CN103772452A - Method for extracting tannin from phyllanthus emblica - Google Patents
Method for extracting tannin from phyllanthus emblica Download PDFInfo
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- CN103772452A CN103772452A CN201410007979.5A CN201410007979A CN103772452A CN 103772452 A CN103772452 A CN 103772452A CN 201410007979 A CN201410007979 A CN 201410007979A CN 103772452 A CN103772452 A CN 103772452A
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- phyllanthus emblica
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- ethyl alcohol
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Abstract
The invention discloses a method for extracting tannin from phyllanthus emblica. The method comprises the following steps of washing the phyllanthus emblica, drying, smashing, sieving, then adding into ethyl alcohol solution, mixing uniformly through stirring, adding cellulase, pectinase and papain, then carrying out ultrasonic-assisted extraction for three times, filtering, combining the extracting solutions, recycling the ethyl alcohol, putting the obtained phyllanthus emblica extracting solution into a magnetic force oscillator and oscillating, then freezing and standing, after layering, taking the supernatant liquid; allowing the obtained supernatant liquid to pass through the pretreated macroporous adsorption resin column; rinsing the macroporous adsorption resin column with deionized water till the effluent is colorless, then eluting with ethyl alcohol solution, collecting the eluant and recycling the ethyl alcohol, then concentrating, freeze drying so as to obtain the finished product tannin. Compared with traditional extraction method, the method is obviously superior, can remarkably improve the yield and purity of the tannin, is simple and easy to operate, has high production efficiency and low production cost, and has important economic benefits.
Description
Technical field
The present invention relates to the extracting method of Weibull in a kind of phyllanthus emblica, belong to traditional Chinese medicine ingredients extractive technique field.
Background technology
Weibull, has another name called tannic acid, is that a class has bioactive polyphenol substance, and it can form the mixture that is insoluble in water with protein, alkaloid, enzyme, glucoside and heavy metal.Its 11-20% ointment is for exudative ulcer, scald, bedsore, hemorrhoid, eczema etc., its 15-20% glycerine solution is for stomatitis, tonsillitis and pharyngolaryngitis etc., also for removing toxic substances, when year to Apomorphinum, scholar, purple foxglove, lead, silver, copper, zinc etc. are poisoning, available its solution gastric lavage; During for colon radiography, in barium sulfate enema, add this product 0.25-0.5% bowel lavage, in order to clean colon, be convenient to develop.Weibull can also suppress the activity of echidnotoxin, and the toxin such as Naja are had to very strong detoxification, and the cleaning wound while also can be used for venomous snake bite, is widely used in field of medicaments.Mainly from the natural phant that contains Weibull, adopt at present water or other solvent extraction both at home and abroad.But it is not high that disclosed Weibull extractive technique also exists extraction yield, the shortcoming that product purity is low, cannot meet the demand in market.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method of extracting Weibull from Chinese medicine phyllanthus emblica is provided, the method Weibull extraction yield is high, and product purity is high.
For achieving the above object, the technical solution used in the present invention is as follows:
An extracting method for Weibull in phyllanthus emblica, comprises the following steps:
(1) get the cleaning, drying of raw material phyllanthus emblica to water ratio lower than 3%, pulverize, cross 60-80 mesh sieve;
(2) getting Phyllanfhus Fruit after above-mentioned sieving, to add the concentration that 10-15 doubly measures be 70-80% ethanolic soln, stir, add again cellulase, the polygalacturonase of 0.01-0.02% and the papoid of 0.01-0.02% of phyllanthus emblica weight 0.02-0.03%, then carry out ultrasonic assisted extraction, ultrasonic temperature is 50-60 ℃, ultrasonic power is 400-600W, extraction time is 20-30min, filter, the ultrasonic assisted extraction filter residue of same solvent of doubly measuring with 10-15 according to the method described above 2 times, united extraction liquid, reclaims ethanol, obtains phyllanthus emblica extracting solution;
(3) phyllanthus emblica extracting solution obtained above is placed in to the magnetic force vibrator 1-2h that vibrates, vibrational frequency is 2500-3000r/min, and then freezing standing 12-24h at 0-5 ℃ of temperature, gets supernatant liquid after layering;
(4) AB-8 macroporous adsorbent resin is soaked to 12-24h in dehydrated alcohol, remove the impurity in resin, after washing with deionized water again, boil 20-30min, then wet method upper prop, with 1-2 BV deionization washing post until without alcohol residue, then pass through resin column with 1-2BV 5%HC solution, after 1-2h, be washed till neutrality with deionized water, then with 1-2BV 5%NaOH solution-treated, after 1-2h, be washed till neutrality with deionized water;
(5) clear liquor step (3) being obtained with the flow velocity of 0.5-1.5BV/h by the good AB-8 macroporous adsorptive resins of pre-treatment;
(6) be colourless with washed with de-ionized water AB-8 macroporous adsorptive resins to effluent liquid, and then be that 80-95% ethanolic soln carries out wash-out with the flow velocity of 1-2BV/h by concentration, collect elutriant and reclaim after ethanol, being concentrated into relative density is 1.34-1.38, lyophilize, obtains Weibull finished product.
Beneficial effect of the present invention:
In alcohol extraction process of the present invention, adopt ultrasonic assisted extraction, can greatly improve the extraction yield of Weibull and reduce extraction time, in leaching process, cellulase, polygalacturonase and papoid have also been added simultaneously, can destroy the dense structure of cell walls, accelerate the stripping of phyllanthus emblica effective constituent Weibull, thereby improve the extraction yield of Weibull.In the freezing clarification process of the present invention, adopt magnetic force vibration phyllanthus emblica extracting solution, can promote separating of impurity component and Weibull, improve the purity of Weibull product.The inventive method, compared with traditional extraction process, has obvious superiority, can significantly improve yield and the purity of Weibull, and simple to operation, and production efficiency is high, and production cost is low, has important economic benefit.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment 1
(1) get the cleaning, drying of 500g phyllanthus emblica to water ratio lower than 3%, pulverize, cross 60 mesh sieves;
(2) getting Phyllanfhus Fruit after above-mentioned sieving, to add the concentration of 10 times of amounts be 80% ethanolic soln, stir, then add cellulase, 0.01% polygalacturonase and 0.01% the papoid of phyllanthus emblica weight 0.02%, then carry out ultrasonic assisted extraction, ultrasonic temperature is 50 ℃, ultrasonic power is 400W, and extraction time is 30min, filters, use according to the method described above the ultrasonic assisted extraction filter residue of same solvent 2 times of 10 times of amounts, united extraction liquid, reclaims ethanol, obtains phyllanthus emblica extracting solution;
(3) phyllanthus emblica extracting solution obtained above is placed in to the magnetic force vibrator 2h that vibrates, vibrational frequency is 2500r/min, and then freezing standing 24h at 0 ℃ of temperature, gets supernatant liquid after layering;
(4) AB-8 macroporous adsorbent resin is soaked to 24h in dehydrated alcohol, remove the impurity in resin, after washing with deionized water again, boil 20min, then wet method upper prop, with 1 BV deionization washing post until without alcohol residue, then pass through resin column with 1BV 5%HC solution, after 1h, be washed till neutrality with deionized water, then with 1BV 5%NaOH solution-treated, after 1h, be washed till neutrality with deionized water;
(5) clear liquor step (3) being obtained with the flow velocity of 1BV/h by the good AB-8 macroporous adsorptive resins of pre-treatment;
(6) be colourless with washed with de-ionized water AB-8 macroporous adsorptive resins to effluent liquid, and then be that 90% ethanolic soln carries out wash-out with the flow velocity of 1BV/h by concentration, collecting elutriant reclaims after ethanol, being concentrated into relative density is 1.36, lyophilize, obtain Weibull finished product 65.37g, purity is 99.28%, and Weibull yield is 92.71%.
Embodiment 2
(1) get the cleaning, drying of 500g phyllanthus emblica to water ratio lower than 3%, pulverize, cross 80 mesh sieves;
(2) getting Phyllanfhus Fruit after above-mentioned sieving, to add the concentration of 15 times of amounts be 70% ethanolic soln, stir, then add cellulase, 0.02% polygalacturonase and 0.02% the papoid of phyllanthus emblica weight 0.03%, then carry out ultrasonic assisted extraction, ultrasonic temperature is 60 ℃, ultrasonic power is 600W, and extraction time is 20min, filters, use according to the method described above the ultrasonic assisted extraction filter residue of same solvent 2 times of 15 times of amounts, united extraction liquid, reclaims ethanol, obtains phyllanthus emblica extracting solution;
(3) phyllanthus emblica extracting solution obtained above is placed in to the magnetic force vibrator 1h that vibrates, vibrational frequency is 3000r/min, and then freezing standing 24h at 2 ℃ of temperature, gets supernatant liquid after layering;
(4) AB-8 macroporous adsorbent resin is soaked to 24h in dehydrated alcohol, remove the impurity in resin, after washing with deionized water again, boil 30min, then wet method upper prop, with 2 BV deionization washing posts until without alcohol residue, then pass through resin column with 2BV 5%HC solution, after 2h, be washed till neutrality with deionized water, then with 2BV 5%NaOH solution-treated, after 2h, be washed till neutrality with deionized water;
(5) clear liquor step (3) being obtained with the flow velocity of 1.5BV/h by the good AB-8 macroporous adsorptive resins of pre-treatment;
(6) be colourless with washed with de-ionized water AB-8 macroporous adsorptive resins to effluent liquid, and then be that 95% ethanolic soln carries out wash-out with the flow velocity of 2BV/h by concentration, collecting elutriant reclaims after ethanol, being concentrated into relative density is 1.38, lyophilize, obtain Weibull finished product 66.18g, purity is 99.22%, and Weibull yield is 93.81%.
Claims (1)
1. an extracting method for Weibull in phyllanthus emblica, is characterized in that comprising the following steps:
(1) get the cleaning, drying of raw material phyllanthus emblica to water ratio lower than 3%, pulverize, cross 60-80 mesh sieve;
(2) getting Phyllanfhus Fruit after above-mentioned sieving, to add the concentration that 10-15 doubly measures be 70-80% ethanolic soln, stir, add again cellulase, the polygalacturonase of 0.01-0.02% and the papoid of 0.01-0.02% of phyllanthus emblica weight 0.02-0.03%, then carry out ultrasonic assisted extraction, ultrasonic temperature is 50-60 ℃, ultrasonic power is 400-600W, extraction time is 20-30min, filter, the ultrasonic assisted extraction filter residue of same solvent of doubly measuring with 10-15 according to the method described above 2 times, united extraction liquid, reclaims ethanol, obtains phyllanthus emblica extracting solution;
(3) phyllanthus emblica extracting solution obtained above is placed in to the magnetic force vibrator 1-2h that vibrates, vibrational frequency is 2500-3000r/min, and then freezing standing 12-24h at 0-5 ℃ of temperature, gets supernatant liquid after layering;
(4) AB-8 macroporous adsorbent resin is soaked to 12-24h in dehydrated alcohol, remove the impurity in resin, after washing with deionized water again, boil 20-30min, then wet method upper prop, with 1-2 BV deionization washing post until without alcohol residue, then pass through resin column with 1-2BV 5%HC solution, after 1-2h, be washed till neutrality with deionized water, then with 1-2BV 5%NaOH solution-treated, after 1-2h, be washed till neutrality with deionized water;
(5) clear liquor step (3) being obtained with the flow velocity of 0.5-1.5BV/h by the good AB-8 macroporous adsorptive resins of pre-treatment;
(6) be colourless with washed with de-ionized water AB-8 macroporous adsorptive resins to effluent liquid, and then be that 80-95% ethanolic soln carries out wash-out with the flow velocity of 1-2BV/h by concentration, collecting elutriant reclaims after ethanol, being concentrated into relative density is 1.34-1.38, lyophilize, obtains Weibull finished product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107235840A (en) * | 2017-07-17 | 2017-10-10 | 长沙爱扬医药科技有限公司 | A kind of method of the chlorogenic acid extracting from coffee bean and tannin |
| CN109876031A (en) * | 2019-04-21 | 2019-06-14 | 北京中医药大学 | A kind of enrichment method at phyllemblic tannin position |
| CN111888290A (en) * | 2020-08-18 | 2020-11-06 | 广东丸美生物技术股份有限公司 | Cinnamon bark extract and preparation method and application thereof |
| CN113273643A (en) * | 2021-06-11 | 2021-08-20 | 广东大泽农生物科技股份有限公司 | Tannin preparation for feed and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107235840A (en) * | 2017-07-17 | 2017-10-10 | 长沙爱扬医药科技有限公司 | A kind of method of the chlorogenic acid extracting from coffee bean and tannin |
| CN109876031A (en) * | 2019-04-21 | 2019-06-14 | 北京中医药大学 | A kind of enrichment method at phyllemblic tannin position |
| CN111888290A (en) * | 2020-08-18 | 2020-11-06 | 广东丸美生物技术股份有限公司 | Cinnamon bark extract and preparation method and application thereof |
| CN113273643A (en) * | 2021-06-11 | 2021-08-20 | 广东大泽农生物科技股份有限公司 | Tannin preparation for feed and preparation method thereof |
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