CN108634311A - A kind of process of extraction tealeaves active material - Google Patents

A kind of process of extraction tealeaves active material Download PDF

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Publication number
CN108634311A
CN108634311A CN201810431314.5A CN201810431314A CN108634311A CN 108634311 A CN108634311 A CN 108634311A CN 201810431314 A CN201810431314 A CN 201810431314A CN 108634311 A CN108634311 A CN 108634311A
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China
Prior art keywords
active material
extraction
tea
acid
material according
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CN201810431314.5A
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Chinese (zh)
Inventor
吴迪
伍贤密
王超
王红利
李德斌
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Study On Selenium Resource Development By Ziyang County
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Study On Selenium Resource Development By Ziyang County
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Priority to CN201810431314.5A priority Critical patent/CN108634311A/en
Publication of CN108634311A publication Critical patent/CN108634311A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/163Liquid or semi-liquid tea extract preparations, e.g. gels, liquid extracts in solid capsules
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/166Addition of, or treatment with, enzymes or microorganisms
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/18Extraction of water soluble tea constituents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/125Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17Amino acids, peptides or proteins
    • A23L33/175Amino acids
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Mycology (AREA)
  • Nutrition Science (AREA)
  • Botany (AREA)
  • Dispersion Chemistry (AREA)
  • Microbiology (AREA)
  • Molecular Biology (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a kind of processes of extraction tealeaves active material, belong to tea product technical field.A kind of process of extraction tealeaves active material of the present invention is using water as solvent, using the active ingredient in ultrasonic wave extraction tealeaves, has many advantages, such as that extraction time is short, efficient, active material loss is few;Using three kinds of ion exchange resin separation theanine, tea polyphenols and tea polysaccharide active materials, resin material is reusable, has higher cost performance;Obtained extract purity is high, tea polysaccharide total sugar content >=72%;Purity >=99% of tea polyphenols;Purity >=85% of theanine.

Description

A kind of process of extraction tealeaves active material
Technical field
The invention belongs to tea product technical fields, and in particular to a kind of process of extraction tealeaves active material.
Background technology
The ingredient of 19 beginnings of the century, tealeaves just gradually clearly get up.By the separation and identification of modern science, contain in tealeaves Chemical machine ingredient is up to more than 450 kinds, and inorganic mineral element is up to more than 40 kinds.Organic chemical composition mainly has:Tea polyphenols, Vegetable soda, protein, amino acid, vitamin, pectin element, organic acid, lipopolysaccharides, carbohydrate, enzyme, pigment etc..Inorganic mineral member Element mainly has:Potassium, calcium, magnesium, cobalt, iron, aluminium, sodium, zinc, copper, nitrogen, phosphorus, fluorine, iodine, selenium etc..
With tealeaves research deepen continuously and with the intersection of medical research and infiltration, it has already been proven that theanine has anti- Tumour, promotes the medical functions such as nerve growth at hypertensive tranquilizing;Tea polyphenols have different physiological roles, it is not only good natural Antioxidant also has enhancing Abwehrkraft des Koepers, anti-cancer, antitumor, radioresistance, antibacterial, antiviral, hypoglycemic, reducing blood lipid, pre- Anti- angiocardiopathy, anti-aging, prevent skin it is ultraviolet damage etc. different physiological roles, grease, food, medicine, daily-use chemical industry, The fields such as light industry have broad prospect of application;Tea polysaccharide have a variety of physiological actions, as radiation protection, anticoagulation and antithrombotic, Hypoglycemic etc., it can also enhance body's immunity, experiments have shown that tea polysaccharide has blood pressure lowering, reducing heart rate, resist oxygen lack, increasing It the effects that adding coronary flow, can be with reducing blood lipid, anti arteriosclerosis, anti-inflammatory and anticancer etc..Therefore, safely and effectively from tea The ingredients such as theanine, tea polyphenols and tea polysaccharide are extracted and detached in leaf, and there is important practical significance.
That there are recovery rates is relatively low for the extracting mode of current tealeaves active material, solvent dosage is big, effective component extracts The disadvantages such as purity is low.
Invention content
In view of the above-mentioned problems, the present invention is based on ultrasonic wave extraction, ultrafiltration membrane technique and ion-exchange resin techniques to carry For a kind of process of energy-efficient extraction tealeaves active material.
In order to achieve the above objectives, technical solution proposed by the invention is:A kind of technique side of extraction tealeaves active material Method, it is characterised in that:Include the following steps:
1) 10-30 times of water is added in tea-leaf power, under ul-trasonic irradiation, in 60 DEG C of -80 DEG C of temperature ranges, every time 15-30 minutes, soak extraction 3-5 times repeatedly was separated by filtration to obtain tea extract;
2) tea extract is through being concentrated in vacuo, by concentrate and ethanol solution according to 1:3-1:5 volume ratios are uniformly mixed Merge stirring, polysaccharide precipitation and solution are respectively obtained after filtering;By polysaccharide precipitation water dissolution, pH value 1- is utilized after removing deproteinized 3 strong-acid cation-exchange resin is adsorbed and is detached, and obtains tea polysaccharide;
3) it by solution after Polyose extraction, adjusts pH3.5-5 to obtain film permeate and trapped fluid through ultrafiltration membrance filter with acid, cuts Stay liquid that filtrate and protein feed solid content is obtained by filtration through centrifuge;Filtrate is merged with film permeate, is then handed over cation It changes resin to extract, obtains the resin for being adsorbed with tea polyphenols and acidic aqueous solution;The cation for being adsorbed with tea polyphenols is exchanged Resin is added in absolute ethyl alcohol, is detached under being mixed slowly in 50-60 DEG C, by separation of ethanol liquid reverse osmosis membrane separation with it is dense Contracting, obtains film permeate and trapped fluid, trapped fluid obtains the distillate containing ethyl alcohol and tea polyphenols through low-temperature vacuum drying;
4) by distillate, adjustment pH value is 1-5, then passes through cation exchange resin column and carries out ion exchange, with 10% Concentration ammonium hydroxide elutes, and collects efflux, concentration, and theanine can be obtained in cooling, crystallization, drying.
Further scheme,
Separation solvent for use described in step 2 is any one in absolute ethyl alcohol, acetic acid, acetone.
Further scheme,
It is any one in hydrochloric acid, sulfuric acid and phosphoric acid that acid used in pH value is adjusted in the step 3.
Further scheme,
Ultrafiltration membrane in the step 3 selects aperture O.8-5 micron capillary tubular type ultrafiltration membrane, operating pressure 1.2- 1.6Mpa。
Further scheme,
Efflux in step 4 by ammonium hydroxide elution is concentrated into 1/3-1/5.
Further scheme,
Described in step 2 except deproteinized method be basic protein enzymatic isolation method, basic protein enzyme amount used be 1600- 2000U/g。
Further scheme,
The enzymatic isolation method process conditions are:PH value 9-10,25-30 DEG C of temperature, time 45-75min.
Advantageous effect:
1) a kind of process of extraction tealeaves active material of the invention is using water as solvent, using ultrasonic wave extraction tealeaves In active ingredient, have many advantages, such as that extraction time is short, the loss of efficient, active material is few;
2) a kind of process of extraction tealeaves active material of the invention is using ion exchange resin separation theanine, tea Three kinds of active materials of polyphenol and tea polysaccharide, resin material is reusable, has higher cost performance;
3) a kind of process of extraction tealeaves active material of the invention removes tea leaf protein with enzymatic isolation method, has efficient The advantage of environmental protection;
4) extract purity that a kind of process of extraction tealeaves active material of the invention obtains is high, tea polysaccharide total reducing sugar Content >=72%;Purity >=99% of tea polyphenols;Purity >=85% of theanine.
Specific implementation mode
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below to the specific reality of the present invention The mode of applying elaborates.Many details are elaborated in the following description in order to fully understand the present invention.But this Invention can be much to implement different from other manner described here, and those skilled in the art can be without prejudice to the present invention Similar improvement is done in the case of intension, therefore the present invention is not limited by following public specific implementation mode.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) 10 times of water is added in tea-leaf power, under ul-trasonic irradiation, in 80 DEG C of temperature ranges, 15 minutes every time, instead Multiple soak extraction 5 times, is separated by filtration to obtain tea extract;
2) tea extract is through being concentrated in vacuo, by concentrate and absolute ethyl alcohol according to 1:3 volume ratios are uniformly mixed and stirred for, Polysaccharide precipitation and solution are respectively obtained after filtering;By polysaccharide precipitation water dissolution;With 1600U/g alkali proteases, process conditions For pH value 10,25 DEG C of temperature, the time, 45min removed removing protein;It adsorbs and detaches using the strong-acid cation-exchange resin of pH value 1, Obtain tea polysaccharide;
3) by solution after Polyose extraction, film permeate and trapped fluid are obtained through ultrafiltration membrance filter with sulfuric acid tune pH3.5, is cut Stay liquid that filtrate and protein feed solid content is obtained by filtration through centrifuge;Filtrate is merged with film permeate, is then handed over cation It changes resin to extract, obtains the resin for being adsorbed with tea polyphenols and acidic aqueous solution;The cation for being adsorbed with tea polyphenols is exchanged Resin is added in absolute ethyl alcohol, is detached under being mixed slowly in 50 DEG C, by separation of ethanol liquid reverse osmosis membrane separation and is concentrated, Film permeate and trapped fluid are obtained, trapped fluid obtains the distillate containing ethyl alcohol and tea polyphenols through low-temperature vacuum drying;
4) by distillate, adjustment pH value is 1, then passes through cation exchange resin column and carries out ion exchange, dense with 10% Ammonium hydroxide elution is spent, efflux, concentration are collected, theanine can be obtained in cooling, crystallization, drying.
Embodiment 2
1) 30 times of water is added in tea-leaf power, under ul-trasonic irradiation, in 60 DEG C of temperature ranges, 30 minutes every time, instead Multiple soak extraction 3 times, is separated by filtration to obtain tea extract;
2) tea extract is through being concentrated in vacuo, by concentrate and acetic acid according to 1:5 volume ratios are uniformly mixed and stirred for, filtering After respectively obtain polysaccharide precipitation and solution;By polysaccharide precipitation water dissolution;With 2000U/g alkali proteases, process conditions PH Value 9,30 DEG C of temperature, the time, 75min removed removing protein;It adsorbs and detaches using the strong-acid cation-exchange resin of pH value 3, obtain tea Polysaccharide;
3) by solution after Polyose extraction, film permeate and trapped fluid are obtained through ultrafiltration membrance filter with phosphoric acid tune pH5, is retained Filtrate and protein feed solid content is obtained by filtration through centrifuge in liquid;Filtrate is merged with film permeate, is then exchanged with cation Resin extracts, and obtains the resin for being adsorbed with tea polyphenols and acidic aqueous solution;The cation exchange tree of tea polyphenols will be adsorbed with Fat is added in absolute ethyl alcohol, is detached under being mixed slowly in 60 DEG C, and separation of ethanol liquid reverse osmosis membrane separation and concentration obtain To film permeate and trapped fluid, trapped fluid obtains the distillate containing ethyl alcohol and tea polyphenols through low-temperature vacuum drying;
4) by distillate, adjustment pH value is 5, then passes through cation exchange resin column and carries out ion exchange, dense with 10% Ammonium hydroxide elution is spent, efflux, concentration are collected, theanine can be obtained in cooling, crystallization, drying.
Embodiment 3
1) 20 times of water is added in tea-leaf power, under ul-trasonic irradiation, in 70 DEG C of temperature ranges, 25 minutes every time, instead Multiple soak extraction 4 times, is separated by filtration to obtain tea extract;
2) tea extract is through being concentrated in vacuo, by concentrate and acetone according to 1:4 volume ratios are uniformly mixed and stirred for, filtering After respectively obtain polysaccharide precipitation and solution;By polysaccharide precipitation water dissolution;With 1800U/g alkali proteases, process conditions PH Value 9.5,28 DEG C of temperature, the time, 60min removed removing protein;It adsorbs and detaches using the strong-acid cation-exchange resin of pH value 2, obtain Tea polysaccharide;
3) by solution after Polyose extraction, film permeate and trapped fluid are obtained through ultrafiltration membrance filter with sulfuric acid tune pH4, is retained Filtrate and protein feed solid content is obtained by filtration through centrifuge in liquid;Filtrate is merged with film permeate, is then exchanged with cation Resin extracts, and obtains the resin for being adsorbed with tea polyphenols and acidic aqueous solution;The cation exchange tree of tea polyphenols will be adsorbed with Fat is added in absolute ethyl alcohol, is detached under being mixed slowly in 55 DEG C, and separation of ethanol liquid reverse osmosis membrane separation and concentration obtain To film permeate and trapped fluid, trapped fluid obtains the distillate containing ethyl alcohol and tea polyphenols through low-temperature vacuum drying;
4) by distillate, adjustment pH value is 3, then passes through cation exchange resin column and carries out ion exchange, dense with 10% Ammonium hydroxide elution is spent, efflux, concentration are collected, theanine can be obtained in cooling, crystallization, drying.
Although hereinbefore having been made with reference to some embodiments, present invention is described, do not departing from the present invention's In the case of range, it can be carried out various improvement and can use it is equivalent without replacement technology point therein, especially, as long as There is no technical contradiction, the various features in the various embodiments of institute's careless mistake of the present invention can be combined by either type and be made It is only in omitting length and economize on resources with, the description that the case where not combined in the present invention to these carries out exhaustive row Consider.Therefore, the invention is not limited in specific embodiments disclosed herein, and include falling into claim.

Claims (7)

1. a kind of process of extraction tealeaves active material, is crushed to 30-50 mesh by tealeaves first, it is characterised in that:Method The step of it is as follows:
1) 10-30 times of water is added in tea-leaf power, under ul-trasonic irradiation, in 60 DEG C of -80 DEG C of temperature ranges, each 15-30 Minute, soak extraction 3-5 times repeatedly is separated by filtration to obtain tea extract;
2) tea extract is through being concentrated in vacuo, by concentrate and solvent according to 1:3-1:5 volume ratios are uniformly mixed and stirred for, filtering After respectively obtain polysaccharide precipitation and solution;By polysaccharide precipitation water dissolution, except the strong-acid cation for utilizing pH value 1-3 after deproteinized Exchanger resin is adsorbed and is detached, and obtains tea polysaccharide;
3) by solution after Polyose extraction, pH3.5-5 is adjusted to obtain film permeate and trapped fluid, trapped fluid through ultrafiltration membrance filter with acid Filtrate and protein feed solid content is obtained by filtration through centrifuge;Filtrate is merged with film permeate, then uses cation exchange tree Fat extracts, and obtains the resin for being adsorbed with tea polyphenols and acidic aqueous solution;The cation exchange resin of tea polyphenols will be adsorbed with It is added in absolute ethyl alcohol, is detached under being mixed slowly in 50-60 DEG C, by separation of ethanol liquid reverse osmosis membrane separation and concentrated, Film permeate and trapped fluid are obtained, trapped fluid obtains the distillate containing ethyl alcohol and tea polyphenols through low-temperature vacuum drying;
4) by distillate, adjustment pH value is 1-5, then passes through cation exchange resin column and carries out ion exchange, with 10% concentration Ammonium hydroxide elutes, and collects efflux, concentration, and theanine can be obtained in cooling, crystallization, drying.
2. a kind of process of extraction tealeaves active material according to claim 1, it is characterised in that:Institute in step 2 The separation solvent for use stated is any one in absolute ethyl alcohol, acetic acid, acetone.
3. a kind of process of extraction tealeaves active material according to claim 1, it is characterised in that:The step 3 Acid used in middle adjusting pH value is any one in hydrochloric acid, sulfuric acid and phosphoric acid.
4. a kind of process of extraction tealeaves active material according to claim 1, it is characterised in that:The step 3 In ultrafiltration membrane select aperture O.8-5 micron capillary tubular type ultrafiltration membrane, operating pressure 1.2-1.6Mpa.
5. a kind of process of extraction tealeaves active material according to claim 1, it is characterised in that:The step 4 The middle efflux by ammonium hydroxide elution is concentrated into 1/3-1/5.
6. a kind of process of extraction tealeaves active material according to claim 1, it is characterised in that:The removing The method of albumen is basic protein enzymatic isolation method, and basic protein enzyme amount used is 1600-2000U/g.
7. a kind of process of extraction tealeaves active material according to claim 6, it is characterised in that:The enzymolysis Method process conditions are:PH value 9-10,25-30 DEG C of temperature, time 45-75min.
CN201810431314.5A 2018-05-08 2018-05-08 A kind of process of extraction tealeaves active material Pending CN108634311A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113845991A (en) * 2021-10-20 2021-12-28 泸州老窖股份有限公司 Tea wine and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1557841A (en) * 2004-01-14 2004-12-29 中国农业科学院茶叶研究所 Process for synthetic extraction of polysaccharides, tea-polyphenol, theanine, caffeine from tea
CN101020649A (en) * 2007-03-12 2007-08-22 江南大学 Process of separating and purifying natural theanine
CN104926680A (en) * 2015-05-08 2015-09-23 李会杰 Method for extracting bio-active substances from low-grade tea and tea-manufacturing leftovers
CN106543023A (en) * 2016-11-04 2017-03-29 湖北宇隆茶业有限责任公司 The processing method of the extracting method and tealeaf residue of tea polyphenols and theanine in tea old leaf

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1557841A (en) * 2004-01-14 2004-12-29 中国农业科学院茶叶研究所 Process for synthetic extraction of polysaccharides, tea-polyphenol, theanine, caffeine from tea
CN101020649A (en) * 2007-03-12 2007-08-22 江南大学 Process of separating and purifying natural theanine
CN104926680A (en) * 2015-05-08 2015-09-23 李会杰 Method for extracting bio-active substances from low-grade tea and tea-manufacturing leftovers
CN106543023A (en) * 2016-11-04 2017-03-29 湖北宇隆茶业有限责任公司 The processing method of the extracting method and tealeaf residue of tea polyphenols and theanine in tea old leaf

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Title
中国环境科学学会: "《中国环境科学学会学术年会论文集 2009 第4卷》", 30 June 2009, 北京航空航天大学出版社 *
曹博: "茶多酚、茶多糖和茶氨酸的综合提纯研究", 《中国优秀硕士学位论文全文数据库》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113845991A (en) * 2021-10-20 2021-12-28 泸州老窖股份有限公司 Tea wine and preparation method thereof
CN113845991B (en) * 2021-10-20 2024-03-12 泸州老窖股份有限公司 Tea wine and preparation method thereof

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