CN104789128A - Method for extracting vegetable tanning extract from acer truncatum bunge seed coats - Google Patents
Method for extracting vegetable tanning extract from acer truncatum bunge seed coats Download PDFInfo
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- CN104789128A CN104789128A CN201510182329.9A CN201510182329A CN104789128A CN 104789128 A CN104789128 A CN 104789128A CN 201510182329 A CN201510182329 A CN 201510182329A CN 104789128 A CN104789128 A CN 104789128A
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Abstract
The invention discloses a method for extracting a vegetable tanning extract from acer truncatum bunge seed coats. The method specifically comprises the following steps: collecting the acer truncatum bunge seed coats; carrying out drying, crushing, ultrasonic treatment, centrifugation and concentration to obtain the vegetable tanning extract from the acer truncatum bunge seed coats. According to the method, the problem of extraction of the vegetable tanning extract from the acer truncatum bunge seed coats is solved, and thus the truncatum bunge seed coats can be recycled; the method is high in extraction efficiency and rate, low in environmental pollution and cost, easy to operate, relatively high in quality of the obtained vegetable tanning extract, and suitable for large-scale production; a theoretical basis is provided for industrialization of the vegetable tanning extract extracted from the acer truncatum bunge seed coats.
Description
Technical field
The invention belongs to the effective constituent in natural product and derivative technical field thereof, be specifically related to the extracting method of tannin extract in a kind of acer truncatum seed coat.
Background technology
Acer truncatum, Acer truncatum Bunge, Chinese is flat base maple, North China Wu Jiao maple, Se Shu, ingot tree, Chinese sweet gum.English name Shantung Maple.Acer truncatum belongs to Aceraceae, Acer, deciduous tree.Single leaf is to life.Leafly split for palmate 5, sliver tip is gradually sharp, and phyllopodium cuts shape usually, and phyllopodium foot two sliver is carried out downwards sometimes.Flower shape is little, and pattern is yellow-green colour, and inflorescence is for becoming the raw cyme in top.Fruit is samara, flat-section.Fruit wing is wider and be slightly longer than fruit stone, likeness in form ingot.
The resistance to the moon of acer truncatum, is suitable for growing in the area of the cool moist climate of temperature.Its winter hardiness is strong, but is then difficult to growth in too dry and cold area.The growth of acer truncatum requires not tight to soil, all can grow in sour earth, neutral soil and terra calcis, but best to grow in moistening, fertile, that soil layer is deep soil.Acer truncatum belongs to deep-rootedness seeds, and the speed of growth is medium, and disease and pest is less, is widely distributed in northeast, North China, and to Shaanxi, Sichuan, Hubei, south reaches the provinces such as Zhejiang, Jiangxi, Anhui.It is the important green tree species of China.
Acer Truncatum Buge kernel is containing abundant grease, protein, VITAMIN and mineral substance, in addition also containing a small amount of sucrose and reducing sugar, not starch-containing.Research shows, Acer Truncatum Buge kernel oil length is 42.6%, and detect 12 kinds of lipid acid altogether, wherein unsaturated fatty acid content reaches 92%, and Selacholeic acid content is 5.52%.This illustrates that the Acertruncatum Bunge oil that acer truncatum seed squeezes is a kind of high-quality edible oil, is also a kind of oil for health care and medicinal oil.
In the process of acer truncatum seed oil expression, a large amount of remaining acer truncatum seed coat can be produced.Acer truncatum seed coat and fruit wing contain a large amount of condensed type tannin, and fruit wing tannin content is 7.87%, and shell tannin content is 60.24%.This is rare in plant samara, and the height of tannin content is also rare in vegitabilia.With the mimosa extract that low temperature process is produced from acer truncatum seed coat, shell, check through afforestation product inspection center of Ministry of Forestry, its tannin content is 73.6%, non-tannis content is 24.9%, purity is 75%, and every deciding grade and level index all meets the select quality of national standard (GB2622-1981) defined.Acer truncatum tannin belongs to high-quality condensed type tannin, and being developed as of such resource solves that China condensed type tannin lacks, the problem of main dependence on import, provides a new approach.
Tannin (Tannins) is also known as Weibull, tannin, tannic acid.By definition, refer to that relative molecular mass is energy precipitating proteins, the alkaloidal water-soluble polyphenols compound of 500 ~ 3000.It is extensively present in the leaf of plant, fruit, the position such as root and skin, is also that trees are subject to insect infestations and the main component of the insect gall generated; Be mainly used in the fields such as medicine, food, process hides, household chemicals, water treatment.Tannin is the compound of polyphenol camber polymerization, and be yellow or the amorphous bulky powder of brown color, color deepens gradually in atmosphere, has stronger water absorbability; It is insoluble to ether, benzene, chloroform, and soluble in water, ethanol, acetone, the aqueous solution of tannin has astringent taste.
Tannin can react with the protein in organism, polysaccharide, nucleic acid etc., and also variant according to the different mechanism of action of its molecular structure.Hydrolysable Tannins and condensed tannin can be divided into by chemical structure tannin, the former refers to phenolic acid or derivatives thereof and glucose and polyol reaction, by the polyphenol that ester class is formed, at diluted acid, diluted alkaline becomes comparatively simple compounds with hydrolyzable under bacterium effect, Hydrolysable Tannins can be divided into again gallic acid tannin (can generate gallic acid after hydrolysis) and benzoaric acid tannin (having benzoaric acid and ellagic acid to generate after hydrolysis), Hydrolysable Tannins mostly is contained by tradition medicinal plant, as the Turkey-galls of hemostasis and anti-inflammation, the mountain branches and leaves of protection gastrointestinal mucosal, the moutan root bark etc. of Cardiovarscular, condensed tannin mostly is flavan-3-alcohol (its derivative is called catechin) and flavane-3, the polymkeric substance of 4-glycol (its derivative is called leucoanthocyanidin class), can not be hydrolyzed, oxidation dehydration under the effect of acid, alkali or bacterium and be condensed into polymer reddish-brown Bu Rong and precipitate in " spiral shell is red " of water.Contained tannin mainly condensed tannin in food, namely has " spiral shell is red " to generate after the apple of incision, Lee and tea are long placed in.Oligomeric condensed tannin can be entered blood by micro-vascular absorption and have antioxygenation, and polymer cannot absorb, or excretes, or stays in the gastrointestinal tract, protects coat of the stomach from the injury of alcohol, hydrochloric acid because of comparatively strong with protein bound.
Tannin extract (Vegetable tanning extract) namely contains the plant milk extract of tannin, also known as vegatable tannin.From tanning plant raw material, obtain through refining various vegatable tannin Chemicals, the main application of tannin extract is tan leather.Tannin in tannin extract can form multiple spot crosslinking structure with the collagen protein in hide collagen, and the hydrothermal stability of collagen protein, enzymolysis tolerance and chemical reagent tolerance are improved. and tannin can increase the intensity of fiber, makes tanning agent utilize this characteristic just with tannin extract.About 600 BC Mediterranean Zone has used its tan leather, and after this vegetable Tanning Technology expands to the whole world gradually, tannin extract produce processing unit obtain corresponding improvement. tannin extract industry and leather industry closely bound up.
In addition, along with the pollution that the synthesis polymer of minimizing and a large amount of difficult degradation day by day of petroleum resources causes to environment, extensive concern is caused with the research that natural polyphenols replaces phenol to prepare drilling fluid additive. in numerous additive for drilling fluid, be that the drilling fluid thinner that raw material is made is widely used because it is functional with tannin extract.In addition, tannin extract is also used to do filtrate reducer for drilling fluid and profile-controlling and plugging agent, achieves tangible result aborning.
At present, from waste liquid or waste material the test of Adsorption of Heavy Metals element and the research of mechanism a lot, sorbent material is useful is rich in that the wood chip of tannin, wood powder or bark directly process, and also has the tannin extracted in plant or its major ingredient ellagic acid and many kinds of substance to be polymerized.Tannin is fixed on the immobilization tannin that carrier forms and there is selective adsorption performance, and can use by repeated regeneration.With vegetable fibre be wherein carrier be widely used in food, chemical industry and pharmaceutical industry.Being carrier containing the polymkeric substance of various active amino, can from seawater or waste water the heavy metal element such as adsorption uranium, industrial application potential is also very large.
The extracting method being directed to tannin extract in acer truncatum seed coat at present mainly adopts heating and refluxing extraction method, and the method utilizes the principle of solvent thermal refluxing extraction to extract tannin.Shortcoming is that power consumption is large, and pollute high, extraction efficiency is low, and during scale operation, cost is higher.
Summary of the invention
The object of this invention is to provide the extracting method of tannin extract in a kind of acer truncatum seed coat, the method extraction yield is high, can repetitive operation, and extractive technique is simple and easy to do.
The technical solution adopted in the present invention is, the extracting method of tannin extract in a kind of acer truncatum seed coat, specifically implements according to following steps:
Step 1, collection acer truncatum seed coat, kept dry after removing fruit wing and planting benevolence;
Step 2, dry and pulverize, the acer truncatum seed coat filtered out is placed in air dry oven, and pulverizes with pulverizer, then screen, collect the crushed material after sieving;
Step 3, ultrasonication centrifugal, add ethanol and make Extraction solvent, be placed in ultrasonic extractor in the crushed material after sieving; Pour in centrifuge tube centrifugal by ultrasonic rear solution, collected after centrifugation supernatant liquor, then repeat twice, the supernatant liquor obtained three times merges;
Step 4, concentrated, proceeded to by supernatant liquor in rotary evaporation bottle, rotary evaporation concentrates, and prepares tannin extract in acer truncatum seed coat.
Feature of the present invention is also,
In step 2, drying conditions is: time of drying is 10-15h, and described screening conditions were 60 mesh sieves.
In step 5, the concentration of ethanol is 70%, and the mass volume ratio of crushed material and ethanol is: 1:5g/ml-1:15g/ml.
In step 3, ultrasound condition is: ultrasonic time 25min-35min.
In step 3, centrifugal condition is: centrifugal speed 6000rpm, the centrifugal 10min of room temperature.
In step 4, concentrated condition is: thickening temperature 60-70 DEG C.
The invention has the beneficial effects as follows: 1, the invention solves the method extracting tannin extract from acer truncatum seed coat.Extraction efficiency and extraction yield high.Acer truncatum seed coat is remaining waste after Acer Truncatum Buge kernel oil expression, can be recycled by the method to acer truncatum seed coat.Extraction solvent is 70% ethanol, and be common Extraction solvent, environmental pollution is little and cheap and easy to get, is applicable to carrying out scale operation.By the comparison of preliminary experiment to the Extraction solvent extraction efficiency of opposed polarity, think 70% ethanol with to extract the polarity of tannin close, therefore extraction efficiency is the highest.By weighing the quality of the difference determination extract of quality before and after furnace pot, the error that loss produces when shifting extract can be avoided.Calculation result is comparatively accurate.The extract pure color obtained, high containing tannin extract purity, quality is better aborning.
2, the instrument that the present invention uses is easy to obtain, and cost is less, easy handling.
3, the present invention has abandoned the method for traditional employing thermal backflow and lixiviate, and utilize ultrasonic extraction, extraction efficiency is high, and extraction effect is good, economic environmental protection.The supersound extraction time is 30min, and ultrasonic time is too short, extracts insufficient; Ultrasonic time is long, causes excessive instrument loss.
4, during concentrated by rotary evaporation of the present invention, thickening temperature is 60 ~ 70 DEG C, and optimum temperuture is 65 DEG C, and tannin severe oxidation when temperature is too high, affects the application of subsequent extracted product, revolve when temperature is too low steam efficiency low, reduce production capacity.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.Embodiment described below is exemplary, only for explaining the present invention, and can not be interpreted as limitation of the present invention.Attached after instrument unit type and manufacturer in embodiment, unreceipted concrete technology or condition in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
The invention provides the extracting method of tannin extract in a kind of acer truncatum seed coat, specifically implement according to following steps:
Step 1, collection acer truncatum seed coat, kept dry after removing fruit wing and planting benevolence;
Step 2, the analytical balance being 0.1mg by the acer truncatum seed coat service precision filtered out are weighed, and recording quality is M
before oven dry; Then seed coat is placed in air dry oven, heating 10-15 hour, again weigh, recording quality is M
after oven dry, calculate water content M
moisture=M
before oven dry-M
after oven dry;
Step 3, the seed coat pulverizer of oven dry to be pulverized, then with 60 mesh sieves screenings, collect the crushed material after sieving;
Step 4, service precision are that the analytical balance of 0.1mg accurately takes crushed material mg, are placed in triangular flask;
Step 5, in triangular flask, add ethanol make Extraction solvent, triangular flask is placed in ultrasonic extractor, ultrasonic time 30min, wherein, the concentration (volume fraction) of ethanol is 70%, and the mass volume ratio of crushed material and ethanol is: 1:5g/ml-1:15g/ml;
Step 6, ultrasonic rear solution is poured in centrifuge tube centrifugal, centrifugal speed 6000rpm, the centrifugal 10min of room temperature, collected after centrifugation supernatant liquor;
Step 7, again repeating step 5, step 6 twice, the supernatant liquor obtained three times merges;
Step 8, proceed in rotary evaporation bottle by supernatant liquor, rotary evaporation concentrates, thickening temperature 60-70 DEG C;
Step 9, service precision are that the analytical balance of 0.1mg weighs an empty furnace pot weight, are recorded as M
furnace pot, proceed in furnace pot by revolving the extraction solution after steaming, furnace pot is placed on water-bath, and pre-evaporation concentrates, and furnace pot is placed in air dry oven heating 48 hours after solvent evaporation;
Step 10, furnace pot is taken out cooling, service precision is that the analytical balance of 0.1mg weighs with the furnace pot of extract, is recorded as M
after evaporate to dryness, then extract quality M is obtained
extractbe W with extraction yield:
M
extract=M
after evaporate to dryness-M
furnace pot
W=(M
extract/ m) * 100%.
Embodiment 1
(1) the acer truncatum seed coat provided by Yongchun, Sishui County, Shandong Province hall company limited, gathers 20.000g acer truncatum seed coat, kept dry after removing fruit wing and planting benevolence.
(2) analytical balance being 0.1mg by the acer truncatum seed coat service precision filtered out is weighed, recording quality 20.000g.Then seed coat is placed in air dry oven, heat 12 hours, again weigh, recording quality is 19.873, calculates water content M
moisture=20.000-19.873=0.127g;
(3) the seed coat pulverizer of oven dry is pulverized, then screen with 60 mesh sieves.Collect the crushed material after sieving;
(4) service precision is that the analytical balance of 0.1mg accurately takes 20.000g crushed material, is placed in triangular flask;
(5) in triangular flask, accurately add 70% ethanol 200ml and make Extraction solvent.Triangular flask is placed in ultrasonic cleaner, ultrasonic time 30min;
(6) ultrasonic rear solution is poured in centrifuge tube centrifugal, centrifugal speed 6000rpm, the centrifugal 10min of room temperature, collected after centrifugation supernatant liquor
(7) again repeating step (5), (6) twice, the supernatant liquor obtained three times merges;
(8) supernatant liquor is proceeded in rotary evaporation bottle, under the condition of 65 DEG C, rotate evaporation concentration;
(9) service precision is that the analytical balance of 0.1mg weighs an empty furnace pot weight, is recorded as M
furnace pot=92.184g, proceed in furnace pot by revolving the extraction solution after steaming, furnace pot is placed on water-bath, thickening temperature 60 DEG C, pre-evaporation solvent.After solvent evaporation, furnace pot is placed in air dry oven, heats 48 hours;
(10) furnace pot is taken out cooling.Service precision is the furnace pot that the analytical balance of 0.1mg weighs with extract, is recorded as M
after evaporate to dryness=107.466g.Then obtain extract quality M
extractbe W with extraction yield:
M
extract=M
after evaporate to dryness-M
furnace pot=107.466-92.184=15.282g.
W=(M
extract/ 20.000) * 100%=(15.282/20.000) * 100%=76.41%.
Embodiment 2
Gather acer truncatum seed coat 20g, the acer truncatum seed coat filtered out is placed in the dry 10h of air dry oven, pulverizes so that extract, screened 60 mesh sieves and remove the part and impurity that are difficult to extract.With the ethanol ultrasonic extraction of 70%, the mass volume ratio of crushed material and ethanol is 1:5g/ml, ultrasonic time 25min.Centrifugal after supersound extraction, centrifugal speed 6000rpm, makes supernatant liquor and extracts waste residue separately.Ensure that in seed coat, tannin extract is fully extracted in triplicate.Collected after centrifugation supernatant liquor.Supernatant liquor is rotated evaporation concentration under the condition of 60 DEG C.Weigh an empty furnace pot weight, be recorded as M
furnace pot=93.348g, proceeds to solution in furnace pot, water-bath evaporating solvent.Subsequent drying 48 hours; Weigh furnace pot after cooling, be recorded as M
after evaporate to dryness=109.009g.Then obtain extract quality M
extractwith extraction yield W:
M
extract=M
after evaporate to dryness-M
furnace pot=15.661g.
W=(M
extract/ 20.000) * 100%=78.305%.
Embodiment 3
Gather acer truncatum seed coat 20g, the acer truncatum seed coat filtered out is placed in the dry 15h of air dry oven, pulverize so that extract, the part and impurity that are difficult to extract are removed in screening.With the ethanol ultrasonic extraction of 70%, the mass volume ratio of crushed material and ethanol is 1:15g/ml; Ultrasonic time 35min.Centrifugal after supersound extraction, centrifugal speed 6000rpm, the centrifugal 10min of room temperature, make supernatant liquor and extract waste residue separately.Ensure that in seed coat, tannin extract is fully extracted in triplicate.Collected after centrifugation supernatant liquor.Supernatant liquor is rotated evaporation concentration under the condition of 70 DEG C.Weigh an empty furnace pot weight, be recorded as M
furnace pot=92.246g, proceeds to solution in furnace pot, water-bath evaporating solvent.Subsequent drying 48 hours; Weigh furnace pot after cooling, be recorded as M
after evaporate to dryness=108.258g.Then obtain extract quality M
extractwith extraction yield W:
M
extract=M
after evaporate to dryness-M
furnace pot=16.012g.
W=(M
extract/ 20.000) * 100%=80.06%.
Claims (6)
1. the extracting method of tannin extract in acer truncatum seed coat, is characterized in that, specifically implement according to following steps:
Step 1, collection acer truncatum seed coat, kept dry after removing fruit wing and planting benevolence;
Step 2, dry and pulverize, the acer truncatum seed coat filtered out is placed in air dry oven, and pulverizes with pulverizer, then screen, collect the crushed material after sieving;
Step 3, ultrasonication centrifugal, add ethanol and make Extraction solvent, be placed in ultrasonic extractor in the crushed material after sieving; Pour in centrifuge tube centrifugal by ultrasonic rear solution, collected after centrifugation supernatant liquor, then repeat twice, the supernatant liquor obtained three times merges;
Step 4, concentrated, proceeded to by supernatant liquor in rotary evaporation bottle, rotary evaporation concentrates, and prepares tannin extract in acer truncatum seed coat.
2. the extracting method of tannin extract in acer truncatum seed coat according to claim 1, it is characterized in that, in described step 2, drying conditions is: time of drying is 10-15h, and described screening conditions were 60 mesh sieves.
3. the extracting method of tannin extract in acer truncatum seed coat according to claim 1, it is characterized in that, in described step 3, the concentration of ethanol is 70%, and the mass volume ratio of crushed material and ethanol is: 1:5g/ml-1:15g/ml.
4. the extracting method of tannin extract in acer truncatum seed coat according to claim 1, it is characterized in that, in described step 3, ultrasound condition is: ultrasonic time 25min-35min.
5. the extracting method of tannin extract in acer truncatum seed coat according to claim 1, it is characterized in that, in described step 3, centrifugal condition is: centrifugal speed 6000rpm, the centrifugal 10min of room temperature.
6. the extracting method of tannin extract in acer truncatum seed coat according to claim 1, is characterized in that, in described step 4, concentrated condition is: thickening temperature 60-70 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107182655A (en) * | 2017-06-20 | 2017-09-22 | 乐山市奇能米业有限责任公司 | A kind of rice production technique |
| CN107488413A (en) * | 2017-08-24 | 2017-12-19 | 成都圻坊生物科技有限公司 | The extracting method of tannin extract in a kind of granatum |
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2015
- 2015-04-16 CN CN201510182329.9A patent/CN104789128A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101922A (en) * | 1993-10-16 | 1995-04-26 | 西北林学院 | Process for extracting vegetable tannin extract from Pterocarya stenoptera samara |
Non-Patent Citations (3)
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| 杨连利等: "元宝枫单宁类化合物的提取研究", 《皮革化工》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107182655A (en) * | 2017-06-20 | 2017-09-22 | 乐山市奇能米业有限责任公司 | A kind of rice production technique |
| CN107488413A (en) * | 2017-08-24 | 2017-12-19 | 成都圻坊生物科技有限公司 | The extracting method of tannin extract in a kind of granatum |
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