CN109053668A - A method of ester catechin is prepared with tea polyphenols - Google Patents
A method of ester catechin is prepared with tea polyphenols Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of methods for preparing ester catechin with tea polyphenols, belong to separation and extraction technology field.This method is into tea polyphenols plus 60 DEG C~80 DEG C purified waters and stirring and dissolving to solid content are 20% ± 5%；After being cooled to 25 ± 5 DEG C later with 15 ± 5 DEG C/h rate, then with 5~10 DEG C/h, rate of temperature fall is down to 0~5 DEG C, stands 0.5~2h, obtain supernatant liquor 1. with lower sediment 1.；It is 20% ± 5% that 60 DEG C~80 DEG C purified waters and stirring and dissolving to solid content are 1. added to lower sediment, repeats the precipitating that cools down, obtain supernatant liquor 2. with lower sediment 2.；2. lower sediment is dried under reduced pressure, ester catechin is obtained.The present invention is separated ester catechin in tea polyphenols with remaining component using cooling precipitation method very well, environmentally friendly not using any organic solvent, Product Green, safe and environment-friendly.
Description
Technical field
The invention belongs to separation and extraction technology fields, and in particular to a method of ester catechin is prepared with tea polyphenols.
Background technique
Tea polyphenols are the general names of more than the 30 kinds of Polyhydroxy phenol complexs extracted from tealeaves, show acidity, also known as
Tea tannin or tea tannin are the main components to form tealeaves soup look, taste and tea health-care function.In general, in tealeaves
Polyphenols account for 10%~35%(w/w of dry weight of tea leaves), including based on catechin flavanols, flavones and flavonols,
Anthocyanidin and leucoanthocyanidin and phenolic acid and depside, wherein catechin is the bulk composition of tea polyphenols, accounts for about tea polyphenols total amount
80%~90%.
Tea polyphenols are higher than chemical synthesis antioxidant used at present as novel natural food antioxidant, activity,
Such as BBA(butylated hydroxy anisole), BHT(dibutyl hydroxy toluene), China in 1991 by tea polyphenols be included in food country
Standard, tea polyphenols also have anticancer, restraining and sterilizing bacteria, removing human free radical, anti-aging, anti-radiation, reducing blood sugar and blood lipid, enhancing micro-
The pharmacological functions such as blood vessel obdurability.It has broad application prospects in fields such as grease, food, medicine, daily use chemicals.
Tea polyphenols are widely applied in biological medicine, food industry, daily-use chemical industry, grease and field of environment protection, most aobvious
The characteristics of work is that have anti-oxidant, the efficient ability for removing free radical, this is largely the bulk composition by tea polyphenols
What catechin determined.Modern scientific research shows the host compound of tea polyphenols --- catechin is both ideal natural antioxygen
Agent, and be a kind of extremely valuable natural drug raw material.Have fungus growth compared with high inhibition ability, is mainly used for containing grease
The antioxygen of food is fresh-keeping, such as meat, fish, cereal preparation, edible vegetable oil, animal oil.It is what raw material produced with tea polyphenols
Health food can remove internal excessive free radical in time, improve internal SOD activity, enhance autoimmune ability, therefore to people
Body has the multiple functions such as anti-aging, anticancer.With the enhancing of people's health care consciousness, to artificial synthesized antioxidant BBA, BHT
Etc. producing carcinogenic suspicion, and the inoxidizability of tea polyphenols and catechin is more stronger than above two synthetic, and security performance is more
It is good, it is without side-effects.
Catechin mainly includes seven components: EGCG(Epigallo-catechin gallate (EGCG)), ECG(epicatechin do not have
Infanticide acid esters), GCG(nutgall catechin gallic acid ester), EGC(epigallocatechin), GC(nutgall catechin), EC
(epicatechin), C(catechin).Wherein EGCG, ECG, GCG are ester catechin, and EGC, GC, EC, C are simple catechin.With
Going deep into for scientific research, it has been found that ester catechin is in anti-oxidant, antitumor, anti-cardiovascular disease, anti-cancer, radiation protection etc.
It plays and plays an important role in pharmacological effect, therefore to the EGCG(epigallocatechin galla turcica to play a major role in catechin
Acid esters), ECG(L-Epicatechin gallate), GCG(nutgall catechin gallic acid ester) more pay close attention to.Ester catechin
Account for about 85% or so of catechin total amount, wherein the content with EGCG, ECG is most, and they are the effective component of great anticancer.
The currently used ester catechin main method for preparing: resin column chromatography.General technology be dissolution, dilution, on
Column, graded ethanol elution, concentration and recovery alcohol solvent, drying, technique versus busy, production cycle length, (resin price at high cost
Height, and have certain service life, ethyl alcohol recycling loss big), energy consumption high (concentration and recovery alcohol solvent), yield is low (generally washes
De- rate 90% or so).Therefore the problem of how overcome the deficiencies in the prior art is current separation and extraction technology field urgent need to resolve.
Summary of the invention
Ester catechin is prepared with tea polyphenols It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of
Method, this method are divided ester catechin in tea polyphenols and remaining component using cooling precipitation method very well (based on simple catechin)
From, any organic solvent is not used, it is environmentally friendly, it is simple process, at low cost, it is Product Green, safe and environment-friendly.
To achieve the above object, The technical solution adopted by the invention is as follows:
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: adding 60 DEG C~80 DEG C purified waters and stirring and dissolving into tea polyphenols, until solid content is 20%
±5%；It after being cooled to 25 ± 5 DEG C later with 15 ± 5 DEG C/h rate, then with 5~10 DEG C/h rate of temperature fall is down to 0~5 DEG C, stands
0.5~2h, obtain supernatant liquor 1. with lower sediment 1.；
Step (2), reducing temperature twice precipitating: 1. the lower sediment obtained to step (1) is added 60 DEG C~80 DEG C purified waters and stirs
Dissolution, until solid content is 20% ± 5%, after being cooled to 25 ± 5 DEG C later with 15 ± 5 DEG C/h rate, then with 5~10 DEG C/h cooling speed
Rate is down to 0~5 DEG C, after standing 0.5~2h, obtain supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin is obtained.
It is further preferred that being concentrated and dried, obtaining with simple catechu 1. 2. supernatant liquor merges with supernatant liquor after
Tea polyphenols product based on element.
It is further preferred that the purifying coolant-temperature gage is 70 DEG C in step (1) and step (2).
It is further preferred that adding 60 DEG C~80 DEG C purified waters into tea polyphenols, and stirring and dissolving is to admittedly in step (1)
Content is 20%.
It is further preferred that with 15 DEG C/h rate, being cooled to 25 from 60 DEG C~80 DEG C in step (1) and step (2)
±5℃。
It is further preferred that with 15 ± 5 DEG C/h rate, being cooled to from 60 DEG C~80 DEG C in step (1) and step (2)
25℃。
It is further preferred that with 5~10 DEG C/h rate, being cooled to 2 from 25 ± 5 DEG C in step (1) and step (2)
℃。
It is further preferred that with 8 DEG C/h rate, being cooled to 0~5 DEG C from 25 ± 5 DEG C in step (1) and step (2).
It is further preferred that the temperature being dried under reduced pressure is 60~75 DEG C, vacuum degree >=0.075Mpa in step (3).
It is further preferred that the temperature being dried under reduced pressure is 65 DEG C in step (3).
The present invention is primary, reducing temperature twice precipitating is according to gradient cooling: the first stage is to be down to 25 ± 5 DEG C (room temperatures), the
Two-stage is to be down to 0~5 DEG C；The optimal parameter of the step:
1, purifying coolant-temperature gage is added to be advisable with 70 DEG C, too low, is lower than 60 DEG C, is dissolved less than suitable concentration (20% ± 5%)；It is too high,
Higher than 80 DEG C, compound oxidation degradation can be greatly increased；If normal-temperature water is added, solution temperature (70 DEG C) are heated to, are needed
Time is long, and oxidative degradation can also greatly increase；
2, solids level concentration is advisable with 20%；It is too low, it is lower than 15%, sedimentation (yield is low) is insufficient；It is too high, it is higher than 25%, remaining group
Sedimentation is divided to increase, precipitating purity is low；
3, first stage cooling (being down to 25 ± 5 DEG C): rate of temperature fall is advisable with 15 DEG C/h.Cool down too fast, more than 20 DEG C/h, sedimentation
Too fast, the package sedimentation of remaining component increases, and precipitating purity reduces；Too slow, lower than 10 DEG C/h, low efficiency, the production cycle is long.
4, second stage cooling (being down to 0~5 DEG C): rate of temperature fall is advisable with 8 DEG C/h, is preferably cooled to 2 DEG C；Cooling rate
Too fast, more than 10 DEG C/h, viscosity increase is too fast, settles without enough time, and precipitating is insufficient；It is too slow, it is lower than 5 DEG C/h, efficiency
It is low.
The present invention is divided to two gradient coolings: first stage rate of temperature fall is higher than second stage, and the first stage is higher than room temperature, molten
Fluid viscosity increase is slower, therefore rate of temperature fall can be higher；Second stage is lower than room temperature, and solution viscosity increases very fast, rate of temperature fall
Should be relatively slow, it allows ester catechin to have abundant time settlement, is increased with offsetting the too fast viscosity of cooling bring.
Reducing temperature twice settling step of the present invention, optimal parameter, it is completely the same with primary cooling precipitating.
The present invention is to realize separation using solubility between separation component and component ratio difference using cooling chromatography:
Ester catechin solubility is much smaller compared with remaining component solubility, and ester catechin and remaining component ratio are larger
(about 7~8:1), therefore ester catechin is easier to reach the precipitation of over-saturation state.
Carry out second cooling precipitating 1. lower sediment is dissolved after, purpose remove 1. lower sediment wraps up it is a small amount of its
Its component, further purifies ester catechin；By dissolving precipitating twice, the ester catechin product of high-purity can be obtained.
The present invention cools down chromatography process can be
Compared with prior art, the present invention has the advantages that:
(1) after tea polyphenols are water-soluble, separation is realized using solubility between separation component and component ratio difference, is not contacted any organic
Toxic solvent, it is Product Green, safe and environment-friendly；
(2) any organic solvent and resin are not used, product safety is at low cost, and without absorption resolving, product without
Loss, high income；
(3) simple process, with short production cycle.
Detailed description of the invention
Fig. 1 is the flow diagram for the method that the present invention prepares ester catechin with tea polyphenols.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art
Or it is carried out according to product description.Production firm person is not specified in material therefor or equipment, is that can be obtained by purchase
Conventional products.
Embodiment 1
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: weighing the tea polyphenols (ester catechin content 78.52%) of 1.20Kg, is added 6.8Kg's
70 DEG C of purified waters, stirring and dissolving, solid content 20%, after being first cooled to 25 DEG C with 15 DEG C/h rate, then with 8 DEG C/h cooling
Rate is down to 2 DEG C, stands 0.5h, obtain supernatant liquor 1. with lower sediment 1.；
Step (2), reducing temperature twice precipitating: 1. the lower sediment obtained to step (1) is added 70 DEG C of purified waters, stirring and dissolving, until
Solid content is 20%, after being first cooled to 25 DEG C with 15 DEG C/h rate, then with 8 DEG C/h rate of temperature fall is down to 2 DEG C, after standing 0.5h, obtains
To supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin 938g, water are obtained
Divide 3.51%, product content in terms of dry product 99.12%.1. 2. supernatant liquor merges with supernatant liquor after, it is concentrated and dried, obtains with letter
Tea polyphenols product based on single catechin.
Embodiment 2
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: weighing the tea polyphenols (ester catechin content 78.52%) of 1.20Kg, is added 6.8Kg's
70 DEG C of purified waters, stirring and dissolving, solid content 20%, after being cooled to 25 DEG C later with 20 DEG C/h rate, then with 10 DEG C/h drop
Warm rate is down to 2 DEG C, stands 0.5h, obtain supernatant liquor 1. with lower sediment 1.；
Step (2), reducing temperature twice precipitating: 1. 70 DEG C of purified waters and stirring and dissolving is added in the lower sediment obtained to step (1), until
Solid content is 20%, after being cooled to 25 DEG C later with 20 DEG C/h rate, then with 10 DEG C/h rate of temperature fall is down to 2 DEG C, stands 0.5h,
Obtain supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin 945g, water are obtained
Divide 4.28%, product content in terms of dry product 98.27%.1. 2. supernatant liquor merges with supernatant liquor after, it is concentrated and dried, obtains with letter
Tea polyphenols product based on single catechin.
Embodiment 3
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: weighing the tea polyphenols (ester catechin content 78.52%) of 1.20Kg, is added 6.8Kg's
70 DEG C of purified waters, stirring and dissolving, until solid content is 20%, after being cooled to 25 DEG C later with 10 DEG C/h rate, then with 5 DEG C/h cooling
Rate is down to 2 DEG C, stands 0.5h, obtain supernatant liquor 1. with lower sediment 1.；
Step (2), reducing temperature twice precipitating: 1. 70 DEG C of purified waters and stirring and dissolving is added in the lower sediment obtained to step (1), until
Solid content is 20%, after being cooled to 25 DEG C later with 10 DEG C/h rate, then with 5 DEG C/h rate of temperature fall is down to 2 DEG C, stands 0.5h, obtain
To supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains is dried under reduced pressure, the temperature being dried under reduced pressure is 60 DEG C,
Vacuum degree >=0.075Mpa obtains ester catechin 934g, moisture 2.53%, product content in terms of dry product 99.45%.Supernatant liquor
1. after 2. merging with supernatant liquor, being concentrated and dried, obtaining the tea polyphenols product based on simple catechin.
Embodiment 4
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: adding 60 DEG C of purified waters and stirring and dissolving into tea polyphenols, until solid content is 15%；Later
After being cooled to 20 DEG C with 10 DEG C/h rate, then with 5 DEG C/h rate of temperature fall be down to 0 DEG C, stand 0.5h, obtain supernatant liquor 1. and under
Layer precipitating is 1.；
Step (2), reducing temperature twice precipitating: 1. 60 DEG C of purified waters and stirring and dissolving is added in the lower sediment obtained to step (1), until
Solid content is 15%, after being cooled to 20 DEG C later with 10 DEG C/h rate, then with 5 DEG C/h rate of temperature fall is down to 0 DEG C, after standing 0.5h,
Obtain supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin is obtained.Upper layer is clear
1. 2. liquid merges with supernatant liquor after, it is concentrated and dried, obtains the tea polyphenols product based on simple catechin.
Wherein, the temperature being dried under reduced pressure is 60 DEG C, vacuum degree >=0.075Mpa
Embodiment 5
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: adding 80 DEG C of purified waters and stirring and dissolving into tea polyphenols, until solid content is 25%；Later
It after being cooled to 30 DEG C with 20 DEG C/h rate, then with 10 DEG C/h rate of temperature fall is down to 5 DEG C, stands 0.5~2h, obtain supernatant liquor 1.
1. with lower sediment；
Step (2), reducing temperature twice precipitating: 1. 80 DEG C of purified waters and stirring and dissolving is added in the lower sediment obtained to step (1), until
Solid content is 25%, after being cooled to 30 DEG C later with 20 DEG C/h rate, then with 10 DEG C/h rate of temperature fall is down to 5 DEG C, after standing 2h,
Obtain supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin is obtained.Upper layer is clear
1. 2. liquid merges with supernatant liquor after, it is concentrated and dried, obtains the tea polyphenols product based on simple catechin.
Wherein, the temperature being dried under reduced pressure is 75 DEG C, vacuum degree >=0.075Mpa
Embodiment 6
A method of ester catechin being prepared with tea polyphenols, is included the following steps:
Step (1), once cool down precipitating: adding 70 DEG C of purified waters and stirring and dissolving into tea polyphenols, until solid content is 20%；Later
1. and lower layer it after being cooled to 25 DEG C with 15 DEG C/h rate, then with 8 DEG C/h rate of temperature fall is down to 2 DEG C, stands 1h, obtain supernatant liquor
Precipitating is 1.；
Step (2), reducing temperature twice precipitating: 1. 70 DEG C of purified waters and stirring and dissolving is added in the lower sediment obtained to step (1), until
Solid content is 20%, after being cooled to 25 DEG C later with 15 DEG C/h rate, then with 8 DEG C/h rate of temperature fall is down to 2 DEG C, after standing 1h, obtains
To supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin is obtained.Upper layer is clear
1. 2. liquid merges with supernatant liquor after, it is concentrated and dried, obtains the tea polyphenols product based on simple catechin.
Wherein, the temperature being dried under reduced pressure is 65 DEG C, vacuum degree 0.08Mpa
Comparative example 1
Other than solution solid content is 10%, remaining parameter, step are identical with embodiment 1, obtain ester catechin 896g,
Moisture 6.19%, product content in terms of dry product 99.28%.
Comparative example 2
Compared with embodiment 1,2,3, difference: solution solid content is that (first stage is with 25 DEG C/h cooling for 10%, gradient cooling
Rate is down to 25 DEG C from 70 DEG C；Second stage is down to 2 DEG C from 25 DEG C with 15 DEG C/h rate of temperature fall), the complete phase of remaining parameter, step
Together, ester catechin 923g, moisture 5.42%, product content in terms of dry product 96.74% are obtained.
Comparative example 3
Compared with embodiment 1,2,3, difference: solution solid content is that (first stage is cooled down fast 10%, gradient cooling with 5 DEG C/h
Rate is down to 25 DEG C from 70 DEG C；Second stage is down to 2 DEG C from 25 DEG C with 2 DEG C/h rate of temperature fall), remaining parameter, step are identical,
Obtain ester catechin 918g, moisture 3.87%, product content in terms of dry product 99.68%.
Comparative example 4
Other than solution solid content is 30%, remaining parameter, step are identical with embodiment 1, obtain ester catechin 956g,
Moisture 4.63%, product content in terms of dry product 96.59%.
Comparative example 5
Compared with embodiment 1,2,3, difference: solution solid content is that (first stage is with 25 DEG C/h cooling for 30%, gradient cooling
Rate is down to 25 DEG C from 70 DEG C；Second stage is down to 2 DEG C from 25 DEG C with 15 DEG C/h rate of temperature fall), the complete phase of remaining parameter, step
Together, ester catechin 943g, moisture 3.91%, product content in terms of dry product 92.77% are obtained.
Comparative example 6
Compared with embodiment 1,2,3, difference: solution solid content is that (first stage is cooled down fast 30%, gradient cooling with 5 DEG C/h
Rate is down to 25 DEG C from 70 DEG C；Second stage is down to 2 DEG C from 25 DEG C with 2 DEG C/h rate of temperature fall), remaining parameter, step are identical,
Obtain ester catechin 983g, moisture 7.23%, product content in terms of dry product 97.85%.
Ester catechin content is measured using high performance liquid chromatography (HPLC), calculates product yield and purity, record is real
Example and comparative example cooling precipitating time are applied, as a result such as table 1.
Comprehensively consider product yield, purity, production cycle, solution solid content is advisable with 20% ± 5%, is preferred with 20%, gradient
Cooling: first stage rate of temperature fall is advisable with 15 ± 5 DEG C/h, is preferred with 15 DEG C/h；Second stage is advisable with 5~10 DEG C/h, excellent
Select 8 DEG C/h.
Wherein, product yield %=[(ester catechin dry product quality × ester catechin dry product content %)/(tea polyphenol raw materials
Quality × ester catechin content)] × 100%.
From table 1, we can see that the effect of 1-3 of the embodiment of the present invention is superior to comparative example, the present invention is shown
There is good synergistic effect between each parameter, step.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of method for preparing ester catechin with tea polyphenols, which comprises the steps of:
Step (1), once cool down precipitating: adding 60 DEG C~80 DEG C purified waters and stirring and dissolving into tea polyphenols, until solid content is 20%
±5%；It after being cooled to 25 ± 5 DEG C later with 15 ± 5 DEG C/h rate, then with 5~10 DEG C/h rate of temperature fall is down to 0~5 DEG C, stands
0.5~2h, obtain supernatant liquor 1. with lower sediment 1.；
Step (2), reducing temperature twice precipitating: 1. the lower sediment obtained to step (1) is added 60 DEG C~80 DEG C purified waters and stirs
Dissolution, until solid content is 20% ± 5%, after being cooled to 25 ± 5 DEG C later with 15 ± 5 DEG C/h rate, then with 5~10 DEG C/h cooling speed
Rate is down to 0~5 DEG C, after standing 0.5~2h, obtain supernatant liquor 2. with lower sediment 2.；
Step (3), is dried under reduced pressure: 2. the lower sediment that step (2) obtains being dried under reduced pressure, ester catechin is obtained.
2. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that supernatant liquor 1. and
2. supernatant liquor merges after, it is concentrated and dried, obtains the tea polyphenols product based on simple catechin.
3. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that step (1) and step
Suddenly in (2), the purifying coolant-temperature gage is 70 DEG C.
4. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that in step (1), to
Add 60 DEG C~80 DEG C purified waters in tea polyphenols, and stirring and dissolving to solid content is 20%.
5. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that step (1) and step
Suddenly in (2), with 15 DEG C/h rate, 25 ± 5 DEG C are cooled to from 60 DEG C~80 DEG C.
6. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that step (1) and step
Suddenly in (2), with 15 ± 5 DEG C/h rate, 25 DEG C are cooled to from 60 DEG C~80 DEG C.
7. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that step (1) and step
Suddenly in (2), with 5~10 DEG C/h rate, 2 DEG C are cooled to from 25 ± 5 DEG C.
8. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that step (1) and step
Suddenly in (2), with 8 DEG C/h rate, 0~5 DEG C is cooled to from 25 ± 5 DEG C.
9. the method according to claim 1 for preparing ester catechin with tea polyphenols, which is characterized in that in step (3), subtract
Pressing dry dry temperature is 60~75 DEG C, vacuum degree >=0.075Mpa.
10. the method according to claim 9 for preparing ester catechin with tea polyphenols, which is characterized in that in step (3),
The temperature being dried under reduced pressure is 65 DEG C.
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