CN115024370A - Method for extracting tea polyphenol from Pu' er tea leaves by fermentation method - Google Patents
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 55
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 55
- 238000000855 fermentation Methods 0.000 title claims abstract description 36
- 230000004151 fermentation Effects 0.000 title claims abstract description 36
- 235000019224 Camellia sinensis var Qingmao Nutrition 0.000 title claims abstract description 25
- 235000020339 pu-erh tea Nutrition 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 241000228245 Aspergillus niger Species 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 19
- 238000002386 leaching Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
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- 238000001816 cooling Methods 0.000 claims description 4
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- 238000004519 manufacturing process Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
- A23F3/166—Addition of, or treatment with, enzymes or microorganisms
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Abstract
The invention discloses a method for extracting tea polyphenol in Pu 'er tea trimmed leaves by a fermentation method, which adopts a microbial fermentation method to extract effective components of the trimmed waste tea leaves in the Pu' er tea cultivation process; the dissolution rate of the substances contained in the tea leaves is promoted by adopting a pre-extraction fermentation method. The method for extracting tea polyphenol from the Pu' er tea trimmed leaves by the fermentation method provided by the invention fully utilizes field waste tea resources, and accords with the green development concept; by using a pre-extraction pile fermentation method, compared with the method of directly extracting unfermented tea leaves, the tea polyphenol extraction rate is improved by 5-10%; the enzyme generated by the hydrolysis of aspergillus niger in the fermentation process can destroy the cell wall of tea cells, so that effective substances in the cells are more easily dissolved out after the cell wall is destroyed, the extraction rate of tea polyphenol is improved, and the purity of the tea polyphenol obtained by the method is higher compared with that obtained by the traditional method; the method does not use an organic solvent, is more environment-friendly, has simple and easily-operated working procedures and lower cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of extraction of effective components of tea, and particularly relates to a method for extracting tea polyphenol from Pu' er tea pruning leaves by a fermentation method.
Background
Tea polyphenols are the general name of polyphenols in tea, and are white amorphous powder and easily soluble in water. The tea polyphenol has good antioxidant activity, and the antioxidant activity is superior to Butyl Hydroxy Anisole (BHA), dibutyl hydroxy toluene (BHT), tert-butyl hydroquinone (TBHQ) and the like. The study on acute toxicity, subacute toxicity and various pharmacological tests of tea polyphenol by scholars at home and abroad shows that the tea polyphenol is safe and nontoxic. Tea polyphenol is not only a novel natural antioxidant, but also has obvious pharmacological functions of resisting aging, eliminating excessive free radicals of human bodies, reducing fat and weight, reducing blood sugar, reducing blood fat and cholesterol, preventing cardiovascular diseases, inhibiting tumor cells and the like, and has important application in the fields of food processing, medicines, daily chemical industry and the like.
In the tea tree cultivation process, in order to inhibit the top advantages of the tea trees and achieve the purpose of continuous high yield and high quality, tea farmers often regularly prune the tea trees to generate a large amount of waste tea branches and leaves, thereby causing resource waste.
The extraction technology of tea polyphenol mainly comprises the following steps: water extraction, alcohol extraction, organic solvent extraction, ion precipitation, adsorption separation, ultrasonic-microwave synergistic extraction, mechanochemical-assisted extraction, enzymolysis and the like; the method has the advantages of high extraction cost of tea polyphenol, low production efficiency, low purity and great environmental pollution due to the adoption of toxic and volatile organic solvents such as chloroform and the like. And fresh and tender tea leaves or finished tea leaves are mostly adopted as extraction raw materials, the report of extracting tea polyphenol by using trimmed leaves is not provided, and the resource utilization is insufficient.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for extracting tea polyphenol in Pu 'er tea trimmed leaves by a fermentation method, which adopts a microbial fermentation method to extract effective components of the trimmed waste tea leaves in the Pu' er tea cultivation process; by adopting a pre-extraction fermentation method, the dissolution rate of substances contained in the tea is promoted, the problems of low production efficiency and low purity of tea polyphenol in the background technology are solved, the production cost of the tea polyphenol is reduced, and the tea polyphenol is more environment-friendly.
In order to solve the technical problems, the invention is realized by the following technical scheme: a method for extracting tea polyphenol from Pu' er tea trimmed leaves by a fermentation method is characterized by comprising the following steps:
s1 raw material treatment: removing stems of the collected pruned tea branches, taking fresh leaves, and crushing to prepare tea powder for later use;
s2 fermentation: transferring the tea powder prepared in the step 1 into a closed environment, adding active aspergillus niger, uniformly stirring, and covering linen for heat preservation and fermentation;
s3 leaching: adding pure water into the tea powder fermented in the step 2 for extraction;
s4 filtering: filtering and combining the extracting solution obtained in the step 3; naturally cooling;
s5 centrifugation: centrifuging and taking supernatant;
s6 concentration: concentrating the supernatant obtained in the step 5;
s7 impurity removal: freezing the concentrated solution to remove impurities such as protein and polysaccharide;
s8 drying: vacuum freeze drying the frozen concentrated solution to obtain Pu' er tea polyphenol powder;
further, 0.05-0.3g/kg of active aspergillus niger is added into the S2, and the mixture is covered with linen for heat preservation and fermentation for 45-55h, and the temperature is controlled at 30-40 ℃;
further, adding 10-20 times of pure water by weight into the S3 tea powder for leaching, wherein the water temperature is 75-85 ℃, and the leaching times are 2-4 times, and each time lasts for 1-3 h;
further, the S5 is centrifuged for 10-40min by a centrifuge under the condition of 3000r-4000 r/min;
further, concentrating the S6 supernatant at 75-95 ℃ and under the pressure of-0.05-0.1 MPa to 1/20-1/10 of the original volume.
Further, the S7 concentrated solution is frozen to-20 to-40 ℃;
further, carrying out vacuum freeze drying on the S8 condensed liquid under the condition of 0-100 Mpa;
the invention has the beneficial effects that:
1. according to the method for extracting the tea polyphenol in the Pu' er tea trimmed leaves, provided by the invention, the field waste tea leaves are fully utilized, and the green development concept is met;
2. according to the method, the tea polyphenol leaching rate of the pre-extraction pile fermentation method is improved by 5-10% compared with the tea polyphenol leaching rate of the direct extraction of unfermented tea leaves;
3. according to the method, the cell walls of tea cells can be damaged by the enzyme generated by hydrolysis of aspergillus niger in the fermentation process, and effective substances in the cells are dissolved out more easily after the cell walls are damaged, so that the extraction rate of tea polyphenol is improved, and the purity of the tea polyphenol obtained by the method is higher compared with that obtained by a traditional method;
4. the method provided by the invention does not use an organic solvent, can avoid environmental transition pollution, has simple process and low cost, and is suitable for industrial production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a step diagram of a method for extracting tea polyphenol from Pu' er tea leaves by a fermentation method.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, the specific implementation steps of the method for extracting tea polyphenol from the Pu' er tea leaves by fermentation are as follows:
1. raw material treatment: removing stems of the collected pruned tea branches, taking fresh leaves, and crushing to prepare tea powder for later use;
2. fermentation: transferring the tea powder prepared in the step 1 into a closed environment, adding 0.1g/kg of active aspergillus niger, uniformly stirring, covering a linen, keeping the temperature and fermenting for 48 hours, and controlling the temperature to be 35 ℃;
3. leaching: adding 8 times of pure water by weight into the tea powder fermented in the step 2 for leaching, wherein the water temperature is 80 ℃, and the leaching times are 3 times, and each time lasts for 1 hour;
4. and (3) filtering: filtering and combining the extracting solution obtained in the step 3; naturally cooling;
5. centrifuging: centrifuging for 20min at 3500r/min with a centrifuge, and collecting supernatant;
6. concentration: concentrating the supernatant obtained in the step 5 at 85 ℃ and-0.07 MPa to 1/10 of the original volume;
7. removing impurities: freezing the concentrated solution to-30 deg.C, and removing impurities such as protein and polysaccharide;
8. and (3) drying: and (4) carrying out vacuum freeze drying on the frozen concentrated solution under the condition of 50Mpa to obtain Pu' er tea polyphenol powder.
Example 2
This example is another method for extracting tea polyphenols from Pu' er tea leaves by fermentation
The method comprises the following specific implementation steps:
1. raw material treatment: removing stems of the collected pruned tea branches, taking fresh leaves, and crushing to prepare tea powder for later use;
2. fermentation: transferring the tea powder prepared in the step 1 into a closed environment, adding 0.2g/kg of active aspergillus niger, uniformly stirring, covering a linen, keeping the temperature, and fermenting for 50 hours, wherein the temperature is controlled at 40 ℃;
3. leaching: adding 10 times of pure water by weight into the tea powder fermented in the step 2 for leaching, wherein the water temperature is 85 ℃, and the leaching times are 2 times, and each time lasts for 2 hours;
4. and (3) filtering: filtering and combining the extracting solution obtained in the step 3; naturally cooling;
5. centrifuging: centrifuging for 30min at 3800r/min with a centrifuge, and collecting supernatant;
6. concentration: concentrating the supernatant obtained in the step 5 at the temperature of 90 ℃ and under the pressure of-0.06 MPa to 1/12 of the original volume;
7. removing impurities: freezing the concentrated solution to-35 deg.C, and removing impurities such as protein and polysaccharide;
8. and (3) drying: vacuum freeze drying the frozen concentrated solution under 10Mpa to obtain Pu her tea polyphenols powder. The results of the extraction rate of tea polyphenols are shown in Table I.
Example 3
In order to better illustrate that the technology of the invention can well improve the extraction efficiency of tea polyphenol, the same extraction process is adopted, and the tea polyphenol is extracted by using the cut leaves of the unfermented Pu' er tea, and the result is shown in the second table.
Significance analysis of the yield of the epi-polyphenol (one-way analysis of variance)
*p<0.05**p<0.01
Group 1.0: carrying out Aspergillus niger fermentation pretreatment; group 2.0: without fermentation treatment
As can be seen from the above table: the samples of different groups all showed significance (p <0.05) for polyphenol yield (%), meaning that the samples of different groups all showed differences for polyphenol yield (%). The specific analysis shows that: the group showed significance at a level of 0.01 for polyphenol yield (%) (F: 571.042, p: 0.000) and the specific comparison differences revealed that the average value of 1.0 (6.01) was significantly higher than the average value of 2.0 (5.24).
In conclusion, the following steps are carried out: samples of different groups all showed significant differences in polyphenol yield (%). Compared with untreated polyphenol, the yield of the polyphenol obtained by fermentation treatment by using aspergillus niger is obviously improved.
In conclusion, 1, the method for extracting tea polyphenol from the Pu' er tea pruned leaves provided by the invention fully utilizes field waste tea leaves, and accords with the green development concept;
2. according to the method, the tea polyphenol leaching rate of the pre-extraction pile fermentation method is improved by 5-10% compared with the tea polyphenol leaching rate of the direct extraction of unfermented tea leaves;
3. according to the method, the enzyme generated by the hydrolysis of the aspergillus niger can damage the cell wall of the tea cell, so that effective substances in the cell can be dissolved out more easily, the extraction rate of tea polyphenol is improved, and the purity of the tea polyphenol obtained by the traditional method is higher;
4. the method provided by the invention does not use an organic solvent, can avoid environmental transition pollution, has simple process and low cost, and is suitable for industrial production.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for extracting tea polyphenol from Pu' er tea trimmed leaves by a fermentation method is characterized by comprising the following steps:
s1 raw material treatment: removing stems of the collected pruned tea branches, taking fresh leaves, and crushing to prepare tea powder for later use;
s2 fermentation: transferring the tea powder prepared in the step 1 into a closed environment, adding active aspergillus niger, uniformly stirring, and covering linen for heat preservation and fermentation;
s3 leaching: adding pure water into the tea powder fermented in the step 2 for extraction to obtain an extracting solution;
s4 filtering: filtering and combining the extracting solution obtained in the step 3; naturally cooling;
s5 centrifugation: centrifuging the filtrate obtained in the step 4, and taking supernatant;
s6 concentration: concentrating the supernatant obtained in the step 5;
s7 impurity removal: freezing the concentrated solution to remove impurities such as protein and polysaccharide;
s8 drying: and (4) carrying out vacuum freeze drying on the frozen concentrated solution to obtain Pu' er tea polyphenol powder.
2. The method for extracting tea polyphenol from Pu' er tea leaves by fermentation according to claim 1, wherein the active Aspergillus niger of 0.05-0.30g/kg is added into S2, and the leaves are covered with hemp cloth and fermented for 45-55h under the condition of 30-40 ℃.
3. The method for extracting tea polyphenol in Pu' er tea pruned leaves by fermentation according to claim 1, wherein pure water with the weight 6-12 times of that of S3 tea powder is added for extraction, the water temperature is 75-85 ℃, the extraction times are 2-4 times, and each time lasts for 1-3 h.
4. The method for extracting tea polyphenol from the trimmed leaves of Pu' er tea by the fermentation method according to claim 1, wherein the S5 is centrifuged by a centrifuge at 3000 r/min to 4000r/min for 10 min to 40 min.
5. The method for extracting tea polyphenol from Pu' er tea leaves by fermentation according to claim 1, wherein the supernatant of S6 is concentrated under the conditions of 75-95 ℃ and-0.05-0.1 MPa to 1/20-1/10 of the original volume.
6. The method for extracting tea polyphenol from the Pu' er tea leaves by fermentation according to claim 1, wherein the S7 concentrated solution is frozen to-20 to-40 ℃.
7. The method for extracting tea polyphenol from the trimmed Pu' er tea leaves by the fermentation method according to claim 1, wherein the S8 concentrated solution is subjected to vacuum freeze drying under the condition of 0-100 Mpa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232724A (en) * | 2013-03-31 | 2013-08-07 | 新疆刀郎枣业有限公司 | Aspergillus niger liquid fermentation assisted method for extraction of red date pigment |
| CN104497057A (en) * | 2014-12-22 | 2015-04-08 | 腾冲县高黎贡山生态茶业有限责任公司 | Process for extracting tea polyphenols from Yunan dayezhong tea leaves |
| CN110981845A (en) * | 2019-12-20 | 2020-04-10 | 湖北沛丰生物科技股份有限公司 | Method for extracting tea polyphenol from tea leaves and tea branches cut from tea trees |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232724A (en) * | 2013-03-31 | 2013-08-07 | 新疆刀郎枣业有限公司 | Aspergillus niger liquid fermentation assisted method for extraction of red date pigment |
| CN104497057A (en) * | 2014-12-22 | 2015-04-08 | 腾冲县高黎贡山生态茶业有限责任公司 | Process for extracting tea polyphenols from Yunan dayezhong tea leaves |
| CN110981845A (en) * | 2019-12-20 | 2020-04-10 | 湖北沛丰生物科技股份有限公司 | Method for extracting tea polyphenol from tea leaves and tea branches cut from tea trees |
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