CN109053668B - Method for preparing ester catechin from tea polyphenol - Google Patents
Method for preparing ester catechin from tea polyphenol Download PDFInfo
- Publication number
- CN109053668B CN109053668B CN201810827716.7A CN201810827716A CN109053668B CN 109053668 B CN109053668 B CN 109053668B CN 201810827716 A CN201810827716 A CN 201810827716A CN 109053668 B CN109053668 B CN 109053668B
- Authority
- CN
- China
- Prior art keywords
- tea polyphenol
- cooling
- catechin
- temperature
- speed
- 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
Images
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
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyrane Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for preparing ester catechin by using tea polyphenol, belonging to the technical field of separation and extraction. The method comprises the steps of adding purified water with the temperature of 60-80 ℃ into tea polyphenol, stirring and dissolving until the solid content is 20% +/-5%; then cooling to 25 +/-5 ℃ at the speed of 15 +/-5 ℃/h, then cooling to 0-5 ℃ at the speed of 5-10 ℃/h, standing for 0.5-2 h, and obtaining a supernatant (I) and a lower precipitate (I); adding purified water with the temperature of 60-80 ℃ into the lower-layer sediment, stirring and dissolving until the solid content is 20% +/-5%, and repeatedly cooling and precipitating to obtain an upper-layer clear liquid and a lower-layer sediment; drying the lower layer precipitate under reduced pressure to obtain ester type catechin. The invention utilizes a cooling precipitation method to well separate ester catechin from other components in tea polyphenol, does not use any organic solvent, and is environment-friendly, green, safe and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of separation and extraction, and particularly relates to a method for preparing ester catechin by using tea polyphenol.
Background
Tea polyphenol is a general name of a complex of more than 30 kinds of polyhydroxy phenolic compounds extracted from tea leaves, is acidic, is also called tea tannin or tea tannin, and is a main component forming tea liquor color, taste and tea health care function. Generally, the polyphenols in tea comprise 10-35% (w/w) of the dry weight of tea, including flavanols, flavones and flavonols, anthocyanins and anthocyanins, and phenolic acids and depsides, wherein catechin is the main component of tea polyphenols, and accounts for about 80-90% of the total weight of tea polyphenols.
Tea polyphenol as a novel natural food antioxidant has higher activity than the currently used chemically synthesized antioxidants, such as BBA (butyl hydroxy anisole) and BHT (dibutyl hydroxy toluene), is listed as a national food standard in 1991 in China, and also has pharmacological functions of resisting cancer, inhibiting bacteria, killing bacteria, removing free radicals of a human body, resisting aging, resisting radiation, reducing blood sugar and blood fat, enhancing the toughness of microvessels and the like. Has wide application prospect in the fields of grease, food, medicine, daily chemical and the like.
The tea polyphenol is widely applied in the fields of biological medicine, food industry, daily chemical industry, grease and environmental protection, and has the most remarkable characteristics of oxidation resistance and high-efficiency free radical scavenging capability, which is determined by the main component catechin of the tea polyphenol to a great extent. Modern scientific research shows that catechin, a main compound of tea polyphenol, is an ideal natural antioxidant and a valuable natural medicine raw material. Has strong capability of inhibiting the growth of mould, and is mainly used for the antioxidation and fresh-keeping of grease-containing foods, such as meat, fish, flour foods, edible vegetable oil, animal oil and the like. The health food produced by using tea polyphenol as raw material can eliminate excessive free radical in vivo in time, raise SOD activity in vivo and enhance autoimmune capacity, so that it has several functions of resisting senility, resisting cancer, etc. Along with the enhancement of health care consciousness of people, carcinogenic suspicion is generated on artificially synthesized antioxidants BBA, BHT and the like, and the oxidation resistance of tea polyphenol and catechin is stronger than that of the two compositions, so that the tea polyphenol and the catechin have better safety performance and no side effect.
The catechin mainly comprises seven components: EGCG (epigallocatechin gallate), ECG (epicatechin gallate), GCG (gallocatechin gallate), EGC (epigallocatechin), GC (gallocatechin), EC (epicatechin), C (catechin). Wherein EGCG, ECG and GCG are ester catechin, and EGC, GC, EC and C are simple catechin. With the progress of scientific research, people find that ester-type catechin plays an important role in pharmacological drug effects such as oxidation resistance, tumor resistance, cardiovascular disease resistance, cancer prevention, radiation protection and the like, so EGCG (epigallocatechin gallate), ECG (epicatechin gallate) and GCG (gallocatechin gallate) which play a main role in catechin are more concerned. The ester catechin accounts for about 85% of total catechin, contains most EGCG and ECG, and is effective component with anticancer effect.
The main methods for preparing ester catechin commonly used at present comprise: resin column chromatography. The general process comprises the steps of dissolving, diluting, loading on a column, gradient ethanol elution, concentration and recovery of an ethanol solvent and drying, and is relatively complex, long in production period, high in cost (resin is high in price and has a certain service life, and the ethanol recovery loss is large), high in energy consumption (the ethanol solvent is concentrated and recovered), and low in yield (the general elution rate is about 90%). Therefore, how to overcome the defects of the prior art is an urgent problem to be solved in the technical field of separation and extraction at present.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a method for preparing ester catechin by using tea polyphenol.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing ester catechin with tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: adding purified water with the temperature of 60-80 ℃ into the tea polyphenol, stirring and dissolving until the solid content is 20% +/-5%; then cooling to 25 +/-5 ℃ at the speed of 15 +/-5 ℃/h, then cooling to 0-5 ℃ at the speed of 5-10 ℃/h, standing for 0.5-2 h, and obtaining a supernatant (I) and a lower precipitate (I);
step (2), secondary cooling precipitation: adding purified water at 60-80 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20% + -5%, then cooling to 25 + -5 ℃ at the speed of 15 + -5 ℃/h, then cooling to 0-5 ℃ at the speed of 5-10 ℃/h, standing for 0.5-2 h, and obtaining supernatant and the lower-layer precipitate;
and (3) drying under reduced pressure: and (3) drying the lower-layer precipitate obtained in the step (2) under reduced pressure to obtain ester type catechin.
Further, it is preferable that the supernatant liquid (i) and the supernatant liquid (ii) are combined, concentrated and dried to obtain a tea polyphenol product mainly comprising simple catechins.
Further, it is preferable that the temperature of the purified water in the steps (1) and (2) is 70 ℃.
Further, it is preferable that, in the step (1), purified water of 60 to 80 ℃ is added to tea polyphenol and dissolved with stirring until the solid content becomes 20%.
Further, it is preferable that in the step (1) and the step (2), the temperature is decreased from 60 ℃ to 80 ℃ to 25. + -. 5 ℃ at a rate of 15 ℃/h.
Further, it is preferred that in the step (1) and the step (2), the temperature is decreased from 60 ℃ to 80 ℃ to 25 ℃ at a rate of 15. + -. 5 ℃/h.
Further, in the step (1) and the step (2), the temperature is preferably reduced from 25 +/-5 ℃ to 2 ℃ at a rate of 5-10 ℃/h.
Further, in the step (1) and the step (2), the temperature is preferably reduced from 25 +/-5 ℃ to 0-5 ℃ at a rate of 8 ℃/h.
Further, in the step (3), the temperature of the reduced pressure drying is preferably 60-75 ℃, and the vacuum degree is more than or equal to 0.075 Mpa.
Further, in the step (3), the temperature for drying under reduced pressure is preferably 65 ℃.
The primary and secondary cooling precipitation of the invention is cooling according to gradient: the first stage is to reduce the temperature to 25 +/-5 ℃ (room temperature), and the second stage is to reduce the temperature to 0-5 ℃; the optimal parameters of the step are as follows:
1. adding purified water at 70 deg.C, too low, below 60 deg.C, and dissolving to a proper concentration (20% +/-5%); too high, above 80 ℃, the oxidative degradation of the compounds is greatly increased; if normal temperature water is added and heated to the dissolving temperature (70 ℃), the required time is long, and the oxidative degradation is greatly increased;
2. the solid content concentration is preferably 20 percent; too low, below 15%, insufficient settling (low yield); too high, higher than 25%, the rest components are increased in sedimentation, and the precipitation purity is low;
3. the first stage of temperature reduction (to 25 +/-5 ℃): the cooling rate is preferably 15 ℃/h. The temperature is reduced too fast, the temperature exceeds 20 ℃/h, the sedimentation is too fast, the wrapped sedimentation of other components is increased, and the sedimentation purity is reduced; too slow, less than 10 ℃/h, low efficiency and long production cycle.
4. And (3) cooling in the second stage (to 0-5 ℃): the cooling rate is preferably 8 ℃/h, and the temperature is preferably reduced to 2 ℃; the cooling speed is too fast, the temperature exceeds 10 ℃/h, the viscosity is increased too fast, the sedimentation is not enough, and the sedimentation is not sufficient; too slow, below 5 ℃/h, the efficiency is low.
The invention is divided into two gradient cooling: the temperature reduction rate of the first stage is higher than that of the second stage, the temperature of the first stage is higher than room temperature, and the viscosity of the solution is slowly increased, so the temperature reduction rate can be higher; and in the second stage, the solution viscosity is increased more quickly and the cooling rate is slower, so that the ester-type catechins have sufficient time to settle, and the excessive viscosity increase caused by cooling is offset.
The steps of secondary cooling precipitation and the optimal parameters are completely consistent with those of primary cooling precipitation.
The invention adopts temperature reduction chromatography, which realizes separation by utilizing the solubility and the component proportion difference among separated components:
The temperature-reducing chromatography process of the invention can be carried out
Compared with the prior art, the invention has the beneficial effects that:
(1) after the tea polyphenol is dissolved in water, the separation is realized by utilizing the solubility and the component proportion difference among the separated components, and the product is not contacted with any organic toxic solvent, so that the product is green, safe and environment-friendly;
(2) no organic solvent or resin is used, the product is safe, the cost is low, no adsorption and desorption process is adopted, the product is free of loss, and the yield is high;
(3) simple process and short production period.
Drawings
FIG. 1 is a schematic flow chart of the process for preparing ester type catechin using tea polyphenol according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
Example 1
A method for preparing ester catechin from tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: weighing 1.20Kg of tea polyphenol (the content of ester catechin is 78.52%), adding 6.8Kg of purified water at 70 ℃, stirring and dissolving, wherein the content of solid is 20%, cooling to 25 ℃ at the speed of 15 ℃/h, then cooling to 2 ℃ at the speed of 8 ℃/h, standing for 0.5h, and obtaining a supernatant (I) and a lower precipitate (I);
step (2), secondary cooling precipitation: adding purified water of 70 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20%, cooling to 25 ℃ at the speed of 15 ℃/h, then cooling to 2 ℃ at the speed of 8 ℃/h, standing for 0.5h, and obtaining a supernatant and a lower-layer precipitate;
and (3) drying under reduced pressure: and (3) decompressing and drying the lower-layer precipitate obtained in the step (2) to obtain 938g of ester type catechin, 3.51 percent of water and 99.12 percent of product content in terms of dry products. And combining the supernatant I and the supernatant II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Example 2
A method for preparing ester catechin with tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: weighing 1.20Kg of tea polyphenol (the content of ester catechin is 78.52%), adding 6.8Kg of purified water at 70 ℃, stirring for dissolving, wherein the content of solid is 20%, then cooling to 25 ℃ at the rate of 20 ℃/h, then cooling to 2 ℃ at the rate of 10 ℃/h, standing for 0.5h, and obtaining a supernatant I and a lower precipitate I;
step (2), secondary cooling precipitation: adding purified water at 70 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20%, then cooling to 25 ℃ at the rate of 20 ℃/h, then cooling to 2 ℃ at the rate of 10 ℃/h, and standing for 0.5h to obtain upper-layer clear liquid and lower-layer precipitate;
and (3) drying under reduced pressure: and (3) decompressing and drying the lower-layer precipitate obtained in the step (2) to obtain 945g of ester-type catechin, wherein the water content is 4.28 percent, and the product content is 98.27 percent calculated by dry products. And combining the supernatant I and the supernatant II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Example 3
A method for preparing ester catechin from tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: weighing 1.20Kg of tea polyphenol (the content of ester type catechin is 78.52%), adding 6.8Kg of purified water at 70 ℃, stirring and dissolving until the solid content is 20%, then cooling to 25 ℃ at the speed of 10 ℃/h, then cooling to 2 ℃ at the speed of 5 ℃/h, standing for 0.5h, and obtaining a supernatant (i) and a lower precipitate (i);
step (2), secondary cooling precipitation: adding purified water at 70 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20%, then cooling to 25 ℃ at the speed of 10 ℃/h, then cooling to 2 ℃ at the speed of 5 ℃/h, and standing for 0.5h to obtain upper-layer clear liquid and lower-layer precipitate;
and (3) drying under reduced pressure: decompressing and drying the lower-layer precipitate obtained in the step (2), wherein the decompressing and drying temperature is 60 ℃, and the vacuum degree is more than or equal to 0.075Mpa, so that 934g of ester type catechin is obtained, the water content is 2.53%, and the product content is 99.45% in terms of dry products. And combining the supernatant liquid I and the supernatant liquid II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Example 4
A method for preparing ester catechin from tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: adding purified water of 60 ℃ into tea polyphenol, stirring and dissolving until the solid content is 15%; then cooling to 20 ℃ at the speed of 10 ℃/h, then cooling to 0 ℃ at the speed of 5 ℃/h, and standing for 0.5h to obtain a supernatant (I) and a lower precipitate (I);
step (2), secondary cooling precipitation: adding purified water with the temperature of 60 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 15%, then cooling to 20 ℃ at the speed of 10 ℃/h, then cooling to 0 ℃ at the speed of 5 ℃/h, standing for 0.5h, and obtaining upper-layer clear liquid and lower-layer precipitate;
and (3) drying under reduced pressure: and (3) drying the lower-layer precipitate obtained in the step (2) under reduced pressure to obtain ester type catechin. And combining the supernatant liquid I and the supernatant liquid II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Wherein the reduced pressure drying temperature is 60 deg.C, and the vacuum degree is not less than 0.075Mpa
Example 5
A method for preparing ester catechin with tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: adding purified water of 80 ℃ into tea polyphenol, stirring and dissolving until the solid content is 25%; then cooling to 30 ℃ at the rate of 20 ℃/h, then cooling to 5 ℃ at the rate of 10 ℃/h, and standing for 0.5-2 h to obtain a supernatant I and a lower precipitate I;
step (2), secondary cooling precipitation: adding purified water at 80 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 25%, then cooling to 30 ℃ at the rate of 20 ℃/h, then cooling to 5 ℃ at the rate of 10 ℃/h, standing for 2h, and obtaining an upper-layer clear solution and a lower-layer precipitate;
and (3) drying under reduced pressure: and (3) drying the lower-layer precipitate obtained in the step (2) under reduced pressure to obtain ester type catechin. And combining the supernatant liquid I and the supernatant liquid II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Wherein the reduced pressure drying temperature is 75 deg.C, and the vacuum degree is not less than 0.075Mpa
Example 6
A method for preparing ester catechin from tea polyphenols comprises the following steps:
step (1), primary cooling precipitation: adding purified water of 70 ℃ into tea polyphenol, stirring and dissolving until the solid content is 20%; then cooling to 25 ℃ at the rate of 15 ℃/h, then cooling to 2 ℃ at the rate of 8 ℃/h, and standing for 1h to obtain a supernatant (I) and a lower precipitate (I);
step (2), secondary cooling precipitation: adding purified water at 70 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20%, then cooling to 25 ℃ at the rate of 15 ℃/h, then cooling to 2 ℃ at the rate of 8 ℃/h, standing for 1h, and obtaining an upper-layer clear solution and a lower-layer precipitate;
and (3) drying under reduced pressure: and (3) drying the lower-layer precipitate obtained in the step (2) under reduced pressure to obtain ester catechin. And combining the supernatant liquid I and the supernatant liquid II, concentrating and drying to obtain the tea polyphenol product mainly containing simple catechin.
Wherein the reduced pressure drying temperature is 65 deg.C, and the vacuum degree is 0.08Mpa
Comparative example 1
The same procedures as in example 1 were repeated except that the solid content of the solution was 10%, to obtain 896g of ester-type catechin, which had a water content of 6.19% and a product content of 99.28% on a dry basis.
Comparative example 2
Compared with the embodiments 1, 2 and 3, the difference is that: the solid content of the solution is 10%, the temperature is reduced in a gradient manner (the temperature is reduced from 70 ℃ to 25 ℃ at a speed of 25 ℃/h in the first stage, the temperature is reduced from 25 ℃ to 2 ℃ at a speed of 15 ℃/h in the second stage), and the rest parameters and steps are completely the same, so that 923g of ester catechin, 5.42% of water and 96.74% of product content in terms of dry products are obtained.
Comparative example 3
Compared with the embodiments 1, 2 and 3, the difference is that: the solid content of the solution is 10 percent, the temperature is reduced in a gradient way (the temperature is reduced from 70 ℃ to 25 ℃ at the rate of 5 ℃/h in the first stage, the temperature is reduced from 25 ℃ to 2 ℃ at the rate of 2 ℃/h in the second stage), the rest parameters and steps are completely the same, and 918g of ester catechin, 3.87 percent of water and 99.68 percent of product content in terms of dry products are obtained.
Comparative example 4
The procedure was exactly the same as in example 1 except that the solid content of the solution was 30%, to obtain 956g of ester-type catechin, which had a water content of 4.63% and a product content of 96.59% on a dry basis.
Comparative example 5
Compared with the embodiments 1, 2 and 3, the difference is that: the solid content of the solution is 30 percent, the temperature is reduced in a gradient way (the temperature is reduced from 70 ℃ to 25 ℃ at the speed of 25 ℃/h in the first stage, the temperature is reduced from 25 ℃ to 2 ℃ at the speed of 15 ℃/h in the second stage), and the rest parameters and steps are completely the same, so that 943g of ester catechin, 3.91 percent of water and 92.77 percent of product content in terms of dry products are obtained.
Comparative example 6
Compared with the embodiments 1, 2 and 3, the difference is that: the solid content of the solution is 30 percent, the temperature is reduced in a gradient way (the temperature is reduced from 70 ℃ to 25 ℃ at the rate of 5 ℃/h in the first stage, the temperature is reduced from 25 ℃ to 2 ℃ at the rate of 2 ℃/h in the second stage), the rest parameters and steps are completely the same, 983g of ester catechin is obtained, the water content is 7.23 percent, and the product content is 97.85 percent calculated by dry products.
Measuring ester catechin content by High Performance Liquid Chromatography (HPLC), calculating product yield and purity, and recording cooling precipitation time of examples and comparative examples, the results are shown in Table 1.
Comprehensively considering the product yield, the purity and the production period, the solid content of the solution is preferably 20 +/-5 percent, preferably 20 percent, and the temperature is reduced in a gradient way: the cooling rate of the first stage is preferably 15 +/-5 ℃/h, preferably 15 ℃/h; in the second stage, the temperature is preferably 5-10 ℃/h, and more preferably 8 ℃/h.
Wherein, the product yield is% = [ (the mass of the dried ester catechin product x the content of the dried ester catechin%)/(the mass of the tea polyphenol raw material x the content of the ester catechin) ] × 100%.
From table 1, it can be seen that the results of examples 1 to 3 of the present invention are better than those of the comparative examples, and show that the parameters and steps of the present invention have good synergistic effects.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for preparing ester catechin by using tea polyphenol is characterized by comprising the following steps:
step (1), primary cooling precipitation: adding purified water with the temperature of 60-80 ℃ into tea polyphenol, stirring and dissolving until the solid content is 20% +/-5%; then cooling to 25 +/-5 ℃ at the speed of 15 +/-5 ℃/h, then cooling to 0-5 ℃ at the speed of 5-10 ℃/h, standing for 0.5-2 h, and obtaining a supernatant (I) and a lower precipitate (I);
step (2), secondary cooling precipitation: adding purified water at 60-80 ℃ into the lower-layer precipitate obtained in the step (1), stirring and dissolving until the solid content is 20% + -5%, then cooling to 25 + -5 ℃ at the speed of 15 + -5 ℃/h, then cooling to 0-5 ℃ at the speed of 5-10 ℃/h, standing for 0.5-2 h, and obtaining supernatant and the lower-layer precipitate;
and (3) drying under reduced pressure: decompressing and drying the lower-layer precipitate obtained in the step (2) to obtain ester type catechin; the temperature for decompression drying is 60-75 ℃, and the vacuum degree is more than or equal to 0.075 Mpa.
2. The method of claim 1, wherein the supernatant (i) and the supernatant (ii) are combined, concentrated and dried to obtain a tea polyphenol product mainly comprising simple catechins.
3. The method for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein the purified water temperature is 70 ℃ in the step (1) and the step (2).
4. The method for preparing ester-type catechin using tea polyphenol according to claim 1, wherein in the step (1), purified water of 60 to 80 ℃ is added to tea polyphenol and dissolved with stirring until the solid content is 20%.
5. The method for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein in the step (1) and the step (2), the temperature is decreased from 60 ℃ to 80 ℃ to 25 ± 5 ℃ at a rate of 15 ℃/h.
6. The method for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein in the step (1) and the step (2), the temperature is decreased from 60 ℃ to 80 ℃ to 25 ℃ at a rate of 15 ± 5 ℃/h.
7. The method for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein in the step (1) and the step (2), the temperature is decreased from 25 ± 5 ℃ to 2 ℃ at a rate of 5-10 ℃/h.
8. The method for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein in the step (1) and the step (2), the temperature is decreased from 25 ± 5 ℃ to 0-5 ℃ at a rate of 8 ℃/h.
9. The process for preparing ester catechin using tea polyphenol as claimed in claim 1, wherein the temperature of reduced pressure drying in step (3) is 65 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810827716.7A CN109053668B (en) | 2018-07-25 | 2018-07-25 | Method for preparing ester catechin from tea polyphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810827716.7A CN109053668B (en) | 2018-07-25 | 2018-07-25 | Method for preparing ester catechin from tea polyphenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109053668A CN109053668A (en) | 2018-12-21 |
| CN109053668B true CN109053668B (en) | 2022-07-26 |
Family
ID=64835543
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810827716.7A Active CN109053668B (en) | 2018-07-25 | 2018-07-25 | Method for preparing ester catechin from tea polyphenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109053668B (en) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1193994C (en) * | 2002-06-21 | 2005-03-23 | 浙江大学 | Method for purifying monomer of epigallocatechingallate (EGCG) |
| CN1212319C (en) * | 2002-07-23 | 2005-07-27 | 浙江海正药业股份有限公司 | Epi-nutgall catechin gallic acid ester monomer purifying process |
| WO2007041891A1 (en) * | 2005-10-08 | 2007-04-19 | The Hong Kong Polytechnic University | Methods of separating catechins from green tea leaves |
| CN102240343B (en) * | 2011-05-23 | 2013-01-23 | 中国农业科学院茶叶研究所 | Environment-friendly preparation method for high-ester catechin tea polyphenol |
| CN103613575B (en) * | 2013-11-29 | 2016-05-25 | 桂林莱茵生物科技股份有限公司 | The method of purification of a kind of high-load EGCG |
| CN106946837A (en) * | 2017-03-17 | 2017-07-14 | 宁波金昉生物科技有限公司 | The method that ester catechin is separated from green tea |
-
2018
- 2018-07-25 CN CN201810827716.7A patent/CN109053668B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN109053668A (en) | 2018-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101773593B (en) | Method for preparing antioxidative active extractive of sweet potato leaves | |
| CN103992359A (en) | Preparation process for extracting green tea polyphenols from tea | |
| CN102579511A (en) | Method for integrally extracting steroidal compounds, polysaccharides and polyphenols from inonotus obliquus | |
| CN101392008A (en) | Extraction technique of high-purity phlorizin | |
| CN105294632A (en) | Industrial method for preparing lonicera caerulea fruit anthocyanidin from lonicera caerulea fruits | |
| JP3808494B2 (en) | Method for producing high content of proanthocyanidins | |
| CN101366427B (en) | Processing method for cold instant white tea powder | |
| JP2007135481A (en) | Proanthocyanidin-containing tea beverage and method for producing the same | |
| CN109053668B (en) | Method for preparing ester catechin from tea polyphenol | |
| CN103524521A (en) | Preparation method of blackberry ellagic acid | |
| JP4702824B2 (en) | Tea polyphenol composition and method for producing the same | |
| CN103720913B (en) | Method for extracting tea polyphenol from tea leaves by combination of metal ion complexing precipitation and column chromatography | |
| CN108576652B (en) | A method for producing dried meat slice rich in plant polyphenol by use of Mori fructus polyphenol crystal and Mori fructus polyphenol microcapsule, and the prepared dried meat slice | |
| CN105294633A (en) | Industrial method for preparing vaccinium vitis idaea anthocyanidin from vaccinium vitis idaea | |
| JP2009082079A (en) | Functional food composition | |
| JPH07238078A (en) | Purification method of polyphenolic compound | |
| CN114230542A (en) | Method for extracting EGCG from fresh tea leaves | |
| CN105524035A (en) | Manufacturing method of mulberry anthocyanidin | |
| CN112574161A (en) | Preparation method of EGC-rich non-ester tea polyphenol | |
| CN113041306A (en) | Preparation and purification method of tea polyphenol and application of tea polyphenol in weight-reducing products | |
| CN111534366A (en) | Method for preparing oat bran oil rich in polyphenol by using naked oat bran as raw material | |
| CN115844938B (en) | Artemisia sphaerocephala total flavone and preparation method and application thereof | |
| CN110923053A (en) | Method for extracting tea oil with high freezing resistance | |
| CN111675684B (en) | Method for extracting procyanidine from mulberry fruits | |
| CN110256505B (en) | Primary separated matter of common sow thistle alkaloid and separation method and application thereof |
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 | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 666104 Daganba village group of Daganba village committee, dadugang Township, Jinghong City, Xishuangbanna Dai Autonomous Prefecture, Yunnan Province Applicant after: Manchangge tea industry (Xishuangbanna) Co.,Ltd. Address before: 666104 Daganba village group of Daganba village committee, dadugang Township, Jinghong City, Xishuangbanna Dai Autonomous Prefecture, Yunnan Province Applicant before: YUNNAN CHANONG BIOLOGICAL INDUSTRY Co.,Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |