CN114250112A - Process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide - Google Patents

Process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide Download PDF

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CN114250112A
CN114250112A CN202111351707.3A CN202111351707A CN114250112A CN 114250112 A CN114250112 A CN 114250112A CN 202111351707 A CN202111351707 A CN 202111351707A CN 114250112 A CN114250112 A CN 114250112A
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tea
oil
polyphenol
polysaccharide
polypeptide
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褚剑
郭德斌
邱丽聪
涂宗财
王辉
余刚
李军
刘光宪
胡月明
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Huangshanghuang Group Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14—Extraction; Separation; Purification
    • C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14—Extraction; Separation; Purification
    • C07K1/34—Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14—Extraction; Separation; Purification
    • C07K1/36—Extraction; Separation; Purification by a combination of two or more processes of different types
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07K—PEPTIDES
    • C07K2/00—Peptides of undefined number of amino acids; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis

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Abstract

The invention provides a process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide, which comprises the following steps: step one, pretreatment of fresh tea seeds: step two, performing wall breaking on the fresh tea seeds by adopting a three-step wet method: step three, hydrolyzing by using compound biological enzyme: fourthly, demulsifying and breaking bonds by ultrasonic wave and electrolyte: step five, synchronously leaching with warm water: sixthly, separating and purifying the crude tea oil by using a rotating membrane: and seventhly, separating and purifying the aqueous solution rich in the oil tea polypeptide and the oil tea polysaccharide. The process for synchronously extracting the polyphenol tea oil, the tea-oil camellia polypeptide and the tea-oil camellia polysaccharide, provided by the invention, can improve the utilization rate of tea seed meal, reduce resource waste and improve the added value of products.

Description

Process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide
Technical Field
The invention relates to the technical field of food processing, in particular to a process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide.
Background
As is well known, tea oil is a high-quality health edible oil which is rich in functional components such as unsaturated fatty acid, squalene, vitamin E and the like. The tea oil has good conditioning and promoting effects on human cardiovascular and cerebrovascular, digestive system, reproductive system, immune system, nervous system, endocrine system and the like, so the tea oil has higher medical value and enjoys the reputation of 'liquid gold'.
Meanwhile, the by-product of the tea oil after oil extraction contains a large amount of active substances such as protein, polysaccharide, tea saponin, polyphenol and the like, and has wide development space and application prospect. However, various problems exist in the current tea oil extraction and refining process. For example, the unsaturated fatty acid in the tea oil is easily oxidized and the release of polyphenol is influenced when the tea seeds are pressed after being dried; the tea oil is extracted by using an organic solvent, so that organic solvent residue is easily caused, and the use risk of the organic solvent is increased; in addition, the tea oil has low polyphenol content, and bound polyphenol in tea seeds cannot be extracted; the further utilization rate of the tea seed meal after oil extraction or oil extraction is lower, and more process flows need to be added.
Based on the above technical problems, there is a need to provide a novel processing technology for simultaneously extracting polyphenol tea oil, tea-oil polypeptides and tea-oil polysaccharides.
Disclosure of Invention
Therefore, the invention aims to solve the problem that the deep processing effect of the tea oil is limited to a certain extent by lacking a process for simultaneously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide in the prior art.
The invention provides a process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide, wherein the process comprises the following steps:
step one, pretreatment of fresh tea seeds:
selecting fresh tea seeds picked in the current year for hulling, wherein the hulling rate is controlled to be more than 95%;
step two, performing wall breaking on the fresh tea seeds by adopting a three-step wet method:
grinding the fresh tea seeds subjected to shelling in a colloid mill, wherein the grinding granularity is 60-80 meshes, adding purified water according to a preset proportion, uniformly mixing, and performing two-step wall breaking by adopting a 120-150 mesh colloid mill; finally, homogenizing by a homogenizer to obtain a tea seed mixed solution;
step three, hydrolyzing by using compound biological enzyme:
carrying out multi-step enzyme reaction on the homogenized tea seed mixed solution to obtain a hydrolysate; wherein the multi-step enzyme reaction comprises the following steps in sequence: the first step is composite protease hydrolysis; the second step is the hydrolysis of flavourzyme; the third step is cellulose hydrolysis;
fourthly, demulsifying and breaking bonds by ultrasonic wave and electrolyte:
demulsifying and breaking glycosidic bonds of the hydrolysate obtained in the third step, adding sodium chloride and sodium citrate as electrolytes, and demulsifying under the ultrasonic condition to promote the breaking of the glycosidic bonds to finally obtain treated feed liquid;
step five, synchronously leaching with warm water:
heating and stirring the treated feed liquid, then carrying out centrifugal separation, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides;
sixthly, separating and purifying the crude tea oil by using a rotating membrane:
separating the crude tea oil rich in polyphenol by using a rotating membrane to obtain polyphenol tea oil by filtering;
and seventhly, separating and purifying the aqueous solution rich in the oil tea polypeptide and the oil tea polysaccharide:
separating and purifying the water solution rich in the oil tea polypeptide and oil tea polysaccharide by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa to realize separation and purification of polysaccharide and polypeptide, and finally freeze-drying to obtain the oil tea polypeptide and the oil tea polysaccharide.
The process for synchronously extracting the polyphenol tea oil, the tea-oil polypeptides and the tea-oil polysaccharides comprises the following steps of firstly, storing fresh tea seeds for 0-90 days from picking to production and processing, wherein the acid value is 0.6-0.8, the oil content is 40-45%, and the water content is 15-20%.
The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide comprises the following steps of:
grinding the fresh tea seeds subjected to shelling in a colloid mill, wherein the grinding granularity is 60-80 meshes, adding purified water according to the proportion of 1: 4-5, uniformly mixing, and performing two-step wall breaking by adopting a 120-150 mesh colloid mill; finally, homogenizing by a homogenizer to obtain a tea seed mixed solution; wherein the homogenizing pressure is 80-120 MPa, the homogenizing times are 2-3 times, and the mean temperature is 30-40 ℃.
The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide comprises the following steps:
carrying out multi-step enzyme reaction on the homogenized tea seed mixed solution to obtain a hydrolysate; wherein, the first step is hydrolysis of the compound protease, the pH value is adjusted to 8.0-8.5, the temperature is 55-60 ℃, 600-800U/g of the compound protease is added, and the reaction time is 2-3 h; secondly, hydrolyzing the flavourzyme, adjusting the pH value to 7.5-8.0, adjusting the temperature to 55-60 ℃, adding 500-800U/g of flavourzyme, and reacting for 2-3 h; and the third step is cellulase hydrolysis, wherein the pH value is adjusted to 7.0-7.5, the temperature is 55-60 ℃, 400-500U/g of cellulase is added, and the reaction time is 3 hours.
The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide, wherein in the fourth step, the method for demulsifying and breaking bonds by using ultrasonic wave and electrolyte comprises the following steps:
demulsifying and breaking glycosidic bonds of the hydrolysate obtained in the third step, adding 1.5-2% of sodium chloride and 0.7-1% of sodium citrate as electrolytes, and demulsifying under the ultrasonic condition to promote the glycosidic bonds to break to finally obtain the processed feed liquid, wherein the ultrasonic condition is 2000-3000W/m3The ultrasonic time is 5-7 min, and the ultrasonic temperature is 50-60 ℃.
The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide comprises the following steps of:
heating the treated feed liquid to 80-90 ℃, stirring for 30min, then carrying out centrifugal separation at the rotating speed of 6000-8000 r/min for 18-20 min, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides.
The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide comprises the following steps of:
filtering and separating the crude tea oil rich in polyphenol by adopting a rotating membrane to obtain polyphenol tea oil; wherein the filtration precision is 50-100 nm, the fluid temperature is 50-60 ℃, and the fluid pressure is 5-6 MPa.
The process for synchronously extracting the polyphenol tea oil, the tea-oil polypeptide and the tea-oil polysaccharide, wherein in the seventh step, the method for separating and purifying the aqueous solution rich in the tea-oil polypeptide and the tea-oil polysaccharide comprises the following steps:
separating and purifying the water solution rich in the oil tea polypeptide and oil tea polysaccharide by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa to realize separation and purification of polysaccharide and polypeptide, and finally freeze-drying to obtain the oil tea polypeptide and the oil tea polysaccharide; wherein the centrifugal pressure for separation and purification is 1-2 MPa.
The process for synchronously extracting the polyphenol tea oil, the tea-oil tree polypeptide and the tea-oil tree polysaccharide provided by the invention has the following technical effects:
1. fresh tea seeds are used as raw materials, and different from other tea oil production technologies, the drying link of the tea seeds can be reduced, and chemical reactions such as oxidation of fatty acid, denaturation of protein, polymerization of polysaccharide and protein, combination of free phenol and protein/polysaccharide and the like in the tea seeds are reduced, so that the content of the free phenol and the subsequent proteolysis effect are improved;
2. the three-step wet wall breaking technology is adopted, so that the wall breaking effect of tea seed cells can be promoted, and the dissolution of oil and polyphenol can be promoted;
3. the composite biological enzyme technology is adopted to degrade protein and cellulose, so that the emulsification effect of the protein and polysaccharide on the tea oil can be reduced, and the extraction rate of the tea oil is promoted; meanwhile, the bound polyphenol is better exposed, and dissolution of the polyphenol in a later step is promoted;
4. the ultrasonic wave and electrolyte synergistic technology is adopted to perform demulsification on the feed liquid and promote the breakage of glycosidic bonds, the electrolyte can promote hydration degumming, and the synergistic effect of the ultrasonic wave and the electrolyte can cause the demulsification of the oil-tea camellia feed liquid and promote the breakage of the glycosidic bonds of the combined-state polyphenol so as to promote the release of the polyphenol;
5. the water medium method synchronous extraction can realize the synchronous extraction of tea oil, tea seed polypeptide and oil tea polysaccharide rich in polyphenol, improve the utilization rate of tea seed meal, reduce resource waste and improve the added value of products.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of embodiments of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a flow chart of the process for synchronously extracting polyphenol tea oil, tea-oil camellia polypeptide and tea-oil camellia polysaccharide provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. 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.
Referring to fig. 1, the present invention provides a process for synchronously extracting polyphenol tea oil, tea-oil camellia polypeptide and tea-oil camellia polysaccharide, wherein the process comprises the following steps:
s101, pretreating fresh tea seeds.
In the step, fresh tea seeds picked in the current year are used for hulling, and the hulling rate is controlled to be more than 95%. Wherein the storage period from picking to production processing of the fresh tea seeds is 0-90 days, the acid value is 0.6-0.8, the oil content is 40-45%, and the water content is 15-20%.
S102, performing wall breaking on the fresh tea seeds by a three-step wet method.
In the step, the unshelled fresh tea seeds are ground by a colloid mill, the grinding granularity is 60-80 meshes, then purified water is added according to a preset proportion, and after the mixture is uniformly mixed, a 120-150 mesh colloid mill is adopted to carry out two-step wall breaking; and finally homogenizing by adopting a homogenizer to obtain the tea seed mixed liquor.
Specifically, the specific operation steps of performing wall breaking on fresh tea seeds by adopting a three-step wet method are as follows:
grinding the fresh tea seeds subjected to shelling in a colloid mill, wherein the grinding granularity is 60-80 meshes, adding purified water according to the proportion of 1: 4-5, uniformly mixing, and performing two-step wall breaking by adopting a 120-150 mesh colloid mill; finally, homogenizing by a homogenizer to obtain a tea seed mixed solution; wherein the homogenizing pressure is 80-120 MPa, the homogenizing times are 2-3 times, and the mean temperature is 30-40 ℃.
S103, hydrolyzing by using compound biological enzyme.
In the step, the homogenized tea seed mixed solution is subjected to multi-step enzyme reaction to obtain a hydrolysate; wherein the multi-step enzyme reaction comprises the following steps in sequence: the first step is composite protease hydrolysis; the second step is the hydrolysis of flavourzyme; the third step is cellulase hydrolysis.
Specifically, the method for hydrolyzing by the compound biological enzyme comprises the following steps:
carrying out multi-step enzyme reaction on the homogenized tea seed mixed solution to obtain a hydrolysate; wherein, the first step is hydrolysis of the compound protease, the pH value is adjusted to 8.0-8.5, the temperature is 55-60 ℃, 600-800U/g of the compound protease is added, and the reaction time is 2-3 h; secondly, hydrolyzing the flavourzyme, adjusting the pH value to 7.5-8.0, adjusting the temperature to 55-60 ℃, adding 500-800U/g of flavourzyme, and reacting for 2-3 h; and the third step is cellulase hydrolysis, wherein the pH value is adjusted to 7.0-7.5, the temperature is 55-60 ℃, 400-500U/g of cellulase is added, and the reaction time is 3 hours.
And S104, breaking bonds by ultrasonic wave and electrolyte.
And (3) performing demulsification and glycosidic bond fracture treatment on the hydrolysate in the step S103, adding sodium chloride and sodium citrate as electrolytes, and performing demulsification under the ultrasonic condition to promote glycosidic bond fracture to finally obtain treated feed liquid.
Specifically, the method for breaking bonds by demulsification by using ultrasonic wave and electrolyte comprises the following steps:
demulsifying the hydrolysate obtained in the step S103 and breaking glycosidic bond, adding 1.5-2% of sodium chloride and 0.7-1% of sodium citrate as electrolytes, and performing ultrasonic treatmentDemulsifying to promote the breakage of glycosidic bonds to finally obtain the treated feed liquid, wherein the ultrasonic condition is 2000-3000W/m3The ultrasonic time is 5-7 min, and the ultrasonic temperature is 50-60 ℃.
And S105, synchronously leaching with warm water.
In the step, the treated feed liquid is heated and stirred, and then centrifugal separation is carried out, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides.
Specifically, the method for synchronously leaching by warm water comprises the following steps:
heating the treated feed liquid to 80-90 ℃, stirring for 30min, then carrying out centrifugal separation at the rotating speed of 6000-8000 r/min for 18-20 min, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides.
And S106, separating and purifying the crude tea oil by using a rotating membrane.
In the step, the crude tea oil rich in polyphenol is separated by adopting a rotating membrane so as to obtain the polyphenol tea oil by filtering.
Specifically, the method for separating and purifying the crude tea oil by the rotating membrane comprises the following steps:
filtering and separating the crude tea oil rich in polyphenol by adopting a rotating membrane to obtain polyphenol tea oil; wherein the filtration precision is 50-100 nm, the fluid temperature is 50-60 ℃, and the fluid pressure is 5-6 MPa.
S107, separating and purifying the aqueous solution rich in the oil tea polypeptide and the oil tea polysaccharide.
In the step, the water solution rich in the oil tea polypeptide and oil tea polysaccharide is separated and purified by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa so as to realize separation and purification of the polysaccharide and the polypeptide, and finally, freeze drying is carried out to obtain the oil tea polypeptide and the oil tea polysaccharide.
Specifically, the method for separating and purifying the aqueous solution rich in the camellia oleifera polypeptide and the camellia oleifera polysaccharide comprises the following steps:
separating and purifying the water solution rich in the oil tea polypeptide and oil tea polysaccharide by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa to realize separation and purification of polysaccharide and polypeptide, and finally freeze-drying to obtain the oil tea polypeptide and the oil tea polysaccharide; wherein the centrifugal pressure for separation and purification is I-2 MPa.
In the present invention, according to the above-mentioned process for synchronously extracting polyphenol tea oil, tea-oil camellia polypeptide and tea-oil camellia polysaccharide, the technical indexes of the prepared polyphenol tea oil, tea-oil camellia polypeptide and tea-oil camellia polysaccharide are shown in table 1:
table 1: technical indexes of polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide
Product(s) The yield is% Content of effective component
Polyphenol tea oil 35％ The polyphenol content is 36mg/g
Tea seed polypeptide 23.5％ The content of polypeptide is 75%
Oil tea polysaccharide 15.4％ The polysaccharide content is 65%
The process for synchronously extracting the polyphenol tea oil, the tea-oil tree polypeptide and the tea-oil tree polysaccharide provided by the invention has the following technical effects:
1. fresh tea seeds are used as raw materials, and different from other tea oil production technologies, the drying link of the tea seeds can be reduced, and chemical reactions such as oxidation of fatty acid, denaturation of protein, polymerization of polysaccharide and protein, combination of free phenol and protein/polysaccharide and the like in the tea seeds are reduced, so that the content of the free phenol and the subsequent proteolysis effect are improved;
2. the three-step wet wall breaking technology is adopted, so that the wall breaking effect of tea seed cells can be promoted, and the dissolution of oil and polyphenol can be promoted;
3. the composite biological enzyme technology is adopted to degrade protein and cellulose, so that the emulsification effect of the protein and polysaccharide on the tea oil can be reduced, and the extraction rate of the tea oil is promoted; meanwhile, the bound polyphenol is better exposed, and dissolution of the polyphenol in a later step is promoted;
4. the ultrasonic wave and electrolyte synergistic technology is adopted to perform demulsification on the feed liquid and promote the breakage of glycosidic bonds, the electrolyte can promote hydration degumming, and the synergistic effect of the ultrasonic wave and the electrolyte can cause the demulsification of the oil-tea camellia feed liquid and promote the breakage of the glycosidic bonds of the combined-state polyphenol so as to promote the release of the polyphenol;
5. the water medium method synchronous extraction can realize the synchronous extraction of tea oil, tea seed polypeptide and oil tea polysaccharide rich in polyphenol, improve the utilization rate of tea seed meal, reduce resource waste and improve the added value of products.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., 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.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims (8)

1. A process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide is characterized by comprising the following steps:
step one, pretreatment of fresh tea seeds:
selecting fresh tea seeds picked in the current year for hulling, wherein the hulling rate is controlled to be more than 95%;
step two, performing wall breaking on the fresh tea seeds by adopting a three-step wet method:
grinding the fresh tea seeds subjected to shelling in a colloid mill, wherein the grinding granularity is 60-80 meshes, adding purified water according to a preset proportion, uniformly mixing, and performing two-step wall breaking by adopting a 120-150 mesh colloid mill; finally, homogenizing by a homogenizer to obtain a tea seed mixed solution;
step three, hydrolyzing by using compound biological enzyme:
carrying out multi-step enzyme reaction on the homogenized tea seed mixed solution to obtain a hydrolysate; wherein the multi-step enzyme reaction comprises the following steps in sequence: the first step is composite protease hydrolysis; the second step is the hydrolysis of flavourzyme; the third step is cellulose hydrolysis;
fourthly, demulsifying and breaking bonds by ultrasonic wave and electrolyte:
demulsifying and breaking glycosidic bonds of the hydrolysate obtained in the third step, adding sodium chloride and sodium citrate as electrolytes, and demulsifying under the ultrasonic condition to promote the breaking of the glycosidic bonds to finally obtain treated feed liquid;
step five, synchronously leaching with warm water:
heating and stirring the treated feed liquid, then carrying out centrifugal separation, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides;
sixthly, separating and purifying the crude tea oil by using a rotating membrane:
separating the crude tea oil rich in polyphenol by using a rotating membrane to obtain polyphenol tea oil by filtering;
and seventhly, separating and purifying the aqueous solution rich in the oil tea polypeptide and the oil tea polysaccharide:
separating and purifying the water solution rich in the oil tea polypeptide and oil tea polysaccharide by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa to realize separation and purification of polysaccharide and polypeptide, and finally freeze-drying to obtain the oil tea polypeptide and the oil tea polysaccharide.
2. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the first step, the storage period from picking to production processing of fresh tea seeds is 0-90 days, the acid value is 0.6-0.8, the oil content is 40-45%, and the water content is 15-20%.
3. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the second step, the method for breaking the wall of fresh tea seeds by adopting a three-step wet method comprises the following steps:
grinding the fresh tea seeds subjected to shelling in a colloid mill, wherein the grinding granularity is 60-80 meshes, adding purified water according to the proportion of 1: 4-5, uniformly mixing, and performing two-step wall breaking by adopting a 120-150 mesh colloid mill; finally, homogenizing by a homogenizer to obtain a tea seed mixed solution; wherein the homogenizing pressure is 80-120 MPa, the homogenizing times are 2-3 times, and the mean temperature is 30-40 ℃.
4. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the third step, the method for compound biological enzyme hydrolysis comprises the following steps:
carrying out multi-step enzyme reaction on the homogenized tea seed mixed solution to obtain a hydrolysate; wherein, the first step is hydrolysis of the compound protease, the pH value is adjusted to 8.0-8.5, the temperature is 55-60 ℃, 600-800U/g of the compound protease is added, and the reaction time is 2-3 h; secondly, hydrolyzing the flavourzyme, adjusting the pH value to 7.5-8.0, adjusting the temperature to 55-60 ℃, adding 500-800U/g of flavourzyme, and reacting for 2-3 h; and the third step is cellulase hydrolysis, wherein the pH value is adjusted to 7.0-7.5, the temperature is 55-60 ℃, 400-500U/g of cellulase is added, and the reaction time is 3 hours.
5. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the fourth step, the method for breaking bonds by demulsification by ultrasonic wave in cooperation with electrolyte comprises the following steps:
demulsifying and breaking glycosidic bonds of the hydrolysate obtained in the third step, adding 1.5-2% of sodium chloride and 0.7-1% of sodium citrate as electrolytes, and demulsifying under the ultrasonic condition to promote the glycosidic bonds to break to finally obtain the processed feed liquid, wherein the ultrasonic condition is 2000-3000W/m3The ultrasonic time is 5-7 min, and the ultrasonic temperature is 50-60 ℃.
6. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the fifth step, the warm water synchronous leaching method comprises the following steps:
heating the treated feed liquid to 80-90 ℃, stirring for 30min, then carrying out centrifugal separation at the rotating speed of 6000-8000 r/min for 18-20 min, wherein the upper liquid obtained after centrifugal separation is tea oil crude oil rich in polyphenol, and the lower liquid is an aqueous solution rich in tea-oil polypeptides and tea-oil polysaccharides.
7. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the sixth step, the method for separating and purifying the crude tea oil by rotating membrane comprises the following steps:
filtering and separating the crude tea oil rich in polyphenol by adopting a rotating membrane to obtain polyphenol tea oil; wherein the filtration precision is 50-100 nm, the fluid temperature is 50-60 ℃, and the fluid pressure is 5-6 MPa.
8. The process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptides and tea-oil tree polysaccharides as claimed in claim 1, wherein in the seventh step, the method for separating and purifying the aqueous solution rich in tea-oil tree polypeptides and tea-oil tree polysaccharides comprises the following steps:
separating and purifying the water solution rich in the oil tea polypeptide and oil tea polysaccharide by adopting a ceramic membrane with the molecular weight cutoff of 10-15 kDa to realize separation and purification of polysaccharide and polypeptide, and finally freeze-drying to obtain the oil tea polypeptide and the oil tea polysaccharide; wherein the centrifugal pressure for separation and purification is I-2 MPa.
CN202111351707.3A 2021-11-15 2021-11-15 Process for synchronously extracting polyphenol tea oil, tea-oil tree polypeptide and tea-oil tree polysaccharide Pending CN114250112A (en)

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