CN101381420B - Continuous extraction method of pectin, tannin and pigment from persimmon exocarp - Google Patents
Continuous extraction method of pectin, tannin and pigment from persimmon exocarp Download PDFInfo
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- CN101381420B CN101381420B CN2008100796684A CN200810079668A CN101381420B CN 101381420 B CN101381420 B CN 101381420B CN 2008100796684 A CN2008100796684 A CN 2008100796684A CN 200810079668 A CN200810079668 A CN 200810079668A CN 101381420 B CN101381420 B CN 101381420B
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- pectin
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- tannin
- persimmon skin
- persimmon
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Abstract
The invention discloses a continuous extraction method for pectin, tannin and pigment in a persimmon pericarp, which comprises the following steps: a. after the persimmon pericarp is pretreated, the pretreated persimmon pericarp is extracted by water at a temperature which is more than or equal to 70 DEG C and is less than 100 DEG C to obtain an extract and pulp stock; b. the extract is filtered by an ultrafiltration membrane with a cutoff molecular weight of between 10000 and 30000, the trapped part is a pectin liquid, a filtrate is absorbed and separated by a macroporous resin to obtain thetannin; and c. the pulp stock obtained in step a is extracted by acetone at a temperature of between 60 and 70 DEG C, and an extraction liquid is filtered, distilled and dried to obtain the pigment. The method has rich sources of raw materials, is simple, and is more suitable for large-scale industrial production; a used reagent has lower price, small toxicity, and strong maneuverability, and is easy to amplify the technology, and the cost is lower than extraction cost of corresponding products at present. A product extracted by the method is safe and nontoxic, and has simple and reasonable production technology.
Description
Technical field
The present invention relates to a kind of from the persimmon skin method of extracting effective components, the continuous extraction method of pectin, tannin and pigment in especially a kind of persimmon skin.
Background technology
As the by product persimmon skin of persimmon deep processing, account for the 10-15% of persimmon gross weight, output is considerable, uses mainly as food filling at present, and some is local even throw away in vain.Modern medicine study shows: contain more food fibre and pectin substance in the persimmon skin, to promoting human consumption, improve intestinal function and have good effect, and, pectin has special effectiveness in stable containing aspect proteinic beverage such as the milk proem, can avoid condensing because of the interaction between protein granule.The pectin that extracts both can be done commodity selling, also can transform the raw material of producing jelly, jelly work on the spot.
Contain profuse carotenoid and fatty acid ester thereof in the persimmon fruit, carotenoid is used for food color as natural pigment, and is safe; For humans and animals, part carotenoid is the most effective provitamin A, and the 30%-100% of human needs's vitamin A amount can be provided; What is more important carotenoid has certain anti-oxidant activity, can suppress lipid peroxidation, cancellation singlet oxygen, thereby can prevent cellular oxidation damage, preventing cardiovascular disease, especially to reducing tumor incidence unusual effect is arranged;
Also contain in the persimmon fruit and enrich tannin biologically active substances such as (tannin, tannic acids), sophisticated persimmon tannin mainly is distributed in the persimmon skin.It mainly is owing to contain tannin that the persimmon skin is sent out puckery, when persimmon deastringent, can not all take off to the greatest extent by tannic acid wherein, if gross weight is eaten easy formation persimmon stone in stomach together, but then, tannin can stop blooding callus, antibacterial antianaphylaxis, especially have anti-oxidant, delay senility, anticancer change, prevent the effect of cardiovascular and cerebrovascular diseases, in beer, wine making industry, have removal protein, improve the effect of mouthfeel, therefore, as long as reasonably use tannin, allow vouchsafing to the mankind of the Nature serve better surely.
At present, utilization to the persimmon skin mainly is to extract and applied research at pectin both at home and abroad, and report seldom, and extract tannin in the persimmon skin and carotenoid does not appear in the newspapers, in fact, utilizing the persimmon skin to extract in the technological process of pectin, tannin and pigment (carotenoid) are all thrown away as waste, so not only contaminate environment also will cause the waste of resource.
Summary of the invention
The technical problem to be solved in the present invention provides the continuous extraction method of pectin, tannin and pigment in a kind of persimmon skin that extracts effective constituent in the persimmon skin, to improve the utilization ratio of persimmon skin.
For solving the problems of the technologies described above, the present invention adopts following processing step:
A, with after the pre-treatment of persimmon skin, more than or equal to 70 ℃ less than 100 ℃ temperature under with water extraction pretreated persimmon skin, obtain extracting solution and slurry through once extracting; The weight ratio that adds slurry and water in the slurry through once extracting is 1: 10 a deionized water, is that to transfer mixture to the pH value of above-mentioned thick slag and water be 3-5 for the hydrochloric acid of 1-2% with massfraction; More than or equal to 70 ℃ less than 100 ℃ temperature under, behind the insulation boiling above-mentioned adjustment pH value mixture 40-50 minute filtered and obtained extracting solution and through the slurry of second extraction;
B, with said extracted liquid with molecular weight cut off at the ultrafiltration membrance filter of 10000-30000, hold back part and be liquid pectin, filtrate is separated with the wide aperture resin absorption, obtains tannin;
The slurry that obtains among c, the step a is used acetone extract down at 60 ℃-70 ℃, and extraction liquid filtration, distillation, drying obtain pigment.
Adopt the beneficial effect that technique scheme produced to be: patent application of the present invention is a kind of to be a whole set of technical scheme that raw material extracts pectin, tannin and pigment continuously with the Pericarpium Kaki.Raw material sources of the present invention are abundant, and extracting method is simple, is suitable for big industrial production.Less expensive, the toxicity of extracting pectin, tannin and pigment agents useful for same in the persimmon skin in the inventive method are little.Present method is workable, and technology is easy to amplify, and one-tenth should be lower than the extraction cost of present corresponding product.The product safety that the inventive method is extracted is nontoxic, and pectin can be applicable to the jelling agent of jelly, jam, also can be used for making the gelling soft sweets and when producing sour milk as fruit matrix, also can be used as the stablizer of food and thickening material etc.; Tannin can be used for the tanning in the process hides; Food oxydating resistance, anticorrosion; Be used in beer, wine making liquid, have the effect of removing protein, improving mouthfeel; Also can be applicable to beauty treatment, whiten.Carotenoid in the pigment directly extracts from natural phant (persimmon skin), it is fragrant and sweet to distinguish the flavor of, bright in colour, stable in properties, production technique advantages of simple, production process do not adopt any pigment that makes to produce harmful means and medicament that changes, it is a kind of comparatively ideal natural pigment, add in the food, not only make food have happy people's color and luster, but also have the effect of nutritive health-care.
Embodiment
Embodiment 1:
1, persimmon skin pre-treatment: select not have mouldy persimmon skin, clean the back and under 60 ℃ condition, dry, pulverize persimmon skin to diameter and be less than or equal to 2mm.
2, leaching:
A, making beating, pressure are squeezed the juice: adding solid-liquid ratio by the Pericarpium Kaki actual weight is 1: 15 deionized water, soaks 1 hour down at 80 ℃-90 ℃, breaks into pulping then, the pulping of accomplishing fluently is put into squeezing machine squeeze, and obtains extracting solution and slurry.
B, slurry second extraction: at adding solid-liquid ratio in the slurry of once leaching is 1: 10 deionized water, transferring pH value with the hydrochloric acid of 1% (massfraction) is 4.5-5, in temperature is 80 ℃-90 ℃ down insulation boilings 40-50 minutes, and squeezing obtains extracting solution and through the slurry of second extraction.
3, ultrafiltration membrance filter: with said extracted liquid ultrafiltration membrance filter, because the pectin relative molecular weight is 30000-100000, and the relative molecular weight of tannin only has 500-3000, experiment has utilized the difference on the molecular size between the two, adopt molecular weight cut off to hold back pectin at the ultra-filtration membrane of 10000-30000, reach 2%-4% until concentration of pectin, pectin is separated with tannin and pectin is concentrated.
Spissated liquid pectin adopts spraying drying to get pectin powder; Filtrate adopts macroporous resin adsorption to separate, and makes tannin be able to purifying.
4, acetone extract: all slurry acetone extracts, extraction solid-liquid ratio 1: 20g/ml extracted 2 hours down for 60 ℃ in temperature.The extraction liquid that obtains is filtered, underpressure distillation, vacuum-drying obtains wine-colored pigment (carotenoid) solid.Can carry out recycling to extraction agent (acetone).As calculated, extraction yield with this understanding is 79.38mg/100g.
Embodiment 2:
1, persimmon skin pre-treatment: select not have mouldy persimmon skin, clean the back and under 60 ℃ condition, dry, pulverize persimmon skin to diameter and be less than or equal to 2mm.
2, leaching:
A, making beating, pressure are squeezed the juice: the deionized water that by Pericarpium Kaki actual weight adding solid-liquid ratio is 1: 15, soaking 2 hours under more than or equal to 70 ℃ less than 100 ℃ temperature, break into pulping then, the pulping of accomplishing fluently is put into squeezing machine squeeze, obtain extracting solution and slurry through once extracting.
B, slurry second extraction: at adding solid-liquid ratio in the slurry of once leaching is 1: 10 deionized water, transferring pH value with the hydrochloric acid of 1% (massfraction) is 3-5, in temperature is 70 ℃-90 ℃ down insulation boilings 40-50 minutes, and squeezing obtains extracting solution and through the slurry of second extraction.
3, ultrafiltration membrance filter: adopt molecular weight cut off to hold back pectin, reach 2%-4%, pectin is separated with tannin until concentration of pectin at the ultra-filtration membrane of 10000-30000.Filtrate is adopted macroporous resin adsorption to separate and is obtained purified tannin.
The liquid pectin of holding back is with alcohol deposition method precipitating pectin: add ethanol in the liquid pectin of holding back, gained alcohol-pectin mixture is left standstill 4-8h, filter, break up behind the filter cake with massfraction 95% washing with alcohol, press filtration once more obtains the pectin finished product.
4, acetone extract: all slurry acetone extracts, extraction solid-liquid ratio 1: 20g/ml extracted 3 hours down for 50 ℃ in temperature.The extraction liquid that obtains is filtered, underpressure distillation, vacuum-drying obtains wine-colored carotenoid solid.Can carry out recycling to extraction agent.
After testing, in this persimmon skin in the continuous extraction method of pectin, tannin and pigment, the extraction yield of pectin is greater than 85%, product purity is greater than 80%, and degree of gelation is greater than 120, and weight loss on drying is less than 11%, ash content is less than 5%, heavy metal content (in pb) is less than 0.0015%, PH=2.8 ± 0.2, and various indexs all reach GBn246-85 foodstuff additive pectin quality standard; The tannin extraction yield is greater than 83%, and product purity is greater than 75%; The carotenoid extraction yield is greater than 75%, and purity is greater than 80%.
Claims (7)
1. the continuous extraction method of pectin, tannin and pigment in the persimmon skin is characterized in that this method adopts following processing step:
A, with after the pre-treatment of persimmon skin, more than or equal to 70 ℃ less than 100 ℃ temperature under with water extraction pretreated persimmon skin, obtain extracting solution and slurry through once extracting; The weight ratio that adds slurry and water in the slurry through once extracting is 1: 10 a deionized water, is that to transfer mixture to the pH value of above-mentioned thick slag and water be 3-5 for the hydrochloric acid of 1-2% with massfraction; More than or equal to 70 ℃ less than 100 ℃ temperature under, behind the insulation boiling above-mentioned adjustment pH value mixture 40-50 minute filtered and obtained extracting solution and through the slurry of second extraction;
B, with said extracted liquid with molecular weight cut off at the ultrafiltration membrance filter of 10000-30000, hold back part and be liquid pectin, filtrate is separated with the wide aperture resin absorption, obtains tannin;
The slurry that obtains among c, the step a is used acetone extract down at 60 ℃-70 ℃, and extraction liquid filtration, distillation, drying obtain pigment.
2. the continuous extraction method of pectin, tannin and pigment in the persimmon skin according to claim 1 is characterized in that the preprocessing process described in the step a is: with the oven dry of persimmon skin, the persimmon skin after the oven dry is crushed to diameter and is less than or equal to 2mm under 60 ℃ condition.
3. the continuous extraction method of pectin, tannin and pigment in the persimmon skin according to claim 1, it is characterized in that the leaching process described in the step a is: the weight ratio that adds persimmon skin and water in pretreated persimmon skin is 1: 15 a deionized water, soaking 1-2 hour under more than or equal to 70 ℃ less than 100 ℃ temperature, mixture with persimmon skin and water breaks into pulping then, the pulping of accomplishing fluently is squeezed, obtain extracting solution and slurry through once extracting.
4. the continuous extraction method of pectin, tannin and pigment in the persimmon skin according to claim 1 is characterized in that with massfraction being that to transfer mixture to the pH value of above-mentioned thick slag and water be 4.5-5 for the hydrochloric acid of 1-2%.
5. the continuous extraction method of pectin, tannin and pigment in the persimmon skin according to claim 1, it is characterized in that and to add ethanol in the liquid pectin of holding back among the step b, gained alcohol-pectin mixture is left standstill 4-8h, filter, use massfraction 95% washing with alcohol after breaing up filter cake, press filtration once more obtains the pectin finished product.
6. the continuous extraction method of pectin, tannin and pigment in the persimmon skin according to claim 5 is characterized in that pectin finished product spraying drying is made pectin powder.
7. according to the continuous extraction method of pectin, tannin and pigment in any described persimmon skin among the claim 1-6, it is characterized in that being: extraction solid-liquid ratio 1: 20g/ml with the extraction step among the step c, extracted down 2-3 hour at temperature 50-60 ℃, extraction liquid filtration, underpressure distillation, vacuum-drying with obtaining obtain the pigment into dark red solid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100796684A CN101381420B (en) | 2008-10-30 | 2008-10-30 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
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| CN2008100796684A CN101381420B (en) | 2008-10-30 | 2008-10-30 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
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| CN101381420A CN101381420A (en) | 2009-03-11 |
| CN101381420B true CN101381420B (en) | 2011-03-23 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614835A (en) * | 2011-01-28 | 2012-08-01 | 华中农业大学 | Persimmon tannin-containing metal adsorbent and preparation method thereof |
| CN102321383B (en) * | 2011-06-15 | 2013-12-04 | 华南农业大学 | Preparation method for vegetable tannin dye liquor and application thereof in dyeing aspect of real silk fabric |
| CN103013164A (en) * | 2012-12-14 | 2013-04-03 | 桂林普兰德生物科技有限公司 | Method for extracting natural pigment from persimmon peels |
| CN103554292B (en) * | 2013-11-15 | 2015-07-08 | 西安石油大学 | Method for preparing environment-friendly chemical for oil fields by using persimmon peel pectin and application of chemical |
| CN103739741B (en) * | 2013-12-22 | 2015-11-04 | 山东农业大学 | A kind of method extracting pectin from fermentation haw thorn wine pomace |
| CN103882160B (en) * | 2014-04-08 | 2016-02-17 | 广西壮族自治区林业科学研究院 | The purification process of valonex |
| CN104530145B (en) * | 2014-12-30 | 2017-01-18 | 桂林得坤生物科技股份有限公司 | Method for extracting high-purity persimmon tannin from persimmon fruits |
| CN105566512B (en) * | 2015-12-14 | 2018-03-30 | 山东省果树研究所 | A kind of extracting method of persimmon fruit pectin |
| CN112341504A (en) * | 2015-12-21 | 2021-02-09 | 河北科技师范学院 | Method for optimizing conditions for extracting tannin from grape seeds by organic solvent extraction method |
| CN106380495B (en) * | 2016-08-15 | 2019-05-21 | 中国农业科学院农产品加工研究所 | The method of tannin and pectin is continuously extracted from Pericarpium Kaki |
| CN109053826A (en) * | 2018-09-19 | 2018-12-21 | 湖南中茂生物科技有限公司 | A method of tannic acid is extracted in recycling from the acer truncatum seed dregs of rice |
| CN109568993A (en) * | 2018-11-05 | 2019-04-05 | 广州柿宝生物科技有限公司 | A kind of dehydration and drying technique of persimmon tannin concentrate |
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|---|---|---|---|---|
| CN1786081A (en) * | 2004-12-10 | 2006-06-14 | 西北工业大学 | Method of extracting natural yellow pigment from persimon leaf or persion bark |
| JP2007046015A (en) * | 2005-08-12 | 2007-02-22 | Tohoku Univ | Method for producing carotenoid pigment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1786081A (en) * | 2004-12-10 | 2006-06-14 | 西北工业大学 | Method of extracting natural yellow pigment from persimon leaf or persion bark |
| JP2007046015A (en) * | 2005-08-12 | 2007-02-22 | Tohoku Univ | Method for producing carotenoid pigment |
Non-Patent Citations (2)
| Title |
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| 曹安堂 等.柿皮中色素的提取.《天津化工》.2008,第22卷(第1期),46-47. |
| 曹安堂等.柿皮中色素的提取.《天津化工》.2008,第22卷(第1期),46-47. * |
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