CN104530145A - 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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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 technical field prepared by persimmon tannin, particularly a kind of method extracting high purity persimmon tannin from persimmon.
Background technology
Persimmon, Ebenaceae plant berry fruits, country of origin is in China, and cultivation has the history of more than 1,000 year.China is the country of origin of persimmon, is also the country that persimmon cultivated area is maximum and persimmon fruit output is maximum in the world.No matter be cultivated area or fruit yield, China is all in No. 1 in the world, much larger than the summation of other countries in the world.Traditional Chinese medicine is thought, persimmon taste is sweet, puckery, cold in nature, returns lung channel.Record in Compendium of Material Medica " persimmon be spleen, lung, blood system fruit also, the sweet and gas of its taste is flat, and property is puckery and can receive, therefore has the puckery intestines of invigorating the spleen, controls the merit 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, cold in nature, nontoxic; Calyx and receptacle of a persimmon puckery, property is put down, and enters lung, spleen, stomach, large intestine channel; There is heat-clearing to remove dry, moistening the lung and resolving the phlegm, soft heavily fortified point, slake thirst and help produce saliva, invigorating the spleen, control the function such as dysentery, hemostasis, constipation with dry stool, pain due to hemorrhoid or hemorrhage, the disease such as dry cough, laryngalgia, hypertension can be alleviated.So persimmon is the natural health care of chronic bronchitis, hypertension, arteriosclerosis, inside and outside hemorrhoid patients.
Containing a large amount of tannin in persimmon, persimmon tannin is tannic acid again, is a kind of polymkeric substance of polyphenol, has sun-proof moisturizing, anti-wrinkle cosmetic, antisepsis and sterilization, preventing cardiovascular disease, adsorbing metal ions and and protein interaction etc. function.
At present, many people are had to study the method extracting persimmon tannin from persimmon, as application number a kind of method producing persimmon tannin from persimmon disclosed in the Chinese invention patent of 201110161337.7, the method main processes be persimmon screen through cleaning, squeeze the juice, add yeast Concentrated fermentation, ultrasonic-leaching, concentrate, drying obtains Weibull product.But the persimmon tannin purity prepared is low.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method extracting high purity persimmon tannin from persimmon, and the method technique is simple, and easy handling, the persimmon tannin purity prepared is high.
For achieving the above object, the present invention adopts following technical scheme:
From persimmon, extract a method for high purity persimmon tannin, comprise following preparation process:
(1) first by prematurity, the fresh persimmon of look blue or green puckery is cleaned, for subsequent use after broken;
(2) add the alcohol reflux 3 times that volumetric concentration is 70 ~ 90%, each extraction time is 100 ~ 150min, and each Extracting temperature is 85 ~ 95 DEG C, united extraction liquid, and evaporate to dryness obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 15 ~ 20 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 20 ~ 25ml/min flow velocity, counter current chromatograph main frame is opened with 590 ~ 670rpm rotating speed, pump in chromatographic column by moving phase with 5 ~ 7ml/min flow velocity, after moving phase balance, extracting sample solution is by sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, respectively evaporated under reduced pressure, ethyl alcohol recrystallization, obtains high purity persimmon tannin.
Preferably, in step of the present invention (2), during refluxing extraction, ethanol first time add-on is 10 ~ 12 times of persimmon volume, and ethanol second time add-on is 8 ~ 10 times of persimmon volume, and ethanol third time add-on is 6 ~ 9 times of persimmon volume.The present invention carries out 3 refluxing extraction, can extract persimmon tannin composition to greatest extent.
For ensureing the stable performance of persimmon tannin, preferably, in step of the present invention (5), column temperature is set as 15 ~ 25 DEG C.
Friendship effect of the present invention is:
1, the present invention's ethanol carries out 3 refluxing extraction, can extract composition needed for persimmon tannin to greatest extent.
2, the present invention adopts high-speed countercurrent chromatography to carry out separation and purification, and required equipment is cheap, and analysis cost is low, easy handling, and the product purity prepared is high, stable performance.
3, the present invention adopts alcohol extracting and high-speed countercurrent chromatography to carry out separation purifying technique, and technique is simple, workable.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to these embodiments.
Embodiment 1
(1) first by prematurity, the fresh persimmon of look blue or green puckery is cleaned, for subsequent use after broken;
(2) alcohol reflux 3 times that volumetric concentration is 7% is added, ethanol first time add-on is 12 times of persimmon volume, ethanol second time add-on is 10 times of persimmon volume, ethanol third time add-on is 9 times of each extraction times of persimmon volume is 150min, each Extracting temperature is 85 DEG C, united extraction liquid, evaporate to dryness, obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 15 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 20ml/min flow velocity, and to set column temperature be 15 DEG C, open counter current chromatograph main frame with 590rpm rotating speed, moving phase is pumped in chromatographic column with 5ml/min flow velocity, after moving phase balance, extracting sample solution passes through sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, evaporated under reduced pressure respectively, 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 look blue or green puckery is cleaned, for subsequent use after broken;
(2) alcohol reflux 3 times that volumetric concentration is 75% is added, ethanol first time add-on is 11 times of persimmon volume, ethanol second time add-on is 9 times of persimmon volume, ethanol third time add-on is 8 times of each extraction times of persimmon volume is 140min, each Extracting temperature is 90 DEG C, united extraction liquid, evaporate to dryness, obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 16 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 21ml/min flow velocity, and to set column temperature be 18 DEG C, open counter current chromatograph main frame with 610rpm rotating speed, moving phase is pumped in chromatographic column with 6ml/min flow velocity, after moving phase balance, extracting sample solution passes through sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, evaporated under reduced pressure respectively, 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 look blue or green puckery is cleaned, for subsequent use after broken;
(2) alcohol reflux 3 times that volumetric concentration is 80% is added, ethanol first time add-on is 11 times of persimmon volume, ethanol second time add-on is 9 times of persimmon volume, ethanol third time add-on is 7 times of each extraction times of persimmon volume is 125min, each Extracting temperature is 90 DEG C, united extraction liquid, evaporate to dryness, obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 18 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 23ml/min flow velocity, and to set column temperature be 20 DEG C, open counter current chromatograph main frame with 630rpm rotating speed, moving phase is pumped in chromatographic column with 6ml/min flow velocity, after moving phase balance, extracting sample solution passes through sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, evaporated under reduced pressure respectively, 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 look blue or green puckery is cleaned, for subsequent use after broken;
(2) alcohol reflux 3 times that volumetric concentration is 85% is added, ethanol first time add-on is 10 times of persimmon volume, ethanol second time add-on is 8 times of persimmon volume, ethanol third time add-on is 6 times of each extraction times of persimmon volume is 110min, each Extracting temperature is 95 DEG C, united extraction liquid, evaporate to dryness, obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 19 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 24ml/min flow velocity, and to set column temperature be 23 DEG C, open counter current chromatograph main frame with 650rpm rotating speed, moving phase is pumped in chromatographic column with 7ml/min flow velocity, after moving phase balance, extracting sample solution passes through sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, evaporated under reduced pressure respectively, 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 look blue or green puckery is cleaned, for subsequent use after broken;
(2) alcohol reflux 3 times that volumetric concentration is 90% is added, ethanol first time add-on is 10 times of persimmon volume, ethanol second time add-on is 10 times of persimmon volume, ethanol third time add-on is 8 times of each extraction times of persimmon volume is 100min, each Extracting temperature is 90 DEG C, united extraction liquid, evaporate to dryness, obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 20 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 25ml/min flow velocity, and to set column temperature be 25 DEG C, open counter current chromatograph main frame with 670rpm rotating speed, moving phase is pumped in chromatographic column with 6ml/min flow velocity, after moving phase balance, extracting sample solution passes through sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, evaporated under reduced pressure respectively, ethyl alcohol recrystallization, obtains high purity persimmon tannin.
After testing, the purity of product is 97.8%.
Claims (3)
1. from persimmon, extract a method for high purity persimmon tannin, it is characterized in that, comprise following preparation process:
(1) first by prematurity, the fresh persimmon of look blue or green puckery is cleaned, for subsequent use after broken;
(2) add the alcohol reflux 3 times that volumetric concentration is 70 ~ 90%, each extraction time is 100 ~ 150min, and each Extracting temperature is 85 ~ 95 DEG C, united extraction liquid, and evaporate to dryness obtains persimmon tannin crude product;
(3) by the 5:1:1:6 mixing by volume of normal hexane, ethyl acetate, methyl alcohol, water, shake up, stratification, after balance layering, solution is divided into phase up and down, lower to stationary phase, upper as moving phase;
(4) get persimmon tannin dissolving crude product that step (3) obtains in the moving phase of 15 ~ 20 times of volumes, obtain sample solution;
(5) stationary phase is filled chromatography column with 20 ~ 25ml/min flow velocity, counter current chromatograph main frame is opened with 590 ~ 670rpm rotating speed, pump in chromatographic column by moving phase with 5 ~ 7ml/min flow velocity, after moving phase balance, extracting sample solution is by sampling valve sample introduction, then according to ultraviolet color atlas, under 215nm wavelength, collect object component, respectively evaporated under reduced pressure, ethyl alcohol recrystallization, obtains high purity persimmon tannin.
2. the method extracting high purity persimmon tannin from persimmon according to claim 1, it is characterized in that: in step (2), during refluxing extraction, ethanol first time add-on is 10 ~ 12 times of persimmon volume, ethanol second time add-on is 8 ~ 10 times of persimmon volume, and ethanol third time add-on is 6 ~ 9 times of persimmon volume.
3. the method extracting high purity persimmon tannin from persimmon according to claim 1, is characterized in that: in step (5), column temperature is set as 15 ~ 25 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| CN106008616A (en) * | 2016-07-05 | 2016-10-12 | 深圳市美漾无华生物科技有限公司 | Method for extracting persimmon tannin from persimmons |
| CN108395468A (en) * | 2018-03-05 | 2018-08-14 | 陕西师范大学 | A kind of method that puckery persimmon tannin recycles protein in bean curd yellow pulp water |
| 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN106008616A (en) * | 2016-07-05 | 2016-10-12 | 深圳市美漾无华生物科技有限公司 | Method for extracting persimmon tannin from persimmons |
| 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 |
| CN108395468A (en) * | 2018-03-05 | 2018-08-14 | 陕西师范大学 | A kind of method that puckery persimmon tannin recycles protein in bean curd yellow pulp water |
| 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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