CN103833795B - A kind of method extracting low levels tea-polyphenol from fresh tea leaf in its - Google Patents
A kind of method extracting low levels tea-polyphenol from fresh tea leaf in its Download PDFInfo
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Abstract
The invention discloses a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its, belong to natural product chemistry technical field, specifically comprise the following steps: S1. soaks; S2. centrifugal; S3. membrane concentration; S4. evaporation concentration; S5. spraying dry; S6. deironing.The present invention adopts fresh tea leaf in its to be raw material, easy gelatinization when overcoming in traditional technology at high temperature lixiviate after adopting stem tea to pulverize and sieve, the shortcoming of not easily filtering, do medium with purified water and directly isolate low levels tea-polyphenol, decrease the leaching of some fat-soluble agricultural chemicals, low levels tea-polyphenol product polyphenol content prepared by the inventive method is up to 50%, and caffeine is up to 8%, appearance luster oyster, for instant product, water-soluble rear clarity of solution is high, and soup look emerald green.This method has simple to operate, that separation efficiency is high, cost is low, with short production cycle advantage, is applicable to batch production scale operation.
Description
Technical field
The invention belongs to natural product chemistry technical field, be specifically related to a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its.
Background technology
Tea-polyphenol (Teapolyphenols, TP) is a kind of new type natural antioxidant extracted from tealeaves, has anticancer, anti-ageing, a series of important pharmacological function such as radioprotective, removing human free radical, hypoglycemic blood fat.Have broad application prospects in fields such as grease, food, medicine, daily use chemicals.The mixture of the multiple catechin monomers of tea-polyphenol system, wherein having activeconstituents that is anti-oxidant, anticancer and removing interior free yl is nutgall catechin gallic acid ester (epigallocatechingallate, EGCG), it by universally acknowledged for being " the optimal cancer therapy drug extracted from natural phant after taxol ".In October, 2006, food and drug administration (FDA) ratifies tea-polyphenol as new prescription drugs, treats for local (outside) Genital warts caused by human papillomavirus.This is first plant (draft) medicine of FDA according to medicine amendment regulations approval listing in 1962.
Low levels tea-polyphenol refers to that in product, polyphenol content is up to 50%, and caffeine is up to 8%, and low levels tea-polyphenol is applicable to the industries such as food hot drink, cake, is applicable to Grown living.
The traditional method preparing tea-polyphenol from tealeaves is mainly following three classes:
1. tealeaves polar solvent floods by solvent-extraction process, then carries out liquid-liquid extraction separation closely getting liquid, finally concentrates and obtains product.Current suitability for industrialized production mainly adopts this method.Product yield 5%-10%, product purity is 80%-98%.Solvent for use has acetone, ether, methyl alcohol, hexane and trichloromethane etc.This method production cost is high, and easily pollutes.
2. ion catch electron microscopy precipitated metal tea-polyphenol, makes it be separated with trimethyl-xanthine, the method uses the heavy metal poisonous to human body and makes precipitation agent, so the product difficulty of producing by this method reaches the requirement of food and medicine industry.
3. post is separated the key of preparation method technique is column packed material and drip washing.Research shows, adopt post to be separated preparation method, tea-polyphenol yield is between 4%-8%, and purity can reach 98%, but column packed material is very expensive, and with multiple and a large amount of organic solvent during drip washing, is obviously not suitable for suitability for industrialized production.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its be provided, this method have simple to operate, separation efficiency is high, cost is low, with short production cycle, the advantage of energy-conserving and environment-protective.
Object of the present invention is achieved through the following technical solutions: a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its, and it comprises the following steps:
S1. soak: fresh tea leaf in its is placed in extraction unit, add purified water constant temperature and soak 1.8 ~ 2.5h, the mixed solution in extraction unit is crossed 18 ~ 24 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 65 ~ 100 DEG C;
S2. centrifugal: filtrate to be placed in temperature is 30 ~ 50 DEG C, pressure is centrifugal 50 ~ 70s under the environment of 0.2 ~ 0.4MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 6500 ~ 7000 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, be concentrated into solid content >=20%;
S4. evaporation concentration: concentrated solution is heated to temperature >=75 DEG C, evaporation concentration is 40 ~ 50% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 160 ~ 220 DEG C, air outlet temperature 75 ~ 100 DEG C, the feed pressure 15 ~ 20MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, crosses 50 ~ 90 mesh sieves, uses magnet adsorption deironing, mixed by powder after deironing, again sieve, magnet adsorption deironing, obtained low levels tea-polyphenol.
Further, the weight ratio of fresh tea leaf in its described in step S1 and purified water is 1:5 ~ 8.
Further, the magnetic force of magnet described in step S6 is 10000 ~ 15000 Gausses.
The present invention has the following advantages:
1. the present invention adopts fresh tea leaf in its to be raw material, easy gelatinization when overcoming in traditional technology at high temperature lixiviate after adopting stem tea to pulverize and sieve, the shortcoming of not easily filtering;
2. do medium with purified water and directly isolate low levels tea-polyphenol, decrease the leaching of some fat-soluble agricultural chemicals; Overcome in traditional technology and adopt organic solvent leaching residual to bring the healthy disadvantageous problem of people in the product;
3. in purifying process, do not adopt column chromatography, therefore, significantly reduce production cost; When decreasing column chromatography drip washing, required a large amount of water and solvent, have the characteristic of energy-conserving and environment-protective;
4. the low levels tea-polyphenol product that prepared by the inventive method detects known polyphenol content through great many of experiments and is up to 50%, and caffeine is up to 8%, and product appearance light yellow in color is green, and be instant product, water-soluble rear clarity of solution is high, and soup look emerald green.
5. this method has simple to operate, that separation efficiency is high, cost is low, with short production cycle advantage, is applicable to batch production scale operation.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated.
Embodiment 1: a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in extraction unit, adds purified water 10000kg, constant temperature soaks 1.8h, the mixed solution in extraction unit is crossed 18 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 65 DEG C;
S2. centrifugal: filtrate to be placed in temperature is 50 DEG C, pressure is centrifugal 50s under the environment of 0.2MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 6500 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, being concentrated into solid content is 20%;
S4. evaporation concentration: concentrated solution is heated to 75 DEG C, evaporation concentration is 40% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 160 DEG C, air outlet temperature 75 DEG C, the feed pressure 15MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, cross 50 mesh sieves, be the magnet adsorption deironing of 10000 Gausses, mixed by powder, again sieve after deironing, magnet adsorption deironing with magnetic force, obtained content is 46.8% tea-polyphenol 230kg.
Embodiment 2: a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in extraction unit, adds purified water 16000kg, constant temperature soaks 2.5h, the mixed solution in extraction unit is crossed 24 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 100 DEG C;
S2. centrifugal: filtrate to be placed in temperature is 50 DEG C, pressure is centrifugal 70s under the environment of 0.4MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 7000 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, being concentrated into solid content is 30%;
S4. evaporation concentration: concentrated solution is heated to 85 DEG C, evaporation concentration is 50% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 160 DEG C, air outlet temperature 75 DEG C, the feed pressure 15MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, cross 90 mesh sieves, be the magnet adsorption deironing of 15000 Gausses, mixed by powder, again sieve after deironing, magnet adsorption deironing with magnetic force, obtained content is 46.2% tea-polyphenol 240kg.
Embodiment 3: a kind of method extracting low levels tea-polyphenol from fresh tea leaf in its, it comprises the following steps:
S1. soak: fresh tea leaf in its 2000kg is placed in extraction unit, adds purified water 12000kg, constant temperature soaks 2h, the mixed solution in extraction unit is crossed 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 80 DEG C;
S2. centrifugal: filtrate to be placed in temperature is 40 DEG C, pressure is centrifugal 60s under the environment of 0.3MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 6800 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, being concentrated into solid content is 40%;
S4. evaporation concentration: concentrated solution is heated to 90 DEG C, evaporation concentration is 45% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 180 DEG C, air outlet temperature 88 DEG C, the feed pressure 18MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, cross 80 mesh sieves, be the magnet adsorption deironing of 12000 Gausses, mixed by powder, again sieve after deironing, magnet adsorption deironing with magnetic force, obtained content is 47.2% tea-polyphenol 237kg.
Embodiment 4: simultaneous test
1. from Fresh Folium Camelliae sinensis, extract low levels tea-polyphenol:
S1. soak: fresh tea leaf in its 300g is placed in extraction unit, adds purified water 2100g, constant temperature soaks 2.2h, the mixed solution in extraction unit is crossed 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 85 DEG C;
S2. centrifugal: filtrate to be placed in temperature is 45 DEG C, pressure is centrifugal 60s under the environment of 0.25MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 6700 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, being concentrated into solid content is 40%;
S4. evaporation concentration: concentrated solution is heated to 85 DEG C, evaporation concentration is 42% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 170 DEG C, air outlet temperature 90 DEG C, the feed pressure 17MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, crosses 60 mesh sieves, is the magnet adsorption deironing of 12000 Gausses, is mixed by powder, again sieve after deironing, magnet adsorption deironing with magnetic force, obtained low levels tea-polyphenol.
2. from stem tea, extract tea-polyphenol:
Extracting method: S1. soaks: be 300g by stem tea 150g(weight in wet base) be placed in extraction unit, add purified water 2100g, constant temperature soaks 2.2h, the mixed solution in extraction unit is crossed 20 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 85 DEG C;
All the other steps are with experiment 1.
3. detect: the weight of accurate weighing above-mentioned experiment 1,2 products obtained therefrom, adopt following method to measure caffeine, tea-polyphenol, the content of EGCG and the yield of extract in product.
(1) measuring method:
A. the content of caffeine, EGCG adopts the analysis of HPLC method, and chromatographic condition is:
Chromatographic column: C184.6 × 150mm;
Moving phase: water: methyl alcohol: phosphoric acid (77:23:0.1);
Flow velocity: 1.0ml/min;
Wavelength: 280nm;
Column temperature: 30 DEG C;
A. the preparation of standardized solution: learn from else's experience Vanadium Pentoxide in FLAKES green tea control sample (standards calibration through caffeine, the EGCG one-component) 25mg of dry more than 24 hours, accurately weighed, put in 50ml volumetric flask, add water about 40ml, and supersound process makes it dissolve completely, lets cool to room temperature, scale is settled to water, shake up, be the filtering with microporous membrane of 0.45 μm with aperture, obtain final product.
B. need testing solution preparation: precision takes tea leaf extract 25mg, puts 50ml(or 100ml) in volumetric flask, adding water ultrasonicly in right amount makes it dissolve, and taking-up lets cool, and adds water and is settled to scale, shakes up, and is the filtering with microporous membrane of 0.45 μm, obtains final product with aperture.
C. measure: accurate absorption standardized solution and each 20 μ l of need testing solution respectively, inject liquid chromatograph, measure, to obtain final product.
D. result calculates
The content of each component is calculated by following formula:
Each component (%)=(A
sample× C
contrast× V × Fi)/(A
contrast× W) × 100%
In formula: W--sample weight, mg; A
sample--sample peak area; A
contrast--reference substance peak area; C
contrast--reference substance concentration, mg/ml; V--test liquid volume, ml; Each component of Fi--contains coefficient of discharge through what calibrate.
B. the detection method of tea-polyphenol:
A. preparation of reagents:
Ferrous tartrate reagent: ferrous sulfate 1g and 5g Seignette salt, after water dissolution, be settled to 1000ml, and solution should keep in Dark Place.
Phosphate buffered saline buffer:
Sodium phosphate dibasic: take 23.377g Sodium phosphate dibasic, with constant volume after water dissolution in 1000ml.
Potassium primary phosphate: take 9.078g potassium primary phosphate (roasting 2 hours at 105 DEG C) by water dissolution after be settled to 1000ml.
Get after above-mentioned disodium phosphate soln 85ml and potassium dihydrogen phosphate 15ml mixes respectively, be pH7.5 phosphate buffered saline buffer.
B. the preparation of test liquid and mensuration:
Standby for trial-production: precise 100mg green tea extract is to 100ml volumetric flask, add 80ml purified water ultrasonic to dissolving completely, let cool to room temperature, add purified water constant volume, shake up, and accurate 1ml solution of drawing is in 25ml volumetric flask, add 4ml water and 5ml ferrous tartrate solution, fully mix, then the phosphate buffered saline buffer adding pH7.5 is settled to scale, shake up, to obtain final product.
C. measure: measure with spectrophotometer (UV), make reference with blank, measure absorbancy (A) at 540nm place.
D. result calculates: the content obtaining tea-polyphenol by following formula.
Tea-polyphenol (%)=A × 2.88 × 100/m × 100%
In formula: m---example weight (mg); A----absorbancy; 2.88----tea-polyphenol uptake factor.
C. the calculating of extraction yield: yield (%)=product weight/tealeaves weight in wet base × 100% of extract
(2) experimental result: as shown in table 1:
Table 1: the simultaneous test extracting low levels tea-polyphenol from stem tea and Fresh Folium Camelliae sinensis
As known from Table 1: the content of caffeine adopting fresh tea leaf in its to extract low levels tea-polyphenol products obtained therefrom is 6.8%, , EGCG content is 15.1%, the yield of extract is 13%, and the content of caffeine adopting stem tea to extract low levels tea-polyphenol products obtained therefrom is 6.5%, EGCG content is 13.6%, the yield of extract is 10%, all lower than employing fresh tea leaf in its extraction method, and adopt fresh tea leaf in its extraction products obtained therefrom polyphenol content to be 45.3%, little with employing cured leaf extraction method products obtained therefrom polyphenol content difference, illustrate that the method adopting fresh leaf to extract low levels tea-polyphenol is significantly better than adopting cured leaf extraction method.
Claims (1)
1. from fresh tea leaf in its, extract a method for low levels tea-polyphenol product, it is characterized in that, it comprises the following steps:
S1. soak: fresh tea leaf in its is placed in extraction unit, add purified water constant temperature and soak 1.8 ~ 2.5h, the mixed solution in extraction unit is crossed 18 ~ 24 mesh sieves, obtains filtrate; Wherein, described constant temperature soaking temperature is 65 ~ 100 DEG C; The weight ratio of described fresh tea leaf in its and purified water is 1:5 ~ 8;
S2. centrifugal: filtrate to be placed in temperature is 30 ~ 50 DEG C, pressure is centrifugal 50 ~ 70s under the environment of 0.2 ~ 0.4MPa, discard precipitation, centrifugate is used for next-step operation; Wherein, the rotating speed of described whizzer is 6500 ~ 7000 turns/min;
S3. membrane concentration: adopt molecular retention amount be 100 reverse osmosis membrane concentrate centrifugate, be concentrated into solid content >=20%;
S4. evaporation concentration: concentrated solution is heated to temperature >=75 DEG C, evaporation concentration is 40 ~ 50% to solid content, is cooled to normal temperature;
S5. spraying dry: concentrated solution step S4 evaporation concentration crossed carries out spraying dry, controls inlet temperature 160 ~ 220 DEG C, air outlet temperature 75 ~ 100 DEG C, the feed pressure 15 ~ 20MPa of spray-drier;
S6. deironing: pulverized by spraying dry gained solid pulverizer, crosses 50 ~ 90 mesh sieves, is the magnet adsorption deironing of 10000 ~ 15000 Gausses, is mixed by powder, again sieve after deironing, magnet adsorption deironing with magnetic force, obtained low levels tea-polyphenol product.
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| CN1634914A (en) * | 2004-11-23 | 2005-07-06 | 三达膜科技（厦门）有限公司 | Method for producing high pure tea polyphenol with low caffeine |
| CN101971901A (en) * | 2010-11-12 | 2011-02-16 | 安徽农业大学 | Method for preparing high-tea-polyphenol instant tea |
| CN102077882A (en) * | 2010-12-14 | 2011-06-01 | 广州泽力医药科技有限公司 | Technology for preparing high content tea polyphenol using water as single solvent |
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| CN1634914A (en) * | 2004-11-23 | 2005-07-06 | 三达膜科技（厦门）有限公司 | Method for producing high pure tea polyphenol with low caffeine |
| CN101971901A (en) * | 2010-11-12 | 2011-02-16 | 安徽农业大学 | Method for preparing high-tea-polyphenol instant tea |
| CN102077882A (en) * | 2010-12-14 | 2011-06-01 | 广州泽力医药科技有限公司 | Technology for preparing high content tea polyphenol using water as single solvent |
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Denomination of invention: A Method for Extracting Low Content Tea Polyphenols from Fresh Tea Effective date of registration: 20230922 Granted publication date: 20160427 Pledgee: Zhejiang Mintai Commercial Bank Co.,Ltd. Chengdu Pujiang Branch Pledgor: CHENGDU WAGOTT BIO-TECH Co.,Ltd. Registration number: Y2023980058447 |