CN106390911A - Method for preparing volcanic stone adsorbent and method for enriching catechin antioxidants - Google Patents
Method for preparing volcanic stone adsorbent and method for enriching catechin antioxidants Download PDFInfo
- Publication number
- CN106390911A CN106390911A CN201610703128.3A CN201610703128A CN106390911A CN 106390911 A CN106390911 A CN 106390911A CN 201610703128 A CN201610703128 A CN 201610703128A CN 106390911 A CN106390911 A CN 106390911A
- Authority
- CN
- China
- Prior art keywords
- pelelith
- catechin
- ethanol solution
- adsorbent
- mesh
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
Abstract
The invention provides a method for preparing a volcanic stone adsorbent and a method for enriching catechin antioxidants, and the method for preparing the volcanic stone adsorbent includes the following steps: providing 24 mesh to 40 mesh volcano stone particles; using a citric acid aqueous solution for soaking the volcano stone particles for some time, washing and drying the volcano stone particles; and using an ethanol solution for soaking the dried volcano stone particles, washing and drying to obtain the granular volcano stone adsorbent. The method for preparing the volcanic stone adsorbent has the advantages that the adsorbent is made by use of the characteristics of being porous and hard in texture of natural volcanic stones without use of toxic and harmful chemical solvents, an adsorption column is not easy to block, and adsorption and elution efficiency are high.
Description
Technical field
The present invention relates to natural separation preparation field, more particularly, to a kind of method preparing pelelith adsorbent
And the method for enrichment catechin antioxidant.
Background technology
Catechin antioxidant is to extract the one group of polyphenol compound obtaining from tealeaves, has good antioxygen
Multiple physiological active functionses such as change, radioresistance, prevention cardiovascular and cerebrovascular disease and prevention cancerous swelling, are widely used in functional food and guarantor
In strong medicine.
The preparation of tea catechin class antioxidant typically adopts calcium ions precipitate, organic solvent to separate, overcritical dioxy
Change the methods such as carbon extraction or column chromatography for separation.But every kind of method all has certain defect, for example, calcium precipitation is easy
Catechin is caused to aoxidize, purity reduces；There is chemical residue in Batteries by Organic Solvent Partition Process；Supercritical carbon dioxide extraction method becomes
This height；There is chemical residual when in column chromatography for separation method with chemical synthesis resin for adsorbent, and use lignocellulosic to be suction
Easily make chromatographic column blocking lead to elution efficiency low problem when attached dose because quality is soft.
Therefore, need a kind of method of new enrichment catechin antioxidant badly.
Content of the invention
The technical problem to be solved is to provide a kind of method preparing pelelith adsorbent and enrichment catechin
The method of class antioxidant, it can obtain the catechin antioxidant of no chemical residues, and adsorbs and elution efficiency height.
In order to solve the above problems, the invention provides a kind of method preparing pelelith adsorbent, comprise the steps：
24 mesh～40 mesh pelelith particles are provided；
The described pelelith particle some time is soaked using aqueous citric acid solution, and rinses and dry；
Pelelith particle after being dried using alcohol solution dipping, and rinse and dry, obtain the absorption of graininess pelelith
Agent.
Further, described 24 mesh～40 mesh pelelith particles sequentially pass through coarse crushing, fine crushing and acquisition of sieving.
Further, pelelith particle described in described aqueous citric acid solution submergence, soaks described fire using aqueous citric acid solution
The time of mountain stone particle is 12 hours～24 hours.
Further, pelelith particle described in described ethanol solution submergence.
Further, the concentration of described ethanol solution is 50%～90%, the pelelith after being dried using alcohol solution dipping
The time of particle is 12 hours～24 hours.
Further, in the baking step carrying out respectively after aqueous citric acid solution and alcohol solution dipping, drying temperature is
100～110 DEG C.
The present invention also provides a kind of method of enrichment catechin antioxidant, comprises the steps：
Millet paste is provided；
The pelelith adsorbent of above-mentioned preparation method preparation is loaded adsorption column；
Described millet paste is flowed through described adsorption column adsorbed；
Elute described adsorption column with ethanol solution, and collect the ethanol solution after wash-out, obtain and contain catechin antioxygen
The ethanol solution of agent；
Concentrate the described ethanol solution containing catechin antioxidant, and be dried, obtain catechin anti-oxidant
Agent.
Further, described millet paste volume is 3～10 times of described absorption column volume.
Further, after described millet paste flows through described adsorption column, described adsorption column is rinsed with pure water, until non-pigment
Flow out.
Further, elute in described adsorption column step with ethanol solution, the concentration of described ethanol solution is 50%～95%.
Further, in the step concentrating the described ethanol solution containing catechin antioxidant, catechin will be contained
The ethanol solution rotary evaporation inspissator of class antioxidant is evaporated to solid concentration 30%～50% at 40-45 DEG C.
It is an advantage of the current invention that utilizing natural pelelith porous and scleroid feature making adsorbent, do not use
Poisonous and harmful chemical solvent, adsorption column is not easy to be blocked, and absorption and elution efficiency are high.
Specific embodiment
Below the present invention is provided prepares the method for pelelith adsorbent and the method for enrichment catechin antioxidant
Specific embodiment elaborate.
A kind of method preparing pelelith adsorbent of the present invention, comprises the steps：
(1) 24 mesh～40 mesh pelelith particles are provided.
The method obtaining described 24 mesh～40 mesh pelelith particles is：
(10) bulk pelelith for example, is smashed formation 1cm～3cm crushed stone using iron hammer by pelelith described in coarse crushing.
(11) 1cm～3cm pelelith crushed stone for example, is pulverized granulating using pulverizer by pelelith described in fine crushing
Spend less pelelith particle or powder.
(12) sieve, for example, with sieve priority sub-sieve pelelith particle and the powder of 24 mesh and 40 mesh, take on 24 mesh, 40
Now 24 mesh～40 mesh pelelith particles are used for subsequent technique.
(2) adopt aqueous citric acid solution to soak the described 24 mesh～40 mesh pelelith particle some times, and rinse and dry.
The concentration of described aqueous citric acid solution is 10g/L～20g/L, and its consumption is aqueous citric acid solution submergence pelelith
Grain, for example, the volume of described aqueous citric acid solution can be 1 with the volume ratio of described pelelith particle:1、2:1、3:1、
4:1、5:1 etc., soak time be 12～24h, such as 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24
Hour.After immersion finishes, remove aqueous citric acid solution with filtered through gauze, with distilled water flushing pelelith particle to non-pigment stream
Go out, dry at 100～110 DEG C.
(3) adopt the pelelith particle after alcohol solution dipping drying, and rinse and dry, obtain graininess pelelith and inhale
Attached dose.
The concentration of described ethanol solution is 50%～90%, for example, 50%, 60%, 70%, 80%, 90%, using ethanol
Solution soak dry after pelelith particle time be 12 hours～24 hours, such as 12 hours, 14 hours, 16 hours, 18
Hour, 20 hours, 22 hours, 24 hours.Preferably, ethanol solution just pelelith particulate matter described in submergence.After immersion finishes,
Remove ethanol solution with filtered through gauze, flowed out with distilled water flushing pelelith particle to non-pigment, dry at 100～110 DEG C, obtain
To graininess pelelith adsorbent.
Pelelith is the nature of glass acidity volcano effusive rock of a kind of porous, lightweight, and its chemical composition is mainly SiO2、Al2O3
And contain multiple transition metal oxides, have that specific surface area is big, light weight, quality are hard, anticorrosive the features such as.Present invention profit
With natural pelelith porous and scleroid feature make adsorbent, do not use poisonous and harmful chemical solvent, adsorption column is not allowed
Easily blocked, absorption is high with elution efficiency.
The present invention also provides a kind of method of enrichment catechin antioxidant, comprises the steps：
(1) provide millet paste.
The acquisition methods of described millet paste are as follows：The tealeaves that will be dried, such as green tea, with the extracting in boiling water of 10～20 times of weight
30～60min；Remove tea grounds with filtered through gauze, collect millet paste and be cooled to room temperature；By millet paste under 4000～10000rpm rotating speed
Centrifugation 15～30min, takes millet paste supernatant to be used in follow-up enrichment catechin antioxidant technique as millet paste.
(2) the pelelith adsorbent preparing the method being prepared pelelith adsorbent using the present invention is loaded in adsorption column.
(3) described millet paste is flowed through described adsorption column to be adsorbed.
The volume of described millet paste is absorption 3-10 times of column volume, for example, 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times,
10 times.Further, after described millet paste all flows through adsorption column, substitute millet paste with pure water and clean described adsorbate to non-pigment stream
Go out.
(4) elute described adsorption column with ethanol solution, and collect the ethanol solution after wash-out, obtain and resist containing catechin
The ethanol solution of oxidant.
Preferably, the concentration of described ethanol solution be 50%～95%, for example, 50%, 60%, 70%, 80%, 90%,
95%.
(5) concentrate the described ethanol solution containing catechin antioxidant, and be dried, obtain catechin antioxygen
Agent.
Described in concentrating, the method for the ethanol solution containing catechin antioxidant is, will be containing catechin antioxidant
Ethanol solution rotary evaporation inspissator be evaporated to solid concentration 30%～50% at 40-45 DEG C.Thing after concentration
Powder catechin antioxidant is obtained after matter is spray-dried.Tea catechin class with the method enrichment of present invention enrichment
The catechin total content of antioxidant is 758.03～802.84mg/g.
Several embodiments that the present invention be enriched with the method for catechin antioxidant are set forth below, to further illustrate this
Bright advantage.
Embodiment 1：A kind of method being enriched with catechin antioxidant from steaming green tea soup.
(1) adsorbent preparation
Take natural 3 pieces of pelelith (5.6kg), smashed with iron hammer to the crushed stone of 1cm～3cm；With pulverizer by fire
Mountain stone is ground into powder；With 24 mesh sieve sub-sieves；The derrick stone of compass screen surface is continued to pulverize up to whole mistake 24 mesh sieves；Use 40 mesh
Screening sieve, removes the powder that granularity is less than 40 mesh, obtains the pelelith particle that 4.8kg granularity is 24 mesh～40 mesh.
Soak pelelith particle with aqueous citric acid solution (concentration is 10g/L), be the just submergence of aqueous citric acid solution consumption
Pelelith particle is defined, and soak time is 24h；Remove aqueous citric acid solution with filtered through gauze, with distilled water flushing volcano stone flour
Flow out to non-pigment, dry at 100～110 DEG C.
The pelelith particle of drying is immersed in 90% ethanol solution, ethanol solution consumption is with just submergence pelelith
Particle is defined；Soak time 20h；Remove ethanol solution with filtered through gauze, with distilled water flushing pelelith particle to non-pigment stream
Till going out, dry at 100～110 DEG C.The pelelith particle being dried is used as the adsorbent of column chromatography.
(2) millet paste preparation
Take steaming green tea 1500g 15L boiling water extraction 60min, remove tea grounds with filtered through gauze, collect millet paste and be cooled to
Room temperature；Millet paste is centrifuged 30min under 4000rpm rotating speed, obtains supernatant 11.5L, for the absorption point of catechin antioxidant
From and enrichment.
(3) absorption method enrichment millet paste catechin antioxidant
The pelelith granule adsorbent that step (1) is obtained loads adsorption column (diameter 7.0cm, high 95cm)；By step (2)
The whole millet paste supernatants obtaining pour into from adsorption column top and flow through the adsorbent of adsorption column；Treat that millet paste solution all passes through
Afterwards, poured into above adsorption column with 10.0L pure water and flow through adsorption column and be carried out, when efflux non-pigment, use 10.0L
95% ethanol solution wash-out adsorption column, collects the ethanol solution flowing out below adsorption column, obtains and contain catechin antioxidant
Ethanol solution (9.5L)；Ethanol solution is transferred to rotary evaporator and is concentrated into about 420mL in 40-45 DEG C of reduction vaporization, with
Mini Spray-Drier is spray-dried, and obtains 105.6g catechin antioxidant powder.
The sample repeating for 2 times to test detects through HPLC, the catechin of the powder catechin antioxidant of acquisition is total
Content is 802.84 ± 20.51mg/g (table 1).
Powder catechin antioxidant catechin content (mg/g) that table 1. embodiment 1 obtains
Wherein, SD:Standard deviation (standard deviation)；GC:Gallocatechin (gallic acid catechu
Element)；EGC:Epigallocatechin (epi-nutgall acid catechin)；C:Catechin (catechuic acid)；EC:epicatechin
(epicatechin)；EGCG:Epigallocatechin gallate (EGCG)；GCG:
Gallocatechin gallate (gallate-based catechin and gallate)；ECG:Epicatechin gallate (table catechu
Plain gallate)；CG:Catechin gallate (catechin and gallate).
Embodiment 2：A kind of method being enriched with catechin antioxidant from baked green tea soup.
(1) adsorbent preparation
Take 2 pieces of pelelith (5.2kg), smashed with iron hammer to the crushed stone of 1cm～3cm；With pulverizer by pelelith
Block is ground into particle and powder, with 24 mesh sieve sub-sieves, the derrick stone of compass screen surface is continued to pulverize up to whole mistake 24 mesh sieves；With 40
Mesh sieve sub-sieve passes through the particle of 24 mesh, removes the powder at 40 mesh sieve bottoms, obtains the pelelith that 4.3kg granularity is 24 mesh～40 mesh
Grain.
Soak pelelith particle with aqueous citric acid solution (15g/L), its consumption is with aqueous citric acid solution just submergence volcano
Stone particle is defined, and keeps 20h；Remove aqueous citric acid solution with filtered through gauze, with distilled water flushing volcano stone flour to non-pigment stream
Go out, dry at 100～110 DEG C.
The pelelith particle of drying is immersed in 70% ethanol solution, ethanol solution consumption is with just submergence pelelith
Particle is defined；Soak time 24h；Remove ethanol solution with filtered through gauze, with distilled water flushing pelelith particle to non-pigment stream
Till going out, dry at 100～110 DEG C.The pelelith particle being dried is used as the adsorbent of column chromatography.
(2) millet paste preparation
Take baked green tea 1500g 30L boiling water extraction 30min, remove tea grounds with filtered through gauze, collect millet paste and be cooled to
Room temperature；Millet paste is centrifuged 15min in 10000rpm, obtains millet paste supernatant 23.7L, for catechin antioxidant adsorbing separation
And enrichment.
(3) absorption method enrichment millet paste catechin antioxidant
The graininess pelelith adsorbent that step (1) is obtained loads adsorption column (diameter 7.0cm, high 95cm)；By step
(2) the whole millet paste supernatants obtaining pour into from adsorption column top and flow through the adsorbent of adsorption column；Treat that millet paste solution all leads to
Later, poured into above adsorption column with 10.0L pure water and flow through adsorption column and be carried out, when efflux non-pigment, use
10.0L 75% ethanol solution elutes adsorption column, collects the ethanol solution flowing out below adsorption column, obtains and resists containing catechin
The ethanol solution (9.8L) of oxidant；Ethanol solution is transferred to rotary evaporator be concentrated into about in 40-45 DEG C of reduction vaporization
440mL, is spray-dried with Mini Spray-Drier, obtains 123.4g catechin antioxidant powder.
The sample repeating for 2 times to test detects through HPLC, the catechin of the powder catechin antioxidant of acquisition is total
Content is 758.03 ± 4.78mg/g (table 2).
Powder catechin antioxidant catechin content (mg/g) that table 2. embodiment 2 obtains
Wherein, SD:Standard deviation (standard deviation)；GC:Gallocatechin (gallic acid catechu
Element)；EGC:Epigallocatechin (epi-nutgall acid catechin)；C:Catechin (catechuic acid)；EC:epicatechin
(epicatechin)；EGCG:Epigallocatechin gallate (EGCG)；GCG:
Gallocatechin gallate (gallate-based catechin and gallate)；ECG:Epicatechin gallate (table catechu
Plain gallate)；CG:Catechin gallate (catechin and gallate).
Embodiment 3：A kind of method being enriched with catechin antioxidant from roasted green tea soup
(1) adsorbent preparation
Take 3 pieces of pelelith (6.2kg), smashed with iron hammer to the crushed stone of 1cm～3cm, with pulverizer by pelelith
Block is ground into powder, with 24 mesh sieve sub-sieves, the derrick stone of compass screen surface is continued to pulverize up to whole mistake 24 mesh sieves；Divided with 40 mesh sieves
The particle by 24 mesh for the sieve, removes the powder at 40 mesh sieve bottoms, obtains the graininess pelelith that 5.3kg granularity is 24 mesh～40 mesh.
Soak pelelith particle with aqueous citric acid solution (10g/L), its consumption is with aqueous citric acid solution just submergence volcano
Stone particle is defined, and keeps 12h；Remove aqueous citric acid solution with filtered through gauze, extremely colourless with distilled water flushing pelelith particulate matter
Till element flows out, dry at 100～110 DEG C.
The pelelith particle of drying is immersed in 50% ethanol solution, ethanol solution consumption is with just submergence pelelith
Particle is defined；Soak time 12h；Remove ethanol solution with filtered through gauze, with distilled water flushing pelelith particle to non-pigment stream
Till going out, dry at 100～110 DEG C.The pelelith particle being dried is used as the adsorbent of column chromatography.
(2) millet paste preparation
Take roasted green tea 1500g 20L boiling water extraction 45min, remove tea grounds with filtered through gauze, collect millet paste and be cooled to room
Temperature；Millet paste is centrifuged 20min in 8000rpm, obtains supernatant 14.6L, for catechin antioxidant adsorbing separation and enrichment.
(3) absorption method enrichment millet paste catechin antioxidant
The pelelith granule adsorbent that step (1) is obtained loads adsorption column (diameter 7.0cm, high 95cm)；By step (2)
Whole millet paste supernatants of 2 acquisitions pour into from adsorption column top and flow through the adsorbent of adsorption column；Treat that millet paste solution all passes through
Afterwards, poured into above adsorption column with 10.0L pure water and flow through adsorption column and be carried out, when efflux non-pigment, use 10.0L
50% ethanol solution wash-out adsorption column, collects the ethanol solution flowing out below adsorption column, obtains and contain catechin antioxidant
Ethanol solution (10.2L)；Ethanol solution is transferred to rotary evaporator and is concentrated into about 480mL in 40-45 DEG C of reduction vaporization, use
Mini Spray-Drier is spray-dried, and obtains 102.8g powder catechin antioxidant.
The sample repeating for 2 times to test detects through HPLC, the catechin of the powder catechin antioxidant of acquisition is total
Content is 773.19 ± 2.39mg/g (table 3).
Powder catechin antioxidant catechin content (mg/g) that table 3. embodiment 3 obtains
Wherein, SD:Standard deviation (standard deviation)；GC:Gallocatechin (gallic acid catechu
Element)；EGC:Epigallocatechin (epi-nutgall acid catechin)；C:Catechin (catechuic acid)；EC:epicatechin
(epicatechin)；EGCG:Epigallocatechin gallate (EGCG)；GCG:
Gallocatechin gallate (gallate-based catechin and gallate)；ECG:Epicatechin gallate (table catechu
Plain gallate)；CG:Catechin gallate (catechin and gallate).
Embodiment 4：A kind of method being enriched with catechin antioxidant from steaming green tea dust tea soup
(1) adsorbent preparation
Take 2 pieces of pelelith (5.5kg), smashed with iron hammer to the crushed stone of 1cm～3cm, with pulverizer by pelelith
Block is ground into powder, with 24 mesh sieve sub-sieves, the derrick stone of compass screen surface is continued to pulverize up to whole mistake 24 mesh sieves；Divided with 40 mesh sieves
The particle by 24 mesh for the sieve, removes the powder at 40 mesh sieve bottoms, obtains the graininess pelelith that 4.3kg granularity is 24 mesh～40 mesh.
Soak pelelith particle with aqueous citric acid solution (20g/L), its consumption is with aqueous citric acid solution just submergence volcano
Stone particle is defined, and keeps 18h；Remove aqueous citric acid solution with filtered through gauze, extremely colourless with distilled water flushing pelelith particulate matter
Till element flows out, dry at 100～110 DEG C.
The pelelith particle of drying is immersed in 60% ethanol solution, ethanol solution consumption is with just submergence pelelith
Particle is defined；Soak time 18h；Remove ethanol solution with filtered through gauze, with distilled water flushing pelelith particle to non-pigment stream
Till going out, dry at 100～110 DEG C.The pelelith particle being dried is used as the adsorbent of column chromatography.
(2) millet paste preparation
Take steaming green tea end (granular size 60 mesh -80 mesh) 1500g 30L boiling water extraction that steaming green tea process produces
Take 35min, remove tea grounds with filtered through gauze, collect millet paste and be cooled to room temperature；Millet paste is centrifuged 20min in 10000rpm, obtains
Clear liquid 20.7L, for catechin antioxidant adsorbing separation and enrichment.
(3) absorption method enrichment millet paste catechin antioxidant
The pelelith granule adsorbent that step (1) is obtained loads adsorption column (diameter 7.0cm, high 95cm)；By step (2)
Whole millet paste supernatants of 2 acquisitions pour into from adsorption column top and flow through the adsorbent of adsorption column；Treat that millet paste solution all passes through
Afterwards, poured into above adsorption column with 10.0L pure water and flow through adsorption column and be carried out, when efflux non-pigment, use 10.0L
75% ethanol solution wash-out adsorption column, collects the ethanol solution flowing out below adsorption column, obtains and contain catechin antioxidant
Ethanol solution (9.3L)；Ethanol solution is transferred to rotary evaporator and is concentrated into about 460mL in 40-45 DEG C of reduction vaporization, use
Mini Spray-Drier is spray-dried, and obtains 109.4g powder catechin antioxidant.
The sample repeating for 2 times to test detects through HPLC, the catechin of the powder catechin antioxidant of acquisition is total
Content is 773.19 ± 2.39mg/g (table 4).
Powder catechin antioxidant catechin content (mg/g) that table 4. embodiment 4 obtains
Wherein, SD:Standard deviation (standard deviation)；GC:Gallocatechin (gallic acid catechu
Element)；EGC:Epigallocatechin (epi-nutgall acid catechin)；C:Catechin (catechuic acid)；EC:epicatechin
(epicatechin)；EGCG:Epigallocatechin gallate (EGCG)；GCG:
Gallocatechin gallate (gallate-based catechin and gallate)；ECG:Epicatechin gallate (table catechu
Plain gallate)；CG:Catechin gallate (catechin and gallate).
The above is only the preferred embodiment of the present invention it is noted that ordinary skill people for the art
Member, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (10)
1. a kind of method preparing pelelith adsorbent is it is characterised in that comprise the steps：
24 mesh～40 mesh pelelith particles are provided；
The described pelelith particle some time is soaked using aqueous citric acid solution, and rinses and dry；
Pelelith particle after being dried using alcohol solution dipping, and rinse and dry, obtain graininess pelelith adsorbent.
2. the method preparing pelelith adsorbent according to claim 1 is it is characterised in that described 24 mesh～40 mesh volcanoes
Stone particle sequentially passes through coarse crushing, fine crushing and acquisition of sieving.
3. the method preparing pelelith adsorbent according to claim 1 is it is characterised in that described aqueous citric acid solution soaks
Do not have described pelelith particle, be 12 hours～24 hours using the time that aqueous citric acid solution soaks described pelelith particle.
4. the method preparing pelelith adsorbent according to claim 1 is it is characterised in that described ethanol solution submergence institute
State pelelith particle, the concentration of described ethanol solution is 50%～90%, the pelelith after drying using alcohol solution dipping
The time of grain is 12 hours～24 hours.
5. the method preparing pelelith adsorbent according to claim 1 is it is characterised in that in aqueous citric acid solution and second
In the baking step that alcoholic solution is carried out after soaking respectively, drying temperature is 100～110 DEG C.
6. a kind of method of enrichment catechin antioxidant is it is characterised in that comprise the steps：
Millet paste is provided；
The pelelith adsorbent of preparation method according to claim 1 preparation is loaded adsorption column；
Described millet paste is flowed through described adsorption column adsorbed；
Elute described adsorption column with ethanol solution, and collect the ethanol solution after wash-out, obtain and contain catechin antioxidant
Ethanol solution；
Concentrate the described ethanol solution containing catechin antioxidant, and be dried, obtain catechin antioxidant.
7. the method for enrichment catechin antioxidant according to claim 6 is it is characterised in that described millet paste volume is
3～10 times of described absorption column volume.
8. the method for enrichment catechin antioxidant according to claim 7 is it is characterised in that flow through in described millet paste
After described adsorption column, described adsorption column is rinsed, until non-pigment flows out.
9. the method for enrichment catechin antioxidant according to claim 6 is it is characterised in that eluted with ethanol solution
In described adsorption column step, the concentration of described ethanol solution is 50%～95%.
10. the method for enrichment catechin antioxidant according to claim 6 is it is characterised in that containing described in concentration
Have in the step of ethanol solution of catechin antioxidant, the ethanol solution containing catechin antioxidant is steamed with rotation
Send out inspissator and be evaporated to solid concentration 30%～50% at 40-45 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610703128.3A CN106390911B (en) | 2016-08-22 | 2016-08-22 | The method for preparing the method for pelelith adsorbent and being enriched with catechin antioxidant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610703128.3A CN106390911B (en) | 2016-08-22 | 2016-08-22 | The method for preparing the method for pelelith adsorbent and being enriched with catechin antioxidant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106390911A true CN106390911A (en) | 2017-02-15 |
| CN106390911B CN106390911B (en) | 2019-10-22 |
Family
ID=58005191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610703128.3A Active CN106390911B (en) | 2016-08-22 | 2016-08-22 | The method for preparing the method for pelelith adsorbent and being enriched with catechin antioxidant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106390911B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107349914A (en) * | 2017-09-03 | 2017-11-17 | 郑州坤博科技有限公司 | A kind of high-performance adsorbent for Industrial Wastewater Treatment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4331694A (en) * | 1978-12-26 | 1982-05-25 | Union Carbide Corporation | Removal of caffeine by selective adsorption using zeolite adsorbents |
| CN101798355A (en) * | 2010-04-08 | 2010-08-11 | 晋江市恒源科技开发有限公司 | Method for integrated separation and extraction of tea polysaccharide, theanine, polyphenol and caffeine |
| CN102701308A (en) * | 2012-06-12 | 2012-10-03 | 黑龙江省科学院火山与矿泉研究所 | Method for removing organic matters and metal ions in raw mineral water of five connective ponds |
| CN105688929A (en) * | 2016-01-08 | 2016-06-22 | 广州市佳境水处理技术工程有限公司 | Neutral advanced oxidation catalyst with pelelith as carrier and preparing method of neutral advanced oxidation catalyst |
| CN105756295A (en) * | 2016-03-04 | 2016-07-13 | 同济大学 | Urban rainwater recycling reutilization system based on lava rocks |
-
2016
- 2016-08-22 CN CN201610703128.3A patent/CN106390911B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4331694A (en) * | 1978-12-26 | 1982-05-25 | Union Carbide Corporation | Removal of caffeine by selective adsorption using zeolite adsorbents |
| CN101798355A (en) * | 2010-04-08 | 2010-08-11 | 晋江市恒源科技开发有限公司 | Method for integrated separation and extraction of tea polysaccharide, theanine, polyphenol and caffeine |
| CN102701308A (en) * | 2012-06-12 | 2012-10-03 | 黑龙江省科学院火山与矿泉研究所 | Method for removing organic matters and metal ions in raw mineral water of five connective ponds |
| CN105688929A (en) * | 2016-01-08 | 2016-06-22 | 广州市佳境水处理技术工程有限公司 | Neutral advanced oxidation catalyst with pelelith as carrier and preparing method of neutral advanced oxidation catalyst |
| CN105756295A (en) * | 2016-03-04 | 2016-07-13 | 同济大学 | Urban rainwater recycling reutilization system based on lava rocks |
Non-Patent Citations (3)
| Title |
|---|
| CAMELIA ELENA LUCHIAN等: "INFLUENCE OF NANOPOROUS MATERIALS ON THE CHEMICAL COMPOSITION OF MERLOT AND CABERNET SAUVIGNON WINES", 《ENVIRONMENTAL ENGINEERING AND MANAGEMENT JOURNAL》 * |
| 弗朗索瓦·法尔吉斯: "《探索发现-矿物与宝石》", 30 June 2016 * |
| 钱慧丽等: "《预拌砂浆应用技术》", 30 April 2015, 《中国建材工业出版社》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107349914A (en) * | 2017-09-03 | 2017-11-17 | 郑州坤博科技有限公司 | A kind of high-performance adsorbent for Industrial Wastewater Treatment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106390911B (en) | 2019-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102614834B (en) | Method for adsorbing and recovering heavy metals of lead and copper by persimmon tannin-containing metal adsorbent | |
| CN102816640B (en) | Preparation method of jujube extract and application thereof | |
| CN101986855A (en) | Method for preparing low-caffeine high-tea polyphenol tea powder | |
| CN101904877B (en) | New preparation method of low-phenolic acid gingko flavone extractive | |
| CN103254994B (en) | Method for preparing tobacco spice by tobacco fragments and application of spice | |
| CN102973617A (en) | Method for extracting pomegranate peel polyphenol | |
| CN104757190A (en) | Method for extracting tea polyphenol by extraction-adsorption method | |
| Datta et al. | Adsorption of polyphenols from ginger rhizomes on an anion exchange resin Amberlite IR-400–Study on effect of pH and temperature | |
| CN106390911B (en) | The method for preparing the method for pelelith adsorbent and being enriched with catechin antioxidant | |
| CN103819444A (en) | Method for extracting monomeric EGCG from fresh tea | |
| CN103907716B (en) | Improve green tea, jasmine tea concentrate fragrance and reduce the processing method of its bitter taste | |
| CN104189073B (en) | The preparation method of salvianolic acid | |
| CN103404651B (en) | A kind of technology of preparing of instant tea raw material of low caffeine content | |
| CN117397743A (en) | Composition containing coffee powder, green tea and black tea concentrated powder, and preparation and application thereof | |
| CN107412431A (en) | Ultrasonic assistant extracts Physalis pubescens L general flavone and purifying process | |
| CN103830323A (en) | Preparation method of traditional Chinese preparation honeysuckle and radix scutellariae granules | |
| CN101899083B (en) | Preparation method of cyclocarya paliurus acid A | |
| Ma et al. | Convenient isolation of strictinin-rich tea polyphenol from Chinese green tea extract by zirconium phosphate | |
| Li et al. | Extraction and preparation of high-aroma and low-caffeine instant green teas by the novel column chromatographic extraction method with gradient elution | |
| CN101804129A (en) | Method for extracting natural tea polyphenol | |
| CN107486161A (en) | A kind of adsorbent for heavy metal and its application | |
| CN107954968B (en) | Simple and efficient double-liquid-phase extraction, separation and purification and method for preparing high-purity tea polyphenol | |
| CN113499313A (en) | Preparation method of rose hip flesh vitamin C effervescent granules | |
| CN105267440A (en) | Preparation technology of high EGCG low caffeine tea extract | |
| KR101950341B1 (en) | Adsorbent prepared from a shiitake, and the method for obtaining a fraction containing a high concentration of ginsenoside Rg3 using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |