CN110563776B - Preparation process of natural vitamins in cherry - Google Patents
Preparation process of natural vitamins in cherry Download PDFInfo
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- CN110563776B CN110563776B CN201910780334.8A CN201910780334A CN110563776B CN 110563776 B CN110563776 B CN 110563776B CN 201910780334 A CN201910780334 A CN 201910780334A CN 110563776 B CN110563776 B CN 110563776B
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- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
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Abstract
The invention discloses a preparation process of natural vitamins in cherries, which relates to the technical field of cherry processing and comprises the following steps: s1: processing raw materials, namely weighing 100-200 parts by weight of cherry fruits, and then crushing the cherry fruits to obtain fruit pulp for later use; s2: extracting, namely adding 50-100 parts by weight of a pretreating agent into the fruit pulp, then adding 30-60 parts by weight of a prepared extracting agent solution, and then placing the mixture into circulating ultrasonic extraction equipment for extraction to obtain an extracting solution; s3: filtering, and filtering and separating the extracting solution for multiple times to obtain filtrate; s4: molecular distillation, namely adding the filtrate into molecular distillation equipment for molecular distillation treatment to obtain a fraction containing vitamins; s5: and (4) carrying out freeze vacuum drying on the fraction to obtain the natural vitamin. The preparation method has the advantages of simplifying the extraction process of the vitamins in the cherries and improving the extraction yield of the vitamins.
Description
Technical Field
The invention relates to the technical field of plant polyphenol extraction processes, in particular to a preparation process of natural vitamins in cherries.
Background
The cherry is a fruit with rich nutrition, the iron content in the cherry is high, and the iron content in every hundred grams of the cherry is up to 59 milligrams and is positioned at the head of the fruit. The vitamin A content is 4-5 times higher than that of grape, apple and orange. The carotene content is 4-5 times more than that of grape, apple and orange. In addition, the cherry also contains vitamin B, C and mineral elements such as calcium and phosphorus.
Vitamins are a type of trace organic substance that must be obtained from food in order for the human and animal body to maintain normal physiological functions. Vitamin deficiency can cause various diseases, for example, long-term deficiency of vitamin A is easy to cause various eye diseases; vitamin B deficiency causes skin disorders; vitamin C deficiency can cause, among other things, scurvy.
At present, the cherry product processing industry is increasingly strong, food and health care products such as fruit juice beverages, fruit wines and fruit jams processed by fruits are gradually popular in the market, the cherries contain rich vitamins, the process for extracting the vitamins from the cherries usually adopts ethanol for extraction, but the ethanol can also leach fat-soluble components in the cherries, so that the yield of the vitamins obtained after purification and filtration is low.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation process of natural vitamins in cherries, and provides a more convenient extraction process of natural vitamins in cherries, which can obtain higher yield by adding a pretreatment agent and an extraction agent in the extraction process.
The above object of the present invention is achieved by the following technical solutions:
the preparation process of the natural vitamins in the cherries comprises the following steps:
s1: processing raw materials, namely weighing 100-200 parts by weight of cherry fruits, and then crushing the cherry fruits to obtain fruit pulp for later use;
s2: extracting, namely adding 50-100 parts by weight of a pretreating agent into the fruit pulp, then adding 30-60 parts by weight of a prepared extracting agent solution, and then placing the mixture into circulating ultrasonic extraction equipment for extraction to obtain an extracting solution;
s3: filtering, and filtering and separating the extracting solution for multiple times to obtain filtrate;
s4: molecular distillation, namely adding the filtrate into molecular distillation equipment for molecular distillation treatment to obtain a fraction containing vitamins;
s5: and (4) carrying out freeze vacuum drying on the fraction to obtain the natural vitamin.
By adopting the technical scheme, cherry fruits are firstly crushed into pulp, so that cell walls, cytoplasm and cell sap in plant cells are separated under the action of mechanical force, and the nutrient components in the cherries are firstly preliminarily purified. And then, by chemical treatment of the pretreatment agent, the components such as pulp fiber, pectin and the like in the pulp are softened and decomposed, so that the nutrient components in the cherry plant cells are further leached, and simultaneously, the subsequently added extractant solution is promoted to be more uniformly mixed with the pulp, so that the vitamins in the pulp are further leached, and the extraction rate of the vitamins is improved. Then removing insoluble impurities in the pulp by a filtering method to obtain cherry extracting solution, and then purifying by molecular distillation to obtain the natural vitamin. The molecular distillation is operated at a temperature far lower than the boiling point, the separation can be achieved as long as a temperature difference exists, so that the influence of high temperature on vitamins can be reduced, and meanwhile, the molecular distillation is performed under high vacuum, so that the vitamins in the materials are not easily oxidized, and the purification yield of the vitamins is improved.
The invention is further configured to: the pretreating agent comprises the following components in percentage by weight:
by adopting the technical scheme, the cellulase can play a certain decomposition or softening role on plant fiber components in the fruit pulp, opens chemical bonds between the cellulose, and the pectinase can play a certain decomposition and softening role on pectin components in the fruit pulp, so that the extractant solution is easier to permeate, and the extraction effect of vitamins is improved. The enzyme activator and the pH regulator are used for increasing the activity of cellulase and pectinase and improving the extraction efficiency of vitamins.
The invention is further configured to: the pretreatment agent is also added with a protective agent with the weight percentage of 1-3%, and the protective agent comprises the following components in percentage by weight:
by adopting the technical scheme, the natural antibacterial extracting agent is added mainly to improve the antibacterial property of the cherry pulp in the extraction process of vitamins in the cherry pulp, so that the breeding of microorganisms such as bacteria and the like is not easy to occur in the extraction process, meanwhile, part of antibacterial components can still be reserved in the vitamin extracting solution after the production is finished, and the product can still keep a certain long-acting antibacterial and bacteriostatic effect. The rosemary extract, the tert-butyl hydroquinone and the tea polyphenol have certain antioxidant capacity, so that the vitamin can be prevented from being reduced in yield due to oxidation reaction in the extraction process. Meanwhile, the substances also have certain antibacterial activity, and the antibacterial activity of the fruit pulp in the extraction process can be improved to a certain extent.
The invention is further configured to: the natural antibacterial extractant is one or more of purslane extract, radish extract and honeysuckle extract.
By adopting the technical scheme, the purslane, radish and honeysuckle contain antibacterial components, and the effects of inhibiting and killing viruses and bacteria are better, so that the extracting solution obtained by extracting the purslane, radish and honeysuckle with ethanol solution is added into the pretreatment agent for pretreating fruit pulp, so that the antibacterial and bacteriostatic activity of the fruit pulp is improved after the fruit pulp is pretreated, and the influence of bacteria and other microorganisms on the extraction process of the fruit pulp is reduced.
The invention is further configured to: the extractant is oxalic acid solution with the mass concentration of 1-5%, phosphoric acid solution with the mass concentration of 1-5% or mixed solution of the two.
By adopting the technical scheme, the oxalic acid solution or the phosphoric acid solution as the extractant solution has better similar and compatible effects on the vitamins in the fruit pulp, so that the vitamins in the fruit pulp are easier to dissolve and separate. When the vitamin and the vitamin are mixed, the two components in the mixed solution respectively have the effect of extracting the vitamin, and the mixing effect and the extracting effect of the two components are enhanced. When the concentration is lower than 1%, the content of the extractant component in the extractant solution is too low, the extraction effect is not obvious, and when the concentration is higher than 5%, the acid concentration is too high, certain influence is generated on the vitamin, and the yield of the vitamin is reduced.
The invention is further configured to: the crushing process in the step S1 specifically operates as follows:
firstly, soaking cherry fruits in a baking soda solution with the practical mass concentration of 3-5% for 3-8 minutes, then washing with an acetic acid solution with the mass concentration of 0.5-1%, finally washing with deionized water, and then grinding into fruit pulp by using a colloid mill.
Through adopting above-mentioned technical scheme, the cherry fruit is soaked with baking soda solution earlier for some microbial bacteria etc. on cherry fruit surface also can be got rid of to dirt and pesticide residue on cherry fruit surface, and the soaking time should not be too short, and too short can make the washing effect of soaking weaken, and the time of soaking if the overlength then can lead to the nutrient composition in the cherry fruit to cause a large amount of losses. Washing the cherry fruits soaked with the baking soda with a low-concentration acetic acid solution to clean the residual baking soda on the cherry fruits, then washing with clean water, and grinding with a colloid mill to obtain fruit pulp.
The invention is further configured to: the multiple filtering in step S3 specifically includes the following steps:
a. adding the extracting solution into a centrifugal machine for centrifugal separation, and removing precipitates to obtain a first filtrate;
b. then filtering the first filtrate by a hollow fiber filter membrane to obtain a second filtrate;
c. and then filtering the second filtrate by an ultrafiltration membrane to obtain a third filtrate.
By adopting the technical scheme, when the extracting solution is filtered for a plurality of times, firstly, the extracting solution is subjected to rotary centrifugation through a centrifugating agent to separate most of insoluble substance impurities in the fruit pulp from the liquid in the fruit pulp, so as to obtain crude extracting solution, and then, the crude extracting solution is filtered through a hollow fiber filter membrane and an ultrafiltration membrane, so that the residual insoluble substance in the liquid is basically removed, and the ultrafiltration can remove macromolecules in the filtrate, leave micromolecules such as vitamins and the like, so as to purify the vitamins.
The invention is further configured to: and in the step S2, the ultrasonic frequency is 40-50 HZ, the extraction temperature is 23-28 ℃, and the extraction time is 40-60 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the vitamins are extracted by adding the pretreating agent and the extracting agent in the extraction process of the vitamins of the cherries, and then are enriched by filtering for multiple times, so that the yield of the vitamins is improved;
2. by adding antibacterial and antioxidant components into the pretreatment agent in the extraction process, the loss of vitamins in the extraction process is reduced, and the yield of the vitamins is further improved.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention discloses a preparation process of natural vitamins in cherries, which comprises the following steps:
s1: the method comprises the following steps of raw material treatment, weighing 100 parts by weight of cherry fruits, soaking the cherry fruits in a sodium bicarbonate solution with the practical mass concentration of 3% for 3 minutes, washing the cherry fruits with an acetic acid solution with the mass concentration of 1%, finally washing the cherry fruits with deionized water, and grinding the cherry fruits with a colloid mill for later use.
S2: extracting, namely adding 50 parts by weight of a pretreating agent into the fruit pulp, wherein the pretreating agent comprises 10% of cellulase, 10% of pectinase, 2% of an enzyme activator, 1% of a pH regulator, 1% of a protective agent and 75% of deionized water, then adding 30 parts by weight of a prepared oxalic acid solution with the mass concentration of 5%, and then placing the mixture into a circulating ultrasonic extraction device for extraction, wherein the ultrasonic frequency is 50HZ, the extraction temperature is 28 ℃, and the extraction time is 40min, so as to obtain an extracting solution. The protective agent in the pretreating agent comprises 2% of natural antibacterial extracting agent, 0.5% of rosemary extract, 0.1% of tert-butyl hydroquinone, 1% of tea polyphenol and 96.4% of deionized water. The natural antibacterial extractant is herba Portulacae extractive solution.
S3: filtering, namely a, adding the extracting solution into a centrifugal machine for centrifugal separation, and removing precipitates to obtain a first filtrate;
b. then filtering the first filtrate by a hollow fiber filter membrane to obtain a second filtrate;
c. and then filtering the second filtrate by an ultrafiltration membrane to obtain a third filtrate. (ii) a
S4: molecular distillation, namely adding the third filtrate into molecular distillation equipment for molecular distillation treatment to obtain a fraction containing vitamins;
s5: and (4) carrying out freeze vacuum drying on the fraction to obtain the natural vitamin.
The difference between the examples 2-5 and the example 1 is that the cherry fruit, the pretreating agent and the extracting agent are respectively calculated according to the parts by weight in the following table.
Examples | Cherry fruit | Pretreating agent | Extraction agent |
Example 2 | 125 | 62.5 | 37.5 |
Example 3 | 150 | 75 | 45 |
Example 4 | 175 | 87.5 | 52.5 |
Example 5 | 200 | 100 | 60 |
Examples 6 to 9 are different from example 1 in that the pretreatment agent comprises the following components in percentage by weight.
The difference between the examples 10-13 and the example 1 is that the components in the protective agent are in the following table in percentage by weight.
Examples 14 to 18 differ from example 1 in that the components of the natural antibacterial extractant are in the following table in proportion.
Examples | Purslane extract | Radish extract | Honeysuckle extract |
Example 14 | 0 | 1 | 0 |
Example 15 | 0 | 0 | 1 |
Example 16 | 1 | 1 | 1 |
Example 17 | 1 | 1 | 0 |
Example 18 | 0.5 | 0.5 | 1 |
Examples 19 to 23 differ from example 1 in that the components in the extractant were as follows in terms of mass concentration.
Examples | Oxalic acid solution | Phosphoric acid solution |
Example 19 | 1% | 1% |
Example 20 | 2% | 3% |
Example 21 | 0% | 5% |
Example 22 | 3% | 4% |
Example 23 | 4% | 5% |
Examples 24 to 27 differ from example 1 in that the baking soda concentration, the soaking time, and the acetic acid concentration in step S1 are shown in the following table.
Examples | Concentration of sodium bicarbonate | Soaking time | Concentration of acetic acid |
Example 24 | 3.5 | 4.25 | 0.625 |
Example 25 | 4 | 5.5 | 0.75 |
Example 26 | 4.5 | 6.75 | 0.875 |
Example 27 | 5 | 8 | 1 |
Examples 28 to 31 are different from example 1 in that the ultrasonic frequency, the extraction temperature and the extraction time in the extraction process of step S2 are shown in the following table.
Examples | Ultrasonic frequency | Temperature of extraction | Extraction time |
Example 28 | 42.5 | 24.25 | 45 |
Example 29 | 45 | 25.5 | 50 |
Example 30 | 47.5 | 26.75 | 55 |
Example 31 | 50 | 28 | 60 |
Comparative example
Comparative example 1 differs from example 1 in that: the extraction process of step S2 is: adding 95% ethanol into the pulp, and extracting in ultrasonic extraction equipment at ultrasonic frequency of 50HZ and extraction temperature of 28 deg.C for 40min to obtain extractive solution.
Comparative example 2 is different from example 1 in that a protecting agent is not added to the pretreating agent;
comparative example 3 is different from example 1 in that a pretreating agent was not used in step S2.
Detection method
Vitamin content test
The test method comprises the following steps: 10ml of the finished natural vitamin of example 1, comparative example 1 and comparative example 3 was accurately taken out into a 250ml conical flask, then 100ml of distilled water, 10ml of HAc and 5ml of 0.5% starch indicator which were freshly boiled and cooled to room temperature were added, and immediately titrated with an iodine standard solution until the solution showed a stable blue color and remained unchanged for 30 seconds, that is, the titration endpoint was reached, titration was carried out in parallel three times, and then the vitamin C content was calculated. The concentration of the iodine standard solution was 0.05mol L-1。
Group of | Average content of vitamin C |
Example 1 | 54% |
Comparative example 1 | 37% |
Comparative example 3 | 42% |
And (4) conclusion: as can be seen from the above table, the comparison result between example 1 and comparative example 1 shows that the content of vitamin C in the finished product prepared by the process of the present invention in example 1 is significantly higher than that in the finished product extracted by ethanol in the conventional process in comparative example 1, and the comparison between example 1 and comparative example 3 shows that the addition of the pretreatment agent can make the leaching of vitamin in cherry pulp more complete and improve the yield of vitamin.
Antibacterial and bacteriostatic test
The test method comprises the following steps: inoculating test bacteria (Staphylococcus aureus) on agar culture medium, dripping into center to extract vitamin, culturing at 37 deg.C for 24 hr, and observing the reproduction condition of bacteria and halo size in aseptic area around the sample with magnifier. The width of the stop band is increased from 1 level to 10 levels in sequence. The width of the stop band represents the magnitude of the antimicrobial efficacy.
A conclusion is drawn; according to the above table, the width of the blocking tape in the embodiment 1 is obviously larger than that in the comparative examples 1-3, and the width of the blocking tape represents the antibacterial capacity of the reagent, so that the vitamin prepared by the invention has stronger antibacterial capacity, and the antibacterial and bacteriostatic components in the protective agent play an antibacterial and bacteriostatic role on the vitamin.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (3)
1. The preparation method of the natural vitamins in the cherry is characterized by comprising the following steps: the method comprises the following steps:
s1: processing raw materials, namely weighing 100-200 parts by weight of cherry fruits, and then crushing the cherry fruits to obtain fruit pulp for later use;
s2: extracting, namely adding 50-100 parts by weight of a pretreating agent into the fruit pulp, then adding 30-60 parts by weight of a prepared extracting agent solution, and then placing the mixture into circulating ultrasonic extraction equipment for extraction to obtain an extracting solution;
s3: filtering, and filtering and separating the extracting solution for multiple times to obtain filtrate; the multiple filtering in step S3 specifically includes the following steps:
a. adding the extracting solution into a centrifugal machine for centrifugal separation, and removing precipitates to obtain a first filtrate;
b. then filtering the first filtrate by a hollow fiber filter membrane to obtain a second filtrate;
c. then filtering the second filtrate by an ultrafiltration membrane to obtain a third filtrate;
s4: molecular distillation, namely adding the third filtrate into molecular distillation equipment for molecular distillation treatment to obtain a fraction containing vitamins;
s5: freeze vacuum drying the fraction to obtain natural vitamins;
the pretreating agent comprises the following components in percentage by weight:
10-20% of cellulase;
5-10% of pectinase;
2-5% of an enzyme activator;
1-3% of a pH regulator;
65-80% of deionized water;
the pretreatment agent is also added with a protective agent with the weight percentage of 1-3%, and the protective agent comprises the following components in percentage by weight:
2-5% of a natural antibacterial extracting agent;
0.5-1% of rosemary extract;
0.1-1% of tert-butyl hydroquinone;
1-2% of tea polyphenol;
the balance of deionized water;
the natural antibacterial extractant is selected from one or more of purslane extract, radish extract and honeysuckle extract;
the extractant is oxalic acid solution with the mass concentration of 1-5%, phosphoric acid solution with the mass concentration of 1-5% or mixed solution of the two.
2. The method for preparing natural vitamins in cherries according to claim 1, wherein the natural vitamins comprise: the crushing process in the step S1 specifically operates as follows:
firstly, soaking cherry fruits in a baking soda solution with the practical mass concentration of 3-5% for 3-8 minutes, then washing with an acetic acid solution with the mass concentration of 0.5-1%, finally washing with deionized water, and then grinding into fruit pulp by using a colloid mill.
3. The method for preparing natural vitamins in cherries according to claim 1, wherein the natural vitamins comprise: and in the step S2, the ultrasonic frequency is 40-50 HZ, the extraction temperature is 23-28 ℃, and the extraction time is 40-60 min.
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