CN114128821A - Method for extracting tea polyphenol - Google Patents
Method for extracting tea polyphenol Download PDFInfo
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- CN114128821A CN114128821A CN202111418556.9A CN202111418556A CN114128821A CN 114128821 A CN114128821 A CN 114128821A CN 202111418556 A CN202111418556 A CN 202111418556A CN 114128821 A CN114128821 A CN 114128821A
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- tea polyphenol
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- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 148
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 146
- 241001122767 Theaceae Species 0.000 title claims abstract 31
- 238000000034 method Methods 0.000 title claims description 44
- 238000000605 extraction Methods 0.000 claims abstract description 75
- 239000000843 powder Substances 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000005189 flocculation Methods 0.000 claims abstract description 29
- 230000016615 flocculation Effects 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 26
- 102000004190 Enzymes Human genes 0.000 claims abstract description 22
- 108090000790 Enzymes Proteins 0.000 claims abstract description 22
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920001661 Chitosan Polymers 0.000 claims abstract description 21
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 16
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 13
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960001948 caffeine Drugs 0.000 claims abstract description 11
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims description 33
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 229940088598 enzyme Drugs 0.000 claims description 20
- 108090000145 Bacillolysin Proteins 0.000 claims description 15
- 102000035092 Neutral proteases Human genes 0.000 claims description 15
- 108091005507 Neutral proteases Proteins 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
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- 108010059892 Cellulase Proteins 0.000 claims description 12
- 108010059820 Polygalacturonase Proteins 0.000 claims description 12
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- 238000004519 manufacturing process Methods 0.000 abstract description 8
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- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 description 2
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical compound O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
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- OHZCFWMJMWFNFP-ZVGUSBNCSA-L (2r,3r)-2,3-dihydroxybutanedioate;iron(2+) Chemical compound [Fe+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O OHZCFWMJMWFNFP-ZVGUSBNCSA-L 0.000 description 1
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 229940057006 ferrous tartrate Drugs 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 150000002206 flavan-3-ols Chemical class 0.000 description 1
- 235000011987 flavanols Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000002216 flavonol derivatives Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000473 propyl gallate Substances 0.000 description 1
- 229940075579 propyl gallate Drugs 0.000 description 1
- 235000010388 propyl gallate Nutrition 0.000 description 1
- 230000017854 proteolysis Effects 0.000 description 1
- 239000011802 pulverized particle Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 description 1
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- -1 vitamin Polyphenols Chemical class 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/36—Freezing; Subsequent thawing; Cooling
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The application relates to the technical field of natural active substance extraction methods, and particularly discloses a tea polyphenol extraction method. The extraction method of tea polyphenol comprises the steps of enzymolysis treatment, flocculation separation, supercritical fluid impurity removal, concentration, drying and the like; carrying out enzymolysis on tea powder by using composite wall-breaking enzyme to fully dissolve out tea polyphenol; then sequentially using chitosan flocculation liquid and ethanol for flocculation separation to remove macromolecular substances and theanine; then removing caffeine with supercritical carbon dioxide; finally, concentrating and drying to obtain tea polyphenol powder with high purity and high extraction rate; the preparation method is simple, industrial production can be realized, the extraction rate and purity of the tea polyphenol are high, and high-value byproducts can be fully recovered in the production process.
Description
Technical Field
The application relates to the technical field of natural active substance extraction methods, in particular to a tea polyphenol extraction method.
Background
Tea Polyphenols (Green Tea Polyphenols), also known as vitamin Polyphenols, are the general name for Polyphenols in Tea, including flavanols, anthocyanins, flavonoids, flavonols and phenolic acids. As most of the tea polyphenol contains 2 or more ortho-hydroxyl polyphenols, the tea polyphenol has strong hydrogen supply capability and strong reduction capability, and is an ideal antioxidant and color retention agent in the food industry. In addition, the tea polyphenol has inhibitory activity on nearly a hundred kinds of bacteria in the nature, shows broad-spectrum antibacterial property, and is a good food preservative. In view of the wide application of tea polyphenol in the food field, the separation and extraction technology is developed increasingly.
In the related art, an organic solvent extraction method is the most widely used method in tea polyphenol extraction methods. The principle is to extract and separate different compounds in tea by utilizing the solubility difference of different solvents. The method has the advantages of extraction rate of tea polyphenol of only 10-15% and low extraction rate.
The ion precipitation method comprises leaching tea polyphenol with water solution, and processing by centrifugal separation, acid dissolution, solvent extraction, etc. according to the principle that tea polyphenol can be complexed with metal ions to obtain high-purity tea polyphenol. And the inorganic salt precipitator has large DH value fluctuation in the precipitation and dissolution process, so that the tea polyphenol is easily oxidized and damaged, and meanwhile, metal salts are remained, so that the product safety is unstable.
The adsorption separation extraction method generally comprises adsorbing the Tea extract with a polymeric adsorbent, eluting with 95% ethanol solution to desorb GTP (Green Tea polyphenols) adsorbed on the adsorbent in ethanol, distilling under reduced pressure to recover ethanol, and vacuum drying or spray drying the concentrated solution to obtain Tea polyphenols. The method has high requirements on the adsorbent, and the dosage of the adsorbent is large. Because tea polyphenol is easily oxidized, substances such as protein, polysaccharide and the like in tea block pores between the adsorbents, so that adsorption resin prepared from the adsorbents is inactivated, and the production cost is high. Meanwhile, the purity of the tea polyphenol prepared by the method is 60-80 percent, which is lower than that of the tea polyphenol prepared by the ion precipitation method.
The supercritical carbon dioxide extraction method is to extract tea polyphenol by using fluid with temperature and pressure slightly exceeding or approaching the critical temperature and critical pressure and between gas and liquid as an extracting agent, so as to realize the separation and purification of the tea polyphenol. According to the reported results, it is possible that the solubility of tea polyphenol in critical carbon dioxide is 10 due to the low solubility of tea polyphenol in critical carbon dioxide-6The weight fraction is of order of magnitude, even if ethanol is used as entrainer, the solubility of tea polyphenol is only improved to 10-5The weight fraction is in order of magnitude, so that the extraction rate of the tea polyphenol is low, and the industrialization has technical obstacles.
In view of the above-mentioned related technologies, the applicant considers that there is a need to develop a tea polyphenol separation and extraction technology suitable for industrial production, so that the extraction rate and purity of tea polyphenol are high.
Disclosure of Invention
In order to develop a tea polyphenol separation and extraction technology which has high purity and high extraction rate and is suitable for industrial production, the application provides an extraction method of tea polyphenol.
The application provides a tea polyphenol extraction method, which adopts the following technical scheme:
the extraction method of tea polyphenol comprises the following steps:
and (3) enzymolysis treatment: adding tea powder into distilled water, wherein the weight ratio of the tea powder to the distilled water is 1 (10-20), heating to 20-60 ℃, keeping the temperature, adding composite wall-breaking enzyme into the solution, and carrying out enzymolysis treatment on the tea powder, wherein the weight of the composite wall-breaking enzyme is 0.1-0.3% of the weight of the tea powder; carrying out enzymolysis for 0.5-3 h under the condition that the pH value is 4-7 to obtain enzymolysis treatment liquid;
flocculation separation: adding a chitosan flocculation liquid into the enzymolysis treatment liquid, wherein the content of chitosan in the chitosan flocculation liquid is 0.1-0.5 wt%, and the weight ratio of the chitosan flocculation liquid to the tea powder is (2-10): 1, stirring and separating to obtain primary tea polyphenol filtrate; adding ethanol into the primary tea polyphenol filtrate, wherein the weight ratio of the ethanol to the tea powder is (0.1-0.5): 1, stirring and separating to obtain secondary tea polyphenol filtrate;
supercritical fluid purification: extracting caffeine from the secondary tea polyphenol filtrate by using a carbon dioxide extracting agent, dynamically extracting for 50-70 min at 20-40 ℃ and 25-29 MPa, separating out the carbon dioxide extracting agent, and taking the residual liquid as refined tea polyphenol filtrate;
concentrating and drying, namely concentrating and drying the refined tea polyphenol filtrate to obtain tea polyphenol powder.
By adopting the technical scheme, the raw materials of the tea powder are subjected to enzymolysis by adopting the composite wall-breaking enzyme, and because the tea polyphenol exists in the cell sap, the tea cells are decomposed by using the composite wall-breaking enzyme, so that the tea polyphenol is fully dissolved out, and the content of the tea polyphenol in the enzymolysis treatment solution is improved;
the enzymolysis treatment liquid contains a large amount of macromolecular substances such as enzyme protein, protein in tea cells, tea polysaccharide and the like and micromolecular substances such as theanine and the like, the macromolecular substances exist in the enzymolysis treatment liquid in a suspension and colloid state, and chitosan is used for adsorbing the macromolecular substances, so that the macromolecular substances are flocculated and then retained by a filter membrane to realize solid-liquid separation; adding ethanol into the filtrate after the primary separation, flocculating theanine, residual macromolecular substances and residual chitosan in the solution, and intercepting by a filter membrane again to realize solid-liquid separation and purify tea polyphenol; the chitosan and the ethanol are used together to perform a synergistic effect in flocculation and impurity separation, so that the purity of the tea polyphenol is obviously improved;
impurities such as protein, tea polysaccharide and theanine can be separated from the enzymolysis treatment liquid, and the enzymolysis treatment liquid is purified; the impurities obtained by separation are rich in nutrient components required by growth of animals and plants, and can be recycled as fertilizer or feed, and the like, so that the added value of an industrial production line is improved;
the extraction efficiency of the caffeine in the supercritical carbon dioxide fluid is high, the difficulty is low, and the extraction rate of the tea polyphenol in the supercritical carbon dioxide fluid is low, so that the caffeine can be separated from the secondary tea polyphenol filtrate along with the supercritical carbon dioxide fluid, on one hand, the secondary tea polyphenol filtrate is further purified, the caffeine is removed, the refined tea polyphenol filtrate is obtained, the purity of the tea polyphenol is improved, and the loss of the tea polyphenol in the process is extremely small and negligible; on the other hand, the caffeine is recovered along with the supercritical carbon dioxide fluid, and the caffeine can be purified subsequently to obtain a high-purity caffeine byproduct, so that the added value of an industrial production line is further increased; because the content of tea polyphenol in the refined tea polyphenol filtrate is high, the concentration efficiency is high, the loss of tea polyphenol in the purification process is reduced, and the tea polyphenol powder with high purity and high extraction rate can be obtained;
in summary, the tea polyphenol extraction method provided by the application has the following advantages: firstly, the treatment efficiency of each step is high, the treatment difficulty is low, and the method is suitable for industrial production; secondly, because the enzymolysis treatment is efficient and the limitation on raw materials is low, even if tea cells are thick and thick, the tea polyphenol can be fully dissolved out, and the extraction rate of the tea polyphenol is improved; thirdly, because the treatment of each step is efficient and the treatment time is short, the loss of the tea polyphenol in the extraction and purification process is reduced, and the purity of the tea polyphenol is high; fourthly, various byproducts can be fully recovered on the industrial production line, and the added value of the production line is high.
Preferably, the composite wall-breaking enzyme is cellulase, pectinase and neutral protease, and the weight ratio of the cellulase to the pectinase to the neutral protease is 1 (1-2) to 2-3.
By adopting the technical scheme, because substances such as cellulose, pectic substance, protein and the like exist in tea cells of the tea powder to prevent tea polyphenol in the cells from dissolving out, cellulose is decomposed by using cellulase, pectic substance is decomposed by using pectinase, and protein is decomposed by using neutral protease;
and the dosage of various enzymes is limited, so that the decomposition degree of the neutral protease on the protein is moderate, the protein in the tea powder is prevented from being degraded as much as possible on the premise that the tea polyphenol in the tea cells is fully dissolved out, and the removal of the protein in the subsequent flocculation treatment step is facilitated.
Preferably, the temperature is increased to 45-50 ℃ in the enzymolysis treatment step.
Preferably, the enzymolysis treatment time in the enzymolysis treatment step is 1-1.5 h.
Preferably, the pH value in the enzymolysis treatment step is 6.
By adopting the technical scheme, all factors in the enzymolysis treatment time, the enzymolysis temperature and the pH value influence the enzymolysis efficiency, so the enzymolysis temperature, the enzymolysis treatment time and the pH value in the enzymolysis process are controlled, the enzymolysis efficiency is optimal, the dissolution rate of tea polyphenol is improved, and the extraction rate of the tea polyphenol is further improved.
Preferably, the concentration and drying step is performed by using ethyl acetate as an extractant, and then performing reduced pressure concentration under vacuum conditions.
By adopting the technical scheme, the ethyl acetate has wide sources and low cost; and the ethyl acetate and the ethanol in the flocculation separation step have lower boiling point in a vacuum environment, high concentration efficiency, higher tea polyphenol purity and low loss rate.
Preferably, before the enzymolysis treatment step, the tea raw material is crushed at the temperature of between 70 ℃ below zero and 10 ℃ below zero to obtain tea powder.
By adopting the technical scheme, the tea raw material is pretreated in a low-temperature environment, and the method has the following advantages: firstly, the tea raw material is crushed at low temperature, and heat generated in the crushing process has no influence on tea polyphenol, so that the tea polyphenol is not easy to deteriorate; secondly, free water in the tea powder cell sap is condensed and expands in volume, and the cell wall of the tea powder is partially broken, so that the wall breaking and dissolving rate of tea polyphenol in the subsequent enzymolysis process is increased; and thirdly, the tea raw materials are kept fresh, so that the tea raw materials are not limited to fresh raw materials, the transportation is convenient, and the industrial production is facilitated.
Preferably, the temperature during the pulverization is-30 to-20 ℃.
Preferably, the pulverized particle size is 5 to 100 μm.
Through adopting above-mentioned technical scheme, in this parameter range, can be guaranteeing to improve under the prerequisite that the tea polyphenol leaching rate promoted, the energy saving reduces manufacturing cost.
In summary, the present application has the following beneficial effects:
1. the raw materials are sequentially subjected to enzymolysis, flocculation separation, supercritical fluid purification, concentration and drying and other steps to obtain a high-purity high-extraction-rate tea polyphenol product; because the treatment efficiency of each step is high, the treatment difficulty is low, be suitable for industrial production to can fully retrieve multiple accessory product in the processing procedure, the production line added value is high.
2. Cellulase, pectinase and neutral protease are preferably adopted as the composite wall breaking enzyme in the application, and the content of various enzymes is adjusted, so that tea polyphenol in tea cells is fully dissolved out, protein degradation in tea powder is avoided as far as possible, and removal of protein in the subsequent flocculation treatment step is facilitated.
3. In the application, the tea powder is obtained by preferably adopting freezing and crushing, so that the freshness retaining degree of the tea raw material is high, and the area and the transportation time of the raw material are not limited; secondly, the dissolution of tea polyphenol in the subsequent enzymolysis treatment process is facilitated; in addition, the quality of the tea polyphenol is not affected in the crushing process, and the tea polyphenol is not easy to deteriorate.
Detailed Description
Unless otherwise stated, the sources of the raw materials in the present application are as follows:
tea leaf: purchased in local tea factories, and transported to a refrigeration house for storage through a cold chain after impurity removal and cleaning;
cellulase: the enzyme activity is more than or equal to 3500U/g, and the model is SPE-017;
and (3) pectinase: the enzyme activity is more than or equal to 600U/mL, and the product number is FDY-2211;
neutral protease: the enzyme activity is more than or equal to 600U/mL, and the product number is FDG-2209;
cellulase, pectinase and neutral protease are purchased from the summer prosperous group and are food-grade additives, and the production license number of the food additive is SC 20113090600076;
and (3) chitosan: food grade, cat # 0325, purchased from south jing xi meino biotechnology limited, food additive production license number SC 20144172300190.
Preparation example of tea powder
Preparation example 1
A tea powder is prepared by the following steps: removing impurities from fresh tea leaves, cleaning, cold-chain transporting to production factory at 10 + -5 deg.C, pulverizing in a pulverizer at 20 deg.C, sieving, and sieving to obtain tea powder with particle size of 1mm or less.
Preparation examples 2 to 6
Tea powder is different from preparation example 1 in temperature at the time of tea leaf pulverization and screened particle size of tea powder, and specific parameters are shown in table 1 below.
TABLE 1 temperature at tea leaf grinding and sifted particle size of tea leaf powder
| Preparation example | Ambient temperature/deg.C during grinding | Sieving particle size/mum of tea powder |
| Preparation example 2 | -10 | ≤1000 |
| Preparation example 3 | -20 | ≤1000 |
| Preparation example 4 | -30 | ≤1000 |
| Preparation example 5 | -70 | ≤1000 |
| Preparation example 6 | -20 | 5～100 |
Preparation example 7
A tea powder is different from that of preparation example 2 in that fresh tea leaves are replaced by qualities of old tea stored for one year in a sealed container:
examples
Example 1
The extraction method of tea polyphenol comprises the following process steps:
and (3) enzymolysis treatment:
weighing 10kg of tea powder prepared in the preparation example 1, adding the tea powder into 100kg of distilled water, stirring and mixing at a rotating speed of 100rpm, heating the mixed solution to 20 ℃, wherein the temperature of the mixed solution is the temperature of an enzymolysis system; adding citric acid-sodium citrate buffer solution into the mixed solution, adjusting the pH value of an enzymolysis system to be 4, and preserving heat for later use; respectively weighing 2.5g of cellulase, 2.5g of pectinase and 5g of neutral protease, adding the enzymes into the mixed solution, and performing heat preservation and enzymolysis for 3 hours to obtain an enzymolysis treatment solution;
flocculation separation:
weighing 0.1kg of chitosan, adding 99.9kg of water, stirring and uniformly mixing to prepare 0.1wt% chitosan flocculation liquid for later use;
weighing 10kg of 0.1wt% chitosan flocculation liquid, adding into the enzymolysis treatment liquid, stirring and mixing for 0.5h, then feeding into an ultrafiltration device, filtering by using a ten thousand molecular weight ultrafiltration membrane, and recovering filter residues to obtain primary tea polyphenol filtrate;
weighing 1kg of ethanol, adding into the primary tea polyphenol filtrate, stirring and mixing for 0.5h, then feeding into an ultrafiltration device, filtering by using a ten thousand molecular weight ultrafiltration membrane, and recovering filter residues to obtain a secondary tea polyphenol filtrate;
supercritical fluid purification:
transferring the secondary tea polyphenol filtrate to an extraction kettle of a supercritical extraction device, introducing carbon dioxide gas as an extractant, boosting the pressure of the extraction kettle to 25MPa, heating to 20 ℃, dynamically extracting for 70min at the flow rate of carbon dioxide fluid of 100L/h, and collecting the carbon dioxide extractant to obtain a caffeine crude product; the residual liquid in the extraction kettle is refined tea polyphenol filtrate;
concentrating and drying:
adding ethyl acetate into the refined tea polyphenol filtrate in batches for extraction, wherein the volume ratio of the refined tea polyphenol filtrate to the ethyl acetate is 1:0.5 during each extraction, combining ethyl acetate phases after 3 times of extraction to obtain ethyl acetate extract, putting the ethyl acetate extract into vacuum reduced pressure concentration equipment, controlling the pressure in the equipment to be-0.06 MPa, heating to 40 ℃, and preserving heat for concentration for 1h to obtain concentrated solution;
transferring the concentrated solution to a spray dryer, and spray drying at 20 deg.C to obtain tea polyphenols powder.
Examples 2 to 6
The extraction method of tea polyphenol is different from the extraction method of the tea polyphenol in the embodiment 1 in that the sources of tea powder are different; wherein, the tea powder in the example 2 is derived from the preparation example 2; the tea powder of example 3 was derived from preparation example 3; example 4 tea powder was derived from preparation 4; the tea powder of example 5 was derived from preparation example 5; the tea powder of example 6 was derived from preparation example 6; the tea powder of example 7 was derived from preparation example 7.
Examples 8 to 18
The tea polyphenol extraction method is different from the tea polyphenol extraction method in example 1 in that each process parameter in the enzymolysis treatment step is shown in the following table 2.
TABLE 2 Process parameters of the enzymatic treatment step
Examples 19 to 22
The method for extracting tea polyphenol is different from the method in example 18 in that each process parameter in the flocculation separation step is different, and the specific process parameters are shown in the following table 3.
TABLE 3 Process parameters in the flocculation separation step
| Process parameters | Chitosan concentration/wt% | Chitosan flocculation liquid adding amount/kg | Ethanol addition amount/kg |
| Example 18 | 0.1 | 10 | 1 |
| Example 19 | 0.3 | 10 | 1 |
| Example 20 | 0.5 | 10 | 1 |
| Example 21 | 0.3 | 30 | 1 |
| Example 22 | 0.3 | 30 | 5 |
Example 23
The method for extracting tea polyphenol is different from the method in the embodiment 22 in that the process parameters in the supercritical fluid purification step are different, and the specific operations are as follows: transferring the secondary tea polyphenol filtrate to an extraction kettle of a supercritical extraction device, introducing carbon dioxide gas as an extractant, boosting the pressure of the extraction kettle to 29MPa, heating to 40 ℃, dynamically extracting for 50min at the flow rate of carbon dioxide fluid of 100L/h, and collecting the carbon dioxide extractant to obtain a caffeine crude product; the residual liquid in the extraction kettle is refined tea polyphenol filtrate.
Comparative example
Comparative examples 1 to 3
The tea polyphenol extraction method is different from the method in the embodiment 1 in that: the composition of the composite wall-breaking enzyme used in the enzymolysis step is different, and the specific composition of the composite wall-breaking enzyme is shown in table 4 below.
TABLE 4 composite wall-breaking enzyme composition in the step of enzymatic treatment
Comparative example 4
The tea polyphenol extraction method is different from the method in example 19 in that: in the step of flocculation separation, 10kg of chitosan flocculation liquid with the concentration of 0.1wt% is added into the primary tea polyphenol filtrate, and ultrafiltration separation is carried out again to obtain secondary tea polyphenol filtrate.
Comparative example 5
The tea polyphenol extraction method is different from the method in example 19 in that: adding 1kg of ethanol into the enzymolysis treatment liquid in the flocculation separation step, and performing ultrafiltration separation to obtain primary tea polyphenol filtrate; then using 1kg of ethanol for ultrafiltration separation to obtain secondary tea polyphenol filtrate.
Performance test
Detection method
The extraction rate of tea polyphenol:
3g of the sample was weighed out exactly to the ground sample in a conical flask, boiled with distilled water and immediately transferred into a boiling water bath, and the extraction was shaken every second time. Filtering under reduced pressure immediately after leaching. Transferring the filtrate into a 500mL volumetric flask, washing residues for 2-3 times by using a small amount of hot distilled water, filtering the filtrate into the volumetric flask, cooling, and diluting the filtrate to a scale by using the distilled water; accurately sucking 1mL of the test solution, injecting the test solution into a 25mL volumetric flask, adding 4mL of distilled water and 5mL of ferrous tartrate solution, fully mixing, adding phosphate buffer solution to a constant volume to a scale, using a 10mm cuvette at a wavelength of 540nm, using a reagent blank as a reference, and determining absorbance A;
the experimental sample detects that the percentage of the content of the tea polyphenol in the total content of the tea polyphenol (refer to GB/T8313-.
The purity of tea polyphenol is as follows: the tea polyphenol purity was determined according to QB/T2154-1995, in which propyl gallate was used as the standard.
TABLE 5 EXAMPLES 1-7 examination of the extraction yield and purity of tea polyphenols
| Detecting an object | Extraction ratio/% | Purity/%) | Detecting an object | Extraction ratio/% | Purity/%) |
| Example 1 | 81.6 | 92.1 | Example 5 | 84.3 | 92.2 |
| Example 2 | 84.2 | 92.5 | Example 6 | 85.6 | 92.7 |
| Example 3 | 85.0 | 92.2 | Example 7 | 82.3 | 91.3 |
| Example 4 | 84.8 | 92.3 |
Examples 1 to 7 differ in the pretreatment conditions for tea powder. As can be seen from table 5, when comparing example 1 with examples 2 to 7, the tea leaves of example 1 were ground at room temperature, while the tea leaves of examples 2 to 7 were ground under freezing conditions, and the extraction rate of tea polyphenols of examples 2 to 7 was significantly increased, which proved that the freeze grinding was favorable for dissolution of tea polyphenols in the later enzymolysis step;
secondly, the freeze grinding temperatures of the examples 2 to 5 are different, the best freeze grinding temperature is-20 ℃, and when the temperature is lower than the temperature, the extraction rate of the tea polyphenol is not improved, and the energy consumption is larger; above this temperature, the tea polyphenol extraction rate is slightly reduced;
furthermore, the milled particle size of example 6 was smaller than that of example 3 and the extraction rate of tea polyphenols increased from 85.0% to 85.6%, indicating that a decrease in the particle size of the tea powder increased the extraction rate of tea polyphenols;
finally, the tea leaves used in example 7 are old tea, the cell wall thickness of the old tea is not easy to dissolve out, but the extraction rate of grinding the old tea under the freezing condition to prepare tea polyphenol can be better than that of fresh tea at normal temperature, which shows that the application uses the freezing grinding technology to treat the tea leaves, and can break through the limitation of tea raw materials in the prior art, namely, the old tea is difficult to be used for extracting the tea polyphenol due to fermentation and oxidation in the storage process.
TABLE 6 examination results of extraction rate and purity of tea polyphenols in examples 8-12 and comparative examples 1-3
| Detecting an object | Extraction ratio/% | Purity/%) | Detecting an object | Extraction ratio/% | Purity/%) |
| Example 8 | 87.2 | 95.1 | Example 12 | 88.6 | 95.0 |
| Example 9 | 86.2 | 92.6 | Comparative example 1 | 72.1 | 95.2 |
| Example 10 | 87.3 | 92.8 | Comparative example 2 | 75.3 | 90.4 |
| Example 11 | 83.4 | 94.3 | Comparative example 3 | 68.5 | 87.5 |
Combining tables 5 and 6, it can be seen that: firstly, the composite wall-breaking enzymes of examples 6 and 8-11 and comparative examples 1-3 have the same weight, but the compositions of the composite wall-breaking enzymes are different, and the influence on the extraction rate and purity of tea polyphenol is obvious; any two of cellulase, pectinase and neutral protease are used in the comparative examples 1-3 and are compounded according to the weight ratio of 1:1, and the extraction rates of the comparative examples 1-3 are all lower than 80%, which shows that the compounding of the cellulase, the pectinase and the neutral protease has a synergistic effect in the aspect of improving the extraction rate of tea polyphenol; secondly, examples 6, 8-11 show that different weight ratios of cellulase, pectinase and neutral protease have obvious influence on the extraction rate and purity of tea polyphenol: example 8 compared to example 6, the tea polyphenol extraction rate was increased by 1.6% and the purity by 2.4%, which may be due to: the neutral protease content is moderate, so that the cell wall of the tea powder is easy to break, the dissolution rate of active substances contained in the tea powder is high, and meanwhile, the decomposition degree of macromolecular proteins in the active substances is moderate, so that the subsequent flocculation separation is easy to realize, and the tea polyphenol purity is improved; example 11 compared with example 6, the extraction rate of tea polyphenol was reduced by 2.2%, indicating that the reduction of the content of neutral protease significantly causes the reduction of the extraction rate of tea polyphenol.
TABLE 7 EXAMPLES 13-18 examination of the extraction yield and purity of tea polyphenols
| Detecting an object | Extraction ratio/% | Purity/%) | Detecting an object | Extraction ratio/% | Purity/%) |
| Example 13 | 88.9 | 95.4 | Example 16 | 90.2 | 95.1 |
| Example 14 | 88.5 | 95.1 | Example 17 | 90.0 | 94.9 |
| Example 15 | 88.7 | 94.8 | Example 18 | 90.1 | 95.2 |
It can be seen from table 6 and table 7 that the enzymolysis time, the enzymolysis temperature and the pH value of the enzymolysis system have little influence on the extraction rate and purity of tea polyphenol.
TABLE 8 examination results of extraction rate and purity of tea polyphenols in examples 19-23 and comparative examples 4-5
| Detecting an object | Extraction ratio/% | Purity/%) | Detecting an object | Extraction ratio/% | Purity/%) |
| Example 19 | 90.2 | 95.3 | Example 23 | 90.6 | 96.2 |
| Example 20 | 90.1 | 95.5 | Comparative example 4 | 89.8 | 91.4 |
| Example 21 | 90.3 | 95.6 | Comparative example 5 | 90.4 | 90.7 |
| Example 22 | 90.7 | 96.1 |
As can be seen from Table 8, only chitosan flocculation liquid is used for flocculation in comparative example 4, only ethanol is used for extraction and impurity removal in comparative example 5, but the purity of tea polyphenol is lower than that of example 19, and the combination of the chitosan flocculation liquid and the ethanol proves that the synergistic effect is achieved in the aspect of improving the purity of the tea polyphenol.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The extraction method of tea polyphenol is characterized by comprising the following steps:
and (3) enzymolysis treatment: adding tea powder into distilled water, wherein the weight ratio of the tea powder to the distilled water is 1 (10-20), heating to 20-60 ℃, keeping the temperature, adding composite wall-breaking enzyme into the solution, and carrying out enzymolysis treatment on the tea powder, wherein the weight of the composite wall-breaking enzyme is 0.1-0.3% of the weight of the tea powder; carrying out enzymolysis for 0.5-3 h under the condition that the pH value is 4-7 to obtain enzymolysis treatment liquid;
flocculation separation: adding a chitosan flocculation liquid into the enzymolysis treatment liquid, wherein the content of chitosan in the chitosan flocculation liquid is 0.1-0.5 wt%, and the weight ratio of the chitosan flocculation liquid to the tea powder is (1-3) to 1, stirring and separating to obtain primary tea polyphenol filtrate; adding ethanol into the primary tea polyphenol filtrate, wherein the weight ratio of the ethanol to the tea powder is (0.1-0.5): 1, stirring and separating to obtain secondary tea polyphenol filtrate;
removing impurities by supercritical fluid: extracting caffeine from the secondary tea polyphenol filtrate by using a carbon dioxide extracting agent, dynamically extracting for 50-70 min at 20-40 ℃ and 25-29 MPa, separating out the carbon dioxide extracting agent, and taking the residual liquid as refined tea polyphenol filtrate;
concentrating and drying, namely concentrating and drying the refined tea polyphenol filtrate to obtain tea polyphenol powder.
2. The method for extracting tea polyphenol according to claim 1, characterized in that: the composite wall-breaking enzyme is cellulase, pectinase and neutral protease, and the weight ratio of the cellulase to the pectinase to the neutral protease is 1 (1-2) to 2-3.
3. The method for extracting tea polyphenol according to claim 1, characterized in that: and in the enzymolysis treatment step, the temperature is increased to 45-50 ℃.
4. The method for extracting tea polyphenol as claimed in claim 3, characterized in that: the enzymolysis treatment time in the enzymolysis treatment step is 1-1.5 h.
5. The method for extracting tea polyphenol according to claim 4, characterized in that: the pH value in the enzymolysis treatment step is 6.
6. The method for extracting tea polyphenol according to claim 1, characterized in that: in the concentration and drying step, ethyl acetate is used as an extractant for extraction, and then the concentration is carried out under vacuum condition.
7. The method for extracting tea polyphenol according to claim 1, characterized in that: before the enzymolysis treatment step, the tea raw material is crushed at the temperature of between 70 ℃ below zero and 10 ℃ below zero to obtain tea powder.
8. The method for extracting tea polyphenol as claimed in claim 7, characterized in that: the temperature during the crushing is-30 to-20 ℃.
9. The method for extracting tea polyphenol according to claim 1, characterized in that: the crushed particle size is 5-100 μm.
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