CN104530145B - Method for extracting high-purity persimmon tannin from persimmon fruits - Google Patents
Method for extracting high-purity persimmon tannin from persimmon fruits Download PDFInfo
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- CN104530145B CN104530145B CN201410840699.2A CN201410840699A CN104530145B CN 104530145 B CN104530145 B CN 104530145B CN 201410840699 A CN201410840699 A CN 201410840699A CN 104530145 B CN104530145 B CN 104530145B
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Abstract
The invention belongs to the technical field of preparation of persimmon tannin and particularly relates to a method for extracting high-purity persimmon tannin from persimmon fruits. The method comprises the following steps of: washing the persimmon fruits, smashing, extracting with ethanol in a refluxing way, carrying out liquid-liquid chromatographic separation and purification on a high-speed countercurrent chromatographic instrument by using a two-phase solvent system to obtain high-purity persimmon tannin, wherein the two-phase solvent system is composed of n-hexane, ethyl acetate, methanol and water at a volume ratio of 5:1:1:6. The process provided by the invention is simple, is easy to operate and is low in analysis cost, and the prepared persimmon tannin is high in purity.
Description
Technical field
The invention belongs to the technical field of persimmon tannin preparation, extract high-purity persimmon tannin from persimmon particularly to a kind of
Method.
Background technology
Persimmon, Ebenaceae plant berry fruits, original producton location is in China, the cultivation history of existing more than 1,000 year.China is persimmon
The country of origin of son, is also that persimmon cultivated area is maximum in the world and the most country of persimmon fruit yield.Either cultivated area is still
Fruit yield, China all in No. 1 in the world, much larger than the summation of other countries in the world.Traditional Chinese medicine is thought, persimmon
Sub sweet, puckery, cold in nature, return lung warp.Described in Compendium of Material Medica, " persimmon is the fruit of spleen, lung, blood system, and it is sweet and gas is put down, and property is puckery
And can receive, therefore have the puckery intestines of invigorating the spleen, control the work(of hemostasis of coughing." simultaneously, the calyx and receptacle of a persimmon, persimmon sugar, persimmon leaf all can be used as medicine.Persimmon fruit sweet-puckery flavor, property
Cold, nontoxic；Calyx and receptacle of a persimmon puckery, mild-natured, enter lung, spleen, stomach, large intestine channel；Have heat-clearing go dry, moistening lung for removing phlegm, softening hard masses, slake thirst and help produce saliva, strong
Spleen, control the functions such as dysentery, hemostasis, the diseases such as dry and hard excrement, pain due to hemorrhoid or bleeding, dry cough, laryngalgia, hypertension can be alleviated.So,
Persimmon is chronic bronchitis, hypertension, artery sclerosis, the natural health care of inside and outside hemorrhoid patients.
In persimmon contain substantial amounts of tannin, persimmon tannin is tannic acid again, is a kind of polymer of polyphenol, have sun-proof moisturizing,
Anti-wrinkle cosmetic, antisepsis and sterilization, prevention of cardiovascular disease, adsorbing metal ions and and protein interaction etc. function.
At present, there is the method that persimmon tannin is extracted in many people's researchs from persimmon, as Application No. 201110161337.7
A kind of method producing persimmon tannin from persimmon disclosed in Chinese invention patent, the method main processes are to pass through persimmon
Cleaning is screened, squeezes the juice, adds yeast Concentrated fermentation, ultrasonic-leaching, concentrate, be dried to obtain tannin acid product.It but is prepared into
The persimmon tannin purity arriving is low.
Content of the invention
The technical problem to be solved is to provide a kind of method extracting high-purity persimmon tannin from persimmon, the party
, it is easy to operate, the persimmon tannin purity preparing is high for method process is simple.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of method extracting high-purity persimmon tannin from persimmon, including following preparation process:
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 70～90% is added to extract 3 times, each extraction time is 100～150min,
Each Extracting temperature is 85～95 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 15～20 times of volumes, obtain sample molten
Liquid；
(5) fixing phase is filled chromatography column with 20～25ml/min flow velocity, adverse current is opened with 590～670rpm rotating speed
Chromatograph main frame, mobile phase is pumped in chromatographic column with 5～7ml/min flow velocity, after flowing balances each other, takes sample solution to pass through
Sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure, ethanol weight
Crystallization, obtains high-purity persimmon tannin.
Preferably, in step (2) of the present invention, during refluxing extraction, ethanol first time addition is the 10～12 of persimmon volume
Times, second addition of ethanol is 8～10 times of persimmon volume, and ethanol third time addition is 6～9 times of persimmon volume.This
Invention carries out 3 refluxing extraction, can extract persimmon tannin composition to greatest extent.
For ensureing the stable performance of persimmon tannin it is preferable that in step of the present invention (5), column temperature is set as 15～25 DEG C.
The friendship effect of the present invention is:
1st, present invention ethanol carries out 3 refluxing extraction, can extract composition needed for persimmon tannin to greatest extent.
2nd, the present invention is isolated and purified using high-speed countercurrent chromatography, and equipment needed thereby is cheap, analysis cost low it is easy to behaviour
Make, the product purity preparing is high, stable performance.
3rd, the present invention carries out separation purifying technique using alcohol extracting and high-speed countercurrent chromatography, and process is simple is workable.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 7% is added to extract 3 times, ethanol first time addition is the 12 of persimmon volume
Times, second addition of ethanol is 10 times of persimmon volume, when ethanol third time addition is 9 times of each extractions of persimmon volume
Between be 150min, each Extracting temperature is 85 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 15 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 20ml/min flow velocity, and set column temperature as 15 DEG C, with 590rpm rotating speed
Open counter-current chromatograph main frame, mobile phase is pumped in chromatographic column with 5ml/min flow velocity, after flowing balances each other, takes sample molten
Liquid passes through sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure,
Ethyl alcohol recrystallization, obtains high-purity persimmon tannin.
After testing, the purity of product is 95.2%.
Embodiment 2
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 75% is added to extract 3 times, ethanol first time addition is the 11 of persimmon volume
Times, second addition of ethanol is 9 times of persimmon volume, when ethanol third time addition is 8 times of each extractions of persimmon volume
Between be 140min, each Extracting temperature is 90 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 16 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 21ml/min flow velocity, and set column temperature as 18 DEG C, with 610rpm rotating speed
Open counter-current chromatograph main frame, mobile phase is pumped in chromatographic column with 6ml/min flow velocity, after flowing balances each other, takes sample molten
Liquid passes through sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure,
Ethyl alcohol recrystallization, obtains high-purity persimmon tannin.
After testing, the purity of product is 96.5%.
Embodiment 3
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 80% is added to extract 3 times, ethanol first time addition is the 11 of persimmon volume
Times, second addition of ethanol is 9 times of persimmon volume, when ethanol third time addition is 7 times of each extractions of persimmon volume
Between be 125min, each Extracting temperature is 90 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 18 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 23ml/min flow velocity, and set column temperature as 20 DEG C, with 630rpm rotating speed
Open counter-current chromatograph main frame, mobile phase is pumped in chromatographic column with 6ml/min flow velocity, after flowing balances each other, takes sample molten
Liquid passes through sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure,
Ethyl alcohol recrystallization, obtains high-purity persimmon tannin.
After testing, the purity of product is 98.9%.
Embodiment 4
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 85% is added to extract 3 times, ethanol first time addition is the 10 of persimmon volume
Times, second addition of ethanol is 8 times of persimmon volume, when ethanol third time addition is 6 times of each extractions of persimmon volume
Between be 110min, each Extracting temperature is 95 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 19 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 24ml/min flow velocity, and set column temperature as 23 DEG C, with 650rpm rotating speed
Open counter-current chromatograph main frame, mobile phase is pumped in chromatographic column with 7ml/min flow velocity, after flowing balances each other, takes sample molten
Liquid passes through sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure,
Ethyl alcohol recrystallization, obtains high-purity persimmon tannin.
After testing, the purity of product is 94.9%.
Embodiment 5
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 90% is added to extract 3 times, ethanol first time addition is the 10 of persimmon volume
Times, second addition of ethanol is 10 times of persimmon volume, when ethanol third time addition is 8 times of each extractions of persimmon volume
Between be 100min, each Extracting temperature is 90 DEG C, merges extract, is evaporated, obtains persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, balance point
Layer after, solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (3) obtains in the mobile phase of 20 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 25ml/min flow velocity, and set column temperature as 25 DEG C, with 670rpm rotating speed
Open counter-current chromatograph main frame, mobile phase is pumped in chromatographic column with 6ml/min flow velocity, after flowing balances each other, takes sample molten
Liquid passes through sample introduction valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure,
Ethyl alcohol recrystallization, obtains high-purity persimmon tannin.
After testing, the purity of product is 97.8%.
Claims (3)
1. a kind of method extracting high-purity persimmon tannin from persimmon is it is characterised in that include following preparation process:
(1) first by prematurity, the fresh persimmon of color green grass or young crops puckery is cleaned, standby after crushing；
(2) alcohol reflux that volumetric concentration is 70～90% is added to extract 3 times, each extraction time is 100～150min, every time
Extracting temperature be 85～95 DEG C, merge extract, be evaporated, obtain persimmon tannin crude product；
(3) by the 5:1:1:6 mixing by volume of n-hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering,
Solution is divided into phase up and down, lower as fixing phase, upper as mobile phase；
(4) take the persimmon tannin dissolving crude product that step (2) obtains in the mobile phase of 15～20 times of volumes, obtain sample solution；
(5) fixing phase is filled chromatography column with 20～25ml/min flow velocity, adverse current chromatogram is opened with 590～670rpm rotating speed
Instrument main frame, mobile phase is pumped in chromatographic column with 5～7ml/min flow velocity, after flowing balances each other, takes sample solution to pass through sample introduction
Valve injection, then according to ultraviolet chromatogram, under 215nm wavelength, collects purpose component, respectively evaporated under reduced pressure, ethyl alcohol recrystallization,
Obtain high-purity persimmon tannin.
2. according to claim 1 from persimmon extract high-purity persimmon tannin method it is characterised in that: in step (2),
During refluxing extraction, ethanol first time addition is 10～12 times of persimmon volume, and second addition of ethanol is the 8 of persimmon volume
～10 times, ethanol third time addition is 6～9 times of persimmon volume.
3. according to claim 1 from persimmon extract high-purity persimmon tannin method it is characterised in that: in step (5),
Column temperature is set as 15～25 DEG C.
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| CN105218834A (en) * | 2015-11-10 | 2016-01-06 | 桂林茗兴生物科技有限公司 | The method of high molecular tannin is extracted from persimmon |
| CN105218602A (en) * | 2015-11-10 | 2016-01-06 | 桂林茗兴生物科技有限公司 | The method of small-molecular-weight tannin is extracted from persimmon |
| CN105218601A (en) * | 2015-11-10 | 2016-01-06 | 桂林茗兴生物科技有限公司 | The method of tannin is extracted from persimmon |
| CN106008616B (en) * | 2016-07-05 | 2018-08-07 | 深圳市美漾无华生物科技有限公司 | A method of extracting persimmon tannin from persimmon |
| CN108395468B (en) * | 2018-03-05 | 2021-08-10 | 陕西师范大学 | Method for recovering protein in bean curd yellow slurry by using astringent persimmon tannin |
| CN108676043A (en) * | 2018-07-26 | 2018-10-19 | 大连民族大学 | A method of extracting tannic acid from persimmon |
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| CN101381420B (en) * | 2008-10-30 | 2011-03-23 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN101613383A (en) * | 2009-08-03 | 2009-12-30 | 五峰赤诚生物科技有限公司 | A kind of method of from persimmon, producing persimmon tannin |
| JP2012179037A (en) * | 2011-02-28 | 2012-09-20 | Masahiro Sano | Method for processing food material having acidity from persimmon peel |
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Address after: No. 72, Gong Cheng street, Gong town, Gongcheng Yao Autonomous County, the Guangxi Zhuang Autonomous Region, the Guangxi Zhuang Autonomous Region Patentee after: GUILIN DEKUN BIOTECHNOLOGY CO., LTD. Address before: 541004 the Guangxi Zhuang Autonomous Region City, Guilin Qixing District, west of the Ming Road, the New District No. five (13-1) venture building, block B315, No. B Patentee before: GUILIN DEKUN BIOTECHNOLOGY CO., LTD. |
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Granted publication date: 20170118 Termination date: 20171230 |