CN103599256B - A kind of spraying extraction binding resin legal system that utilizes is for the method for tea-polyphenol - Google Patents
A kind of spraying extraction binding resin legal system that utilizes is for the method for tea-polyphenol Download PDFInfo
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- CN103599256B CN103599256B CN201310521486.9A CN201310521486A CN103599256B CN 103599256 B CN103599256 B CN 103599256B CN 201310521486 A CN201310521486 A CN 201310521486A CN 103599256 B CN103599256 B CN 103599256B
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- polyphenol
- tealeaves
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Abstract
Utilize spraying to extract binding resin legal system for a method for tea-polyphenol, first tealeaves is removed impurity, pulverize; Then extract with water spray; Extracting solution adds mineral acid adjust ph, leaves standstill and makes the abundant sedimentation of precipitate, with the solid impurity occurred after centrifuging removing acidifying; The tea-polyphenol obtaining high-content is separated further by upper resin column; Concentrating under reduced pressure obtains medicinal extract, obtains tea-polyphenol finished product with micro-wave drying method.Efficiency of the present invention is high, effectively can utilize tea resources, and tealeaves utilization ratio is up to 95%, and solvent load is little, with short production cycle, equipment investment is little, running cost is low.
Description
Technical field
The present invention relates to active ingredient of natural plant extraction and separation technology field, particularly a kind of spraying extraction binding resin legal system that utilizes is for the method for tea-polyphenol.
Background technology
Tea-polyphenol is the general name of Polyphenols of Tea, tool removing toxic substances and radiation resistance, radioactive substance effectively can be stoped to invade marrow, and strontium 90 and Co 60 can be made to excrete rapidly, be described as " radiation jinx " by healthy and medical circle.Anticancer, prevention and cure of cardiovascular disease, raising combined immune power, anti peroxidation of lipid, anti-aging, heavy metal salt and the alkalotic anti-solution effect of biology in advance, antiradiation injury, alleviate the untoward reaction of radiotherapy; The effect of preventing decayed tooth permanent tooth and removing halitosis; Digestion-aid effect; Contribute to beauty and skin care; Can keep the original local flavor of food in cake and milk-product making, anti-corruption, prolongs storage period, suppress and kill bacteria, fresh fruit and vegetables spray the tea-polyphenol solution of lower concentration, just can breed by anti-bacteria, keep fruit, the original color of vegetables, reach the object of preservation and antisepsis.Therefore, the extraction process studying tea-polyphenol has certain practical significance.Traditional extracting method is: high temperature water extraction is in conjunction with extraction into ethyl acetate method, and this is also the main method preparing tea-polyphenol at present.Weak point is that Extracting temperature is too high, make the destruction that the main active ingredient in tealeaves is at high temperature subject in various degree, extraction yield be low, tealeaves waste is large, the time is long, energy consumption compared with high, consumption of organic solvent is large.This technique is dispersed into through the effect of high pressure spraying machine by tealeaves fine powder vaporificly to spray in extractor, and water then flows into extractor from bottom under high-pressure.Considerably increase the contact area of tealeaves and Extraction solvent in whole leaching process, fully by the effective constituent stripping in tealeaves, and can realize extract at low temperature.Spray method is used for greatly in dry materials, up to the present there is not yet the report extracting tea-polyphenol by spray method.
Summary of the invention
The invention provides a kind of spraying extraction method that utilizes and prepare the technique of tea-polyphenol, solve that the extraction yield existed in prior art is low, tealeaves waste is large, time long, the more high defect of energy consumption, and the effective constituent in tea raw material can be extracted to greatest extent.
In order to achieve the above object, technical scheme of the present invention is achieved in that
Utilize spraying to extract binding resin legal system for a method for tea-polyphenol, comprise the following steps:
Step one: tealeaves pre-treatment
After tealeaves being removed impurity and limb, be placed in pulverizer and pulverize, cross 80-100 eye mesh screen, stand-by;
Step 2: spraying is extracted
Step one gained tealeaves fine powder is placed in stirred pot, add in the water of 4-6 times amount, abundant stirring, gained feed liquid is dispersed into through the effect of high pressure spraying machine and vaporificly sprays in extractor, water then flows into extractor from bottom under high-pressure, the ratio of tea-leaf power and water is 1:4-6, and the pressure of high pressure spraying machine is 2.0-5.0 MPas, and flow velocity is 500-800L/h;
Step 3: centrifugal or filtering separation
Extracting solution, by centrifugal or filtering separation, obtains clear liquid;
Step 4: acid is heavy, centrifugal
Extracting solution is added dilute hydrochloric acid or dilute sulphuric acid adjust ph is 2.0-5.0, standing 24h makes precipitate fully precipitate, with the solid impurity occurred after centrifuging removing acidifying;
Step 5: upper prop is separated
The lx-20 resin handled well is evenly loaded in resin column, the clarified liq of step 4 gained is slowly poured in resin column, when adsorbing saturated, stop adding liquid, then with the washing impurity of 2-4 times of bed volume, then adsorb with the ethanolysis of 80%, Fractional Collections is containing the component of tea-polyphenol;
Step 6: alcohol eluen concentrated and dry
Alcohol eluen, through being evaporated to without alcohol, adopts vacuum-drying, spraying dry or microwave drying to obtain tea-polyphenol finished product.
Extraction efficiency of the present invention is high, be conducive to making full use of of tea resources, especially to the utilization of tealeaf residue, both effectively make use of the tea dust produced in tealeaves making processes, tealeaf residue utilization ratio is up to 95%, extract completely, and solvent load is little, with short production cycle, equipment investment is little, running cost is low.
The present invention compared with prior art has the following advantages: 1. make tea-polyphenol contained in tealeaves starting material obtain extraction and application to greatest extent, traditional technique extraction yield is low, tealeaves waste is large, and use this Technology that tealeaf residue utilization ratio can be made up to more than 95%, reduce further production cost.2. the rate of recovery of product is elevated to 85% by original 50%, and can obtain the higher tea-polyphenol of purity, and content can reach more than 98%.3. decrease traditional extraction destruction to tea-polyphenol in heat-processed, effectively raise the rate of recovery of tea-polyphenol.4. significantly reduce " waste vapour, waste water, the waste residue " quantity discharged in production process, the demand of the resources such as the organic solvent in production, water vapor significantly reduces, and reduces energy consumption, reduces air, water resource pollution, maintain good ecotope.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment one:
The present embodiment comprises the following steps:
Step one: tealeaves pre-treatment
After tealeaves being removed impurity and limb, be placed in pulverizer and pulverize, cross 80 eye mesh screens, stand-by;
Step 2: spraying is extracted
Step one gained tea-leaf power is placed in stirred pot, add the water of 6 times amount, abundant stirring, gained feed liquid is dispersed into through the effect of high pressure spraying machine and vaporificly sprays in extractor, water then flows into extractor from bottom under high-pressure, the pressure of high pressure spraying machine is 3.0 MPas, and flow velocity is 600L/h;
Step 3: centrifugal or filtering separation
By centrifugal or filtering separation, obtain extracting solution;
Step 4: acid is heavy
Extracting solution being added dilute hydrochloric acid adjust ph is 3.0, then leaves standstill and precipitate is fully precipitated, with the solid impurity occurred after centrifuging removing acidifying;
Step 5: upper prop is separated
Evenly loaded in resin column by the lx-20 resin handled well, slowly poured in resin column by the clarified liq of step 4 gained, the water adsorbing saturated rear use 3 times of bed volumes carries out washing impurity, with the ethanol elution of 80%, and Fractional Collections effluent liquid;
Step 6: alcohol eluen concentrated and dry
Alcohol eluen, through being evaporated to without alcohol, adopts vacuum-drying to obtain tea-polyphenol finished product.
The present embodiment assay
In high effective liquid chromatography for measuring sample, polyphenol content is 98.2%
Embodiment two:
The present embodiment comprises the following steps:
Step one: tealeaves pre-treatment
After tealeaves being removed impurity and limb, the pulverizer being placed in 100 eye mesh screens is pulverized;
Step 2: spraying is extracted
Step one gained tea-leaf power is placed in stirred pot, add the water of 5 times amount, abundant stirring, gained feed liquid is dispersed into through the effect of high pressure spraying machine and vaporificly sprays in extractor, water then flows into transfer tank from bottom under high-pressure, the pressure of high pressure spraying machine is 4.0 MPas, and flow velocity is 700/h;
Step 3: centrifugal or filtering separation
By centrifugal or filtering separation, extracting solution can be obtained;
Step 4: acid is heavy
Extracting solution being added salt acid for adjusting pH value is 4.5, then leaves standstill and precipitate is fully precipitated, with the solid impurity occurred after centrifuging removing acidifying;
Step 5: upper prop is separated
Evenly loaded in resin column by the lx-20 resin handled well, slowly poured in resin column by the clarified liq of step 4 gained, the water adsorbing saturated rear use 3 times of bed volumes is washed.Finally use the ethanol elution of 80%, and Fractional Collections effluent liquid;
Step 6: alcohol eluen concentrated and dry
Alcohol eluen, through being evaporated to without alcohol, adopts vacuum-drying to obtain tea-polyphenol finished product.
The present embodiment assay
In high effective liquid chromatography for measuring sample, polyphenol content is 98.6%
Embodiment three:
The present embodiment comprises the following steps:
Step one: tealeaves pre-treatment
After tealeaves being removed impurity and limb, be placed in pulverizer and pulverize, cross 100 eye mesh screens, stand-by;
Step 2: spraying is extracted
Step one gained tea-leaf power is placed in stirred pot, add the water of 6 times amount, abundant stirring, gained feed liquid is dispersed into through the effect of high pressure spraying machine and vaporificly sprays in extractor, water then flows into extractor from bottom under high-pressure, the pressure of high pressure spraying machine is 5.0 MPas, and flow velocity is 800L/h;
Step 3: centrifugal or filtering separation
By centrifugal or filtering separation, obtain extracting solution;
Step 4: acid is heavy
Extracting solution being added dilute hydrochloric acid adjust ph is 5.0, then leaves standstill and precipitate is fully precipitated, with the solid impurity occurred after centrifuging removing acidifying;
Step 5: upper prop is separated
Evenly loaded in resin column by the lx-20 resin handled well, slowly poured in resin column by the clarified liq of step 4 gained, the water adsorbing saturated rear use 4 times of bed volumes carries out washing impurity, with the ethanol elution of 80%, and Fractional Collections effluent liquid;
Step 6: alcohol eluen concentrated and dry
Alcohol eluen, through being evaporated to without alcohol, adopts vacuum-drying to obtain tea-polyphenol finished product.
The present embodiment assay
In Tartrate-Fe method working sample, the content of tea-polyphenol is higher than 98%
In high effective liquid chromatography for measuring sample, the content of EGCG is 50%
The above; only three better case study on implementation of the present invention; the any restriction not made the present invention, every any simple modification, change, imitation done above case study on implementation for the technology of the present invention content all belongs to the protection domain of technical solution of the present invention.
Claims (1)
1. utilize spraying to extract binding resin legal system for a method for tea-polyphenol, it is characterized in that, comprise the following steps:
Step one: tealeaves pre-treatment
After tealeaves being removed impurity and limb, be placed in pulverizer and pulverize, cross 80-100 eye mesh screen, stand-by;
Step 2: spraying is extracted
Step one gained tealeaves fine powder is placed in stirred pot, add in the water of 4-6 times amount, abundant stirring, gained feed liquid is dispersed into through the effect of high pressure spraying machine and vaporificly sprays in extractor, water then flows into extractor from bottom under high-pressure, the ratio of tea-leaf power and water is 1:4-6, and the pressure of high pressure spraying machine is 2.0-5.0 MPas, and flow velocity is 500-800L/h;
Step 3: centrifugal or filtering separation
Extracting solution, by centrifugal or filtering separation, obtains clear liquid;
Step 4: acid is heavy, centrifugal
Extracting solution is added dilute hydrochloric acid or dilute sulphuric acid adjust ph is 2.0-5.0, standing 24h makes precipitate fully precipitate, with the solid impurity occurred after centrifuging removing acidifying;
Step 5: upper prop is separated
The lx-20 resin handled well is evenly loaded in resin column, the clarified liq of step 4 gained is slowly poured in resin column, when adsorbing saturated, stop adding liquid, then with the washing impurity of 2-4 times of bed volume, then adsorb with the ethanolysis of 80%, Fractional Collections is containing the component of tea-polyphenol;
Step 6: alcohol eluen concentrated and dry
Alcohol eluen, through being evaporated to without alcohol, adopts vacuum-drying, spraying dry or microwave drying to obtain tea-polyphenol finished product.
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| CN201310521486.9A CN103599256B (en) | 2013-10-29 | 2013-10-29 | A kind of spraying extraction binding resin legal system that utilizes is for the method for tea-polyphenol |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562995A (en) * | 2004-04-02 | 2005-01-12 | 胡绍海 | Left ofloxacin and Pidotimod compound preparation tech and its appts. |
| CN1651424A (en) * | 2004-11-25 | 2005-08-10 | 三达膜科技（厦门）有限公司 | Production method of high purity tea polyphenol and caffeine |
| CN101190276A (en) * | 2007-12-14 | 2008-06-04 | 广西大学 | Method for separating and extracting sweet tea tannins |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562995A (en) * | 2004-04-02 | 2005-01-12 | 胡绍海 | Left ofloxacin and Pidotimod compound preparation tech and its appts. |
| CN1651424A (en) * | 2004-11-25 | 2005-08-10 | 三达膜科技（厦门）有限公司 | Production method of high purity tea polyphenol and caffeine |
| CN101190276A (en) * | 2007-12-14 | 2008-06-04 | 广西大学 | Method for separating and extracting sweet tea tannins |
Non-Patent Citations (1)
| Title |
|---|
| 树脂静态吸附法生产茶多酚初步试验;黄秋森等;《福建林业科技》;20090325;第36卷(第01期);35-38 * |
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