicinal value, sweet and light taste, is cool, and has the efficacies of dispelling wind-damp, clearing heat and removing toxicity, strengthening bones and muscles and the like. The vine tea is cool in nature, has high medicinal and nutritional values of stopping bleeding, removing blood stasis, relieving swelling, removing rheumatism, diminishing inflammation, resisting thrombus, reducing blood fat, resisting oxidation and the like, and the tender stems and leaves of the vine tea contain various chemical components including moisture, protein, vitamins, polyphenol, flavone and the like. Wherein the flavonoid compounds have important pharmacological action. Dihydromyricetin is an important flavonoid compound in the dihydromyricetin. Therefore, the extraction and detection of the ampelopsis grossedentata are widely concerned at home and abroad.
In the prior art, the extraction process of the vine tea mainly comprises 2 methods of water extraction and alcohol extraction, and the water extraction method is more researched. Quadrature method is used to investigate the influence of alcohol concentration, dosage, extraction time and times on ampelopsis grossedentata dihydromyricetin. The orthogonal design method for the fructus Myricae Rubrae is used to examine the influence of 3 factors of microwave extraction temperature, radiation time and feed-liquid ratio on the yield of dihydromyricetin in Ampelopsis Grossdentata. The mature osmanthus discusses the influence of the extraction temperature, time and volume of the ampelopsis grossedentata flavone by taking water as an extractant. Although the cost of the extractant is low, the extractant using water as the extractant has high extraction temperature, long-time flavone extraction rate and low purity, increases the difficulty of subsequent separation and purification, and tends to reduce the activity of effective substances such as flavone and the like under the action of long-time high temperature. The extraction rate is low by using alcohol as an extracting agent, the content of the separated effective substances is low, and the defects of solvent residue exist.
In the prior art, the extraction of the ampelopsis grossedentata also comprises a supercritical carbon dioxide extraction method, although the method has small pollution and mild extraction conditions, and is not easy to damage bioactive substances in raw materials, the equipment investment is large, and effective active substances of the ampelopsis grossedentata cannot be extracted to the maximum extent.
For example, the application number is [ CN202110979359.8 ], a process for extracting dihydromyricetin from ampelopsis grossedentata and a process for preparing ampelopsis grossedentata functional beverage, wherein the extraction method comprises the steps of pretreatment, countercurrent extraction treatment, pretreatment of filter residues, extraction and combination of filter residues, reduced pressure concentration of flavonoid extracts, crystallization and the like. The leaching method can fully leach the raw materials, can more thoroughly leach residual flavonoid substances in filter residues, ensures high-efficiency extraction of the flavonoid substances, and has high leaching rate and high flavonoid content. Meanwhile, the extraction method adopts a method combining water extraction, ultrasonic extraction and high-pressure extraction, so that potential pollution caused by the use of organic solvents such as ethanol and the like is avoided.
The extraction process adopts low-temperature countercurrent extraction, adopts a surfactant as a solvent, greatly improves the extraction amount, and fully extracts residual flavone substances in filter residues. However, the problem of solvent residue exists by adopting low-temperature countercurrent leaching and then adding the surfactant, and the surfactant can also damage bioactive substances in the raw materials, so that the content of effective substances in the ampelopsis grossedentata is reduced.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of vine tea extract, the vine tea is extracted by taking vine tea as a raw material, the vine tea extract contains rich active ingredients and has good effects of oxidation resistance, bacteriostasis and the like, and the method has short extraction time and low temperature and can fully extract the active ingredients in the vine tea.
In order to achieve the purpose, the invention is realized by the following technical scheme: the invention provides a preparation method of a vine tea extract, which comprises the following steps:
s1, dissolving the vine tea in a solvent, adding a combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filtrate A;
preferably, the solvent in S1 is deionized water or an ethanol solution with a mass concentration of 60%.
Preferably, the mass ratio of the ampelopsis grossedentata to the combined enzyme to the solvent in the step S1 is 40: (0.4-2): 400.
the preparation method comprises the steps of washing the vine tea to remove impurities, and then dissolving the vine tea in a solvent.
If the solvent contains ions such as calcium and magnesium, the effective components in Ampelopsis Grossdentata can react with polyphenol. Particularly, when the hardness of water exceeds 3 mg/L, the vine tea is extracted, and a large amount of precipitate is found in the extracted tea soup. Therefore, the vine tea is preferably extracted by using low-hardness water which is purified by treatment, and in the invention, the solvent in the S1 is deionized water. Meanwhile, an ethanol solution with the mass concentration of 60% can be used for replacing deionized water for dissolution.
After the vine tea is dissolved, in order to break the cell wall of the vine tea, the invention adopts combined enzyme to carry out enzymolysis on the vine tea.
Preferably, the combined enzyme comprises pectinase, cellulase, amylase and protease in a mass ratio of 1: 1: 1: 1. the combined enzyme can simultaneously destroy intercellular layers and cell walls between cells, further destroy intracellular layers, convert macromolecular substances into small molecular substances, and further easily extract effective substances such as dihydromyricetin and polysaccharide in subsequent treatment.
Then filtering the vine tea solution after enzymolysis to obtain filter residue A and filtrate A, but the extraction effect achieved by only destroying cell walls by enzymolysis is not complete, so the invention carries out acid-base treatment on the filter residue A.
S2, dissolving the filter residue A obtained in the step S1, adding a buffer solution, adjusting the pH value to 2.5-3.5, performing high-pressure microwave treatment, and filtering to obtain filter residue B and filtrate B;
s3, dissolving the filter residue B obtained in the step S2, adding a buffer solution, adjusting the pH value to 8-9, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
preferably, the pressure of the high-pressure microwave treatment in S2-S3 is 400-600 KPa, and the time is 10 min.
According to the invention, the vine tea filter residue after enzymolysis is subjected to acid treatment and then alkali treatment, and simultaneously, the high-pressure microwave assistance is adopted, and the residual protease in the filter residue A is combined, so that the environment that oral drugs are transported and absorbed through gastrointestinal tracts can be highly simulated, and the vine tea filter residue is subjected to deep digestion treatment, thereby being very beneficial to leaching of active ingredients in vine tea.
Secondly, in order to further extract vine tea residues, carrying out ultrasonic extraction on filter residue C obtained after acid-base treatment. The method comprises the following specific steps:
s4, adding a buffering agent into the filter residue C obtained in the step S3, adjusting the pH value of the solution to 3.0-5.0, carrying out ultrasonic extraction, filtering to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract.
Preferably, the ultrasonic extraction conditions in S4 are as follows: extracting with 100W ultrasound at 50 deg.C for 30 min.
Preferably, the ultrasonic extraction liquid in the S4 is filtered by a 0.8um filter membrane.
Preferably, the buffer solution in the S2-S3 is citric acid-disodium hydrogen phosphate, and the buffer solution in the S4 is citric acid. Mainly plays a role in buffering the pH regulation.
In the invention, citric acid as a buffering agent is added into the filter residue C, the pH of the solution is adjusted to 3.0-5.0, deionized water is used as a solvent, and a low-temperature ultrasonic extraction technology is adopted to sufficiently extract active ingredients in the vine tea residue in a short time.
The action mechanism of the ultrasonic-assisted extraction method is mainly that the mechanical action, the cavitation action and the thermal effect generated by ultrasonic waves are utilized to cause the cell walls of the raw materials to be damaged, so that target objects penetrate through cell membranes, the extraction time can be shortened, the volume use is reduced, the extraction temperature is reduced, and the quality and the yield of the target products are improved to a greater extent. The vine tea is extracted by ultrasonic wave assistance, so that the structure and the activity of the extract are not influenced, and the yield of the vine tea is improved to a greater extent.
After the ampelopsis grossedentata is subjected to a series of treatments, filtrate A obtained by enzyme treatment, filtrate B obtained by acid treatment, filtrate C obtained by alkali treatment and filtrate D obtained by low-temperature ultrasonic extraction are mixed together to obtain a crude extract of all the ampelopsis grossedentata.
In order to purify the crude extract of the vine tea, the invention adopts low-temperature alcohol precipitation to ensure that unstable precipitates in the extract are fully separated out, and the vine tea extract prepared by the method is bright in color and luster, the product yield (the mass m of a finished product/the mass m of raw material vine tea) is 80-95 percent, and the vine tea extract contains components such as polysaccharide and the like. The purification steps are as follows:
s5, concentrating the crude extract obtained in S4 to density of 0.9000-1.0000g/cm3Then adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 46-48h, and then filtering the alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in S5 to density of 0.9000-1.0500g/cm3Centrifuging, collecting supernatant, precipitating at 4-5 deg.C for 22-24 hr, and filtering to obtain Ampelopsis Grossdentata extract.
Preferably, the mass ratio of the ethanol with the mass concentration of 95% added in the S5 to the concentrated crude extract is 1: 1.
preferably, the centrifugation conditions in S6 are: centrifuging at 4000r/min for 20 min.
Compared with the prior art, the invention has the following beneficial effects:
1. the vine tea extract is prepared by preliminarily extracting vine tea through enzymolysis, wherein intercellular layers and cell walls among vine tea cells can be simultaneously destroyed, so that cell inner layers are destroyed, the environment that oral drugs are transported and absorbed through gastrointestinal tracts is simulated, and the vine tea filter residues are subjected to deep acid-base digestion treatment, so that active ingredients in the vine tea are very favorably leached out, then the ultrasonic auxiliary technology is adopted, the cell walls of raw materials are destroyed through mechanical action, cavity action and thermal effect generated by ultrasonic waves, the active ingredients in the vine tea are fully extracted in a short time under the condition of low temperature, finally high-concentration alcohol is added for extraction for a certain time, negative active ingredients such as protein, pectin and the like in the extract are removed, and the yield of the active ingredients such as vine tea flavone, polysaccharide and the like is greatly improved. The Ampelopsis grossedentata extract prepared by the method is bright in color, palatable in sour and sweet taste and good in product stability.
2. The preparation method of the vine tea extract provided by the invention has the advantages of short extraction time and low temperature, can fully extract active ingredients in vine tea, adjusts the pH value in the extraction process, and can make the prepared vine tea extract more stable in property through low-temperature alcohol precipitation and other modes.
Drawings
FIG. 1 is a liquid phase diagram of a mixed standard of 6 kinds of saccharides in example 3 of the present invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
The specific embodiment of the invention is as follows:
example 1
A preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of ampelopsis grossedentata, adding into 400g of deionized water, then adding 0.4g of combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filter liquor A, wherein the combined enzyme comprises pectinase, cellulose, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 2.5, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH value of the solution to 3.0, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in S4 to a density of 0.9000g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 46h, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the step S5 to a density of 0.9000g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 22 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 80.1%.
Example 2
A preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea, adding the vine tea into 400g of deionized water, then adding 1.2g of combined enzyme for enzymolysis for 40min, and filtering to obtain a filter residue A and a filter liquor A, wherein the combined enzyme comprises pectinase, cellulose, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8.5, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH of the solution to 4.0, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 0.9500g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47 hours, and then filtering an alcohol precipitation liquid to obtain a filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to a density of 0.9500g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 23 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 82.2%.
Example 3
A preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of ampelopsis grossedentata, adding the ampelopsis grossedentata into 400g of 60% ethanol solution, adding 1.2g of combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filter liquor A, wherein the combined enzyme comprises pectinase, cellulase, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8.5, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH of the solution to 4.0, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 0.9500g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to a density of 0.9500g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 23 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 82.5%.
Example 4
A preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea, adding the vine tea into 400g of deionized water, then adding 1.6g of combined enzyme for enzymolysis for 40min, and filtering to obtain a filter residue A and a filter liquor A, wherein the combined enzyme comprises pectinase, cellulose, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3.2, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8.8, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH of the solution to 4.5, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 0.9800g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47.5 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to a density of 0.9800g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, precipitating at 4 deg.C for 23.5 hr, and filtering to obtain Ampelopsis Grossdentata extract with yield of 82.0%.
Example 5
A preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea, adding the vine tea into 400g of deionized water, then adding 2.0g of combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filter liquor A, wherein the combined enzyme comprises pectinase, cellulose, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3.5, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 9, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH of the solution to 5, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 1.0000g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 48 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to density of 1.0000g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 24 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 81.9%.
Comparative example 1
The difference between comparative example 1 and example 3 is that the enzymolysis was carried out without adding the enzyme combination in comparative example 1. The method comprises the following specific steps:
a preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea;
s2, dissolving the ampelopsis grossedentata in the S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3, performing high-pressure microwave treatment, and filtering to obtain filter residue B and filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8.5, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding 0.8g of citric acid into the filter residue C obtained in the step S3, adjusting the pH of the solution to 4.0, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 0.9500g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to a density of 0.9500g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 23 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 75.1%.
Comparative example 2
The difference between the comparative example 2 and the example 3 is that the environment for transporting and absorbing oral drugs through the gastrointestinal tract is not simulated in the comparative example 2, and the vine tea filter residue is subjected to deep acid-base digestion treatment. The method comprises the following specific steps:
a preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea, adding the vine tea into 400g of 60% ethanol solution, then adding 1.2g of combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filter liquor A, wherein the combined enzyme comprises pectinase, cellulase, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, adding 0.8g of citric acid into the filter residue A obtained in the step S1, adjusting the pH of the solution to 4.0, carrying out ultrasonic extraction for 30min at 50 ℃ and 100W of ultrasonic power, filtering through a 0.8um filter membrane to obtain a filtrate D, and combining the filtrate A and the filtrate D obtained in the step S to obtain a crude extract;
s3, concentrating the crude extract obtained in the step S2 to a density of 0.9500g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s4, concentrating filtrate E obtained by filtering in the S3 to a density of 0.9500g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 23 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 79.3%.
Comparative example 3
Comparative example 3 differs from example 3 in that no ultrasound-assisted extraction was performed in comparative example 3. The method comprises the following specific steps:
a preparation method of vine tea extract comprises the following steps:
s1, weighing 40g of vine tea, adding the vine tea into 400g of 60% ethanol solution, then adding 1.2g of combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filter liquor A, wherein the combined enzyme comprises pectinase, cellulase, amylase and protease in a mass ratio of 1: 1: 1: 1;
s2, dissolving the filter residue A obtained in the step S1 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 3, performing high-pressure microwave treatment, and filtering to obtain a filter residue B and a filtrate B, wherein the pressure of the high-pressure microwave treatment is 400KPa, and the time is 10 min;
s3, dissolving the filter residue B obtained in the step S2 in 400g of deionized water, adding 0.8g of citric acid-disodium hydrogen phosphate, adjusting the pH value to 8.5, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, combining the filtrate A, the filtrate B and the filtrate C obtained in the previous step to obtain a crude extract;
s5, concentrating the crude extract obtained in the step S4 to a density of 0.9500g/cm3And then, mixing the components in a mass ratio of 1: 1, adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 47 hours, and then filtering alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in the S5 to a density of 0.9500g/cm3Centrifuging at 4000r/min for 20min, collecting supernatant, settling at 4 deg.C for 23 hr, and filtering to obtain Ampelopsis grossedentata extract with yield of 76.6%.
As can be seen from the results of examples 1-5 and comparative examples 1-3, the yield of examples 1-5 is significantly higher than that of comparative examples 1-3, which shows that the vine tea extraction method provided by the invention can more fully extract the active ingredients in the vine tea.
Test example 1
Since the vine tea extract prepared in example 3 has the highest yield, the liquid chromatography analysis of the extract obtained in example 3 is carried out according to the invention, and the chromatographic conditions are as follows: analyzing by adopting an HPLC-CAD method, taking acetonitrile-water as a mobile phase, setting the flow rate at 1mL/min, the column temperature at 30 ℃, the sample injection amount at 10uL, adopting a gradient elution mode, and adopting the following parameters of an electrospray detector (CAD): the acquisition frequency is 10 Hz; an optical filter 10 s; the temperature is 35 ℃; air supply: nitrogen gas. The gradient elution procedure was: 0-16 min, 80% -20%; 16-22 min, 75% -25%; 22-33 min, 55% -45%; 33-36 min, 80% -20%.
The liquid phase diagram of the mixed standard substance of 6 kinds of sugars in example 3 is shown in FIG. 1.
Test example 2
In the present invention, the yields of example 2 and example 3 are higher, and the main difference is whether the solvent used in step S1 is water or 60% ethanol, so the present invention performs the determination of the contents of 6 kinds of sugars for example 2 and example 3, and the statistical results of the contents of 6 kinds of sugars are shown in table 1 below.
Table 1 content of saccharide component in ampelopsis grossedentata extract in example 1
| Components | Retention time (min) | Example 2 (mg/g) | Example 3 (mg/g) |
| Arabinol | 12.432 | 0.29 | / |
| Fructose | 13.663 | 0.25 | 0.21 |
| Sorbitol | 15.794 | 0.06 | / |
| Glucose | 19.643 | 0.37 | 0.09 |
| Sucrose | 27.782 | / | 0.19 |
| Maltitol | 28.953 | 0.26 | 0.07 |
As can be seen from Table 1, when water was used as the extract and 60% ethanol was used as the extract, there were differences in the polysaccharide content and composition, and when water was used as the extract, the Ampelopsis grossedentata extract contained 5 kinds of sugar components including arabinitol, fructose, sorbitol, glucose and maltitol, of which the highest content was glucose, and was 0.37 mg/g; when 60% ethanol is used as extractive solution, the Ampelopsis grossedentata extract contains 4 kinds of sugar components including fructose, glucose, sucrose and maltitol, wherein the highest content of fructose is 0.21 mg/g.
Therefore, the vine tea extract preparation method provided by the invention has the advantages that the vine tea extract contains rich active ingredients, has better effects of antioxidation, bacteriostasis and the like, and has short extraction time and low temperature compared with the traditional extraction method, and the active ingredients can be fully extracted.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the specific embodiments of the invention be limited to these descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. A preparation method of an ampelopsis grossedentata extract is characterized by comprising the following steps:
s1, dissolving the vine tea in a solvent, adding a combined enzyme for enzymolysis for 40min, and filtering to obtain filter residue A and filtrate A;
s2, dissolving the residue A obtained in S1, adding a buffer solution, adjusting the pH value to 2.5-3.5, performing high-pressure microwave treatment, and filtering to obtain a residue B and a filtrate B;
s3, dissolving the filter residue B obtained in the step S2, adding a buffer solution, adjusting the pH value to 8-9, performing high-pressure microwave treatment, and filtering to obtain filter residue C and filtrate C;
s4, adding a buffering agent into the filter residue C obtained in the step S3, adjusting the pH value of the solution to 3.0-5.0, carrying out ultrasonic extraction, filtering to obtain a filtrate D, and combining the filtrate A, the filtrate B, the filtrate C and the filtrate D obtained in the step S to obtain a crude extract;
s5, concentrating the crude extract obtained in S4 to density of 0.9000-1.0000g/cm3Then adding ethanol with the mass concentration of 95% to carry out alcohol precipitation for 46-48h, and then filtering the alcohol precipitation liquid to obtain filtrate E;
s6, concentrating filtrate E obtained by filtering in S5 to density of 0.9000-1.0500g/cm3Centrifuging, collecting supernatant, precipitating at 4-5 deg.C for 22-24 hr, and filtering to obtain Ampelopsis grossedentata extract.
2. The preparation method of ampelopsis grossedentata extract according to claim 1, wherein the mass ratio of ampelopsis grossedentata to the combined enzyme to the solvent in S1 is 40: (0.4-2): 400.
3. the method for preparing ampelopsis grossedentata extract according to claim 1, wherein the mass ratio of the combined enzymes in S1, including pectinase, cellulase, amylase and protease, is 1: 1: 1: 1.
4. the method for preparing the ampelopsis grossedentata extract according to claim 1, wherein the solvent in S1 is deionized water or an ethanol solution with a mass concentration of 60%.
5. The preparation method of ampelopsis grossedentata extract according to claim 1, wherein the buffer in S2-S3 is citric acid-disodium hydrogen phosphate, and the buffer in S4 is citric acid.
6. The method as claimed in claim 1, wherein the pressure of the high pressure microwave treatment in S2-S3 is 400-600 KPa, and the time is 10 min.
7. The method for preparing ampelopsis grossedentata extract according to claim 1, wherein the ultrasonic extraction conditions in S4 are as follows: extracting with 100W ultrasound at 50 deg.C for 30 min.
8. The method for preparing Ampelopsis grossedentata extract as claimed in claim 1, wherein the sonicated extract of S4 is filtered through a 0.8um filter.
9. The preparation method of the ampelopsis grossedentata extract as claimed in claim 1, wherein the mass ratio of the 95% ethanol added in S5 to the concentrated crude extract is 1: 1.
10. the method for preparing Ampelopsis grossedentata extract as claimed in claim 1, wherein the centrifugation conditions in S6 are as follows: centrifuge at 4000r/min for 20 min.
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|---|---|---|---|---|
| CN115137091A (en) * | 2022-07-11 | 2022-10-04 | 湖北中烟工业有限责任公司 | Method for extracting waste tobacco stems of cigars |
| CN115212154A (en) * | 2022-08-17 | 2022-10-21 | 广州华铄生物科技有限公司 | Preparation method of vine tea fermentation filtrate and application of vine tea fermentation filtrate in cosmetics |
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| CN109692248A (en) * | 2017-10-24 | 2019-04-30 | 汉寿康运医药科技有限公司 | A kind of vine tea total flavone extracting method |
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| CN109692248A (en) * | 2017-10-24 | 2019-04-30 | 汉寿康运医药科技有限公司 | A kind of vine tea total flavone extracting method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115137091A (en) * | 2022-07-11 | 2022-10-04 | 湖北中烟工业有限责任公司 | Method for extracting waste tobacco stems of cigars |
| CN115212154A (en) * | 2022-08-17 | 2022-10-21 | 广州华铄生物科技有限公司 | Preparation method of vine tea fermentation filtrate and application of vine tea fermentation filtrate in cosmetics |
| CN115212154B (en) * | 2022-08-17 | 2023-09-19 | 广州华铄生物科技有限公司 | Preparation method of vine tea fermentation filtrate and application of vine tea fermentation filtrate in cosmetics |
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