CN109053826A - A method of tannic acid is extracted in recycling from the acer truncatum seed dregs of rice - Google Patents
A method of tannic acid is extracted in recycling from the acer truncatum seed dregs of rice Download PDFInfo
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- CN109053826A CN109053826A CN201811094107.1A CN201811094107A CN109053826A CN 109053826 A CN109053826 A CN 109053826A CN 201811094107 A CN201811094107 A CN 201811094107A CN 109053826 A CN109053826 A CN 109053826A
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- tannic acid
- extracted
- acer truncatum
- seed dregs
- recycling
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/08—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals directly attached to carbocyclic rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The method that the present invention provides a kind of to extract tannic acid from the acer truncatum seed dregs of rice, the characteristic being had differences according to the degree of polymerization, molecular weight, polarity and the solubility of compounds different in tannic acid, gradient extracting, fractional extraction impurity elimination are selected, repurity etc. obtains tannic acid.Its beneficial effect is that this method can effectively extract all kinds of tannic acid in the acer truncatum seed dregs of rice, and the method is quick and easy, and process is short, high-efficient, strong operability, at low cost, and products obtained therefrom purity and recovery rate are high.By the extraction to tannic acid in acer truncatum seed, can either effective detoxification, and be conducive to the comprehensive utilization of acer truncatum, while avoiding it and polluting the environment.
Description
Technical field
The invention belongs to technical field of plant extraction, and it is single to recycle extraction from the acer truncatum seed dregs of rice more particularly, to one kind
The method of peaceful acid.
Background technique
Acer truncatum also known as acer monoes are Chinese endemic trees, are traditional Ornamental trees, another is pure natural,
Nuisanceless, high nutrition dual-purpose of drug and food tree species.Ingot maple leaves are rich in brass, chlorogenic acid, polysaccharide etc..Acer truncatum seed particle
Greatly, oil content is high, and is rich in the various actives substances such as grease, protein, nervonic acid, vitamin E, tannic acid, wherein nervonic acid
Content is up to 5%, so acer truncatum seed is both excellent edible vegetable oil material, it is also medicines and health protection materials.
The tannin acid content of acer truncatum kind skin is up to 60%, rarely found in general vegetable tanning material.Tannic acid is a kind of water-soluble
Property, phenolic compound of the molecular weight between 500~3000 Da, do not dissolve in ether, benzene, chloroform, soluble easily in water, ethyl alcohol, third
Ketone.Tannic acid is not single compound, and chemical component is more complicated, is broadly divided into two kinds, Hydrolysable Tannins and condensed tannin, preceding
Person refers to the polyphenol that phenolic acid or derivatives thereof is mainly formed by esters with glucose or polyalcohol, acts in diluted acid, diluted alkaline and bacterium
Lower hydrolyzable can be divided into gallic acid tannin (gallic acid is produced after hydrolysis) and benzoaric acid at compared with simple compounds
Tannin (have after hydrolysis benzoaric acid i.e. tan peanut at), condensed tannin system flavan-3-alcohol (its derivative is known as catechin)
With the polymer (more than three monomers polymerizeing) of flavane -3,4- glycol (its derivative is known as leucoanthocyanidin class), cannot be hydrolyzed,
Oxidation is dehydrated and is condensed into macromolecule rufous " spiral shell is red " not soluble in water and precipitates under the action of acid, alkali or bacterium.Institute in food
It is mainly condensed tannin containing tannin, two kinds of tannin generally exist simultaneously, there is convergence, sun-proof, crease-resistant, moisturizing, anti-corrosion and other effects,
It is widely used in fields such as food, chemical industry, cosmetics, medicine.Meanwhile tannic acid is also the main next of astringent taste in acer truncatum seed
Source not only influences palatability, but also is difficult to digest, or even have hypotoxicity.Therefore, the tannic acid in acer truncatum seed is removed, is weight
The detoxification step wanted, is conducive to the comprehensive utilization of acer truncatum.
Currently, the extraction of tannic acid is usually to utilize organic solvent or water from medicinal plant Chinese gall, dendrobium nobile, tower drawing
It extracts, to be pulverized and sieved before these raw material abstractions, or particle is made and extracts again, complex steps, and what is obtained is mostly
Hydrolyzable tannin, for Hydrolysable Tannins in addition to toxicity is greater than condensed tannin, application range is also relatively small.
Summary of the invention
To solve the above problems, the present invention provides a kind of method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice, the party
Method selects gradient according to the characteristic that the degree of polymerization, molecular weight, polarity and solubility have differences in compounds different in tannic acid
Tannic acid is extracted in extracting, fractional extraction impurity elimination, repurity, is conducive to the comprehensive utilization of acer truncatum.
The present invention provides a kind of method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice, specifically includes the following steps:
1) it slightly mentions: weighing the acer truncatum seed dregs of rice, adjust pH to 2~4, extracted 3 ~ 4 times in 60~65 DEG C of gradients, press solid-liquid ratio 1 every time:
5~10 are added extractant, are concentrated after merging filtrate after extraction, obtain tannic acid crude extract；
2) impurity elimination: the extractant that 1~2 times of volume is sequentially added in the tannic acid crude extract into step 1) carries out classification extraction
It takes, further extracts tannin acid blend respectively by polarity, while being separated again with impurity such as sugar, albumen, filtered, merge filter
It is concentrated after liquid, obtains tannic acid extracting solution；
3) purify: it is 0.1~0.5g/mL that the tannic acid extracting solution that step 2 obtains, which is diluted with water tannin acid concentration, surveys pH
Loading in chromatographic column after value, the flow velocity of the loading is 20mL/min hereinafter, coutroi velocity is conducive to tannin acid and consolidates
Surely then the fastness combined is eluted away the impurity such as carbohydrate remaining in extracting solution, amino acid using eluent, elute
Flow velocity be 30~50mL/min, excessive velocities are easy to rinse in the target tannic acid fixed, elute to transparent, explanation
Impurity is rinsed well substantially, then is eluted whole tannic acid from stationary phase using 100% acetone, flow velocity 50mL/min
Hereinafter, collecting eluent, it is concentrated and dried to obtain tannic acid.
Further, in the step 1) extractant be acetone or alcohol, wherein the concentration of acetone or alcohol be 40%~
100%, since tannin acid is best in the dissolubility of water, acetone, ethyl alcohol, the acetone or alcohol pair of different moisture content is set
The little tannin acid blend extraction effect of purity is more preferable.
Further, gradient is extracted in the step 1), and in the concentration gradient for the extractant of use, each gradient spacing is big
In 20%, for example, extracting the Extractant concentration used for the first time and extracting the extractor concentration absolute value of the difference used for second needs
It is greater than and is equal to 20%, the gradient extraction process more than is conducive to the abundant of different solubilities tannic acid in the acer truncatum seed dregs of rice
It extracts.
Further, gradient is extracted in the step 1), is using 40% acetone, 60% acetone, 100% acetone extracts by several times.
Further, it is 1% that the extractant of the fractional extraction in the step 2, which is followed successively by ethyl acetate, water and content of hydrochloric acid,
~10% methanol.
Further, content of hydrochloric acid is 4% in methanol in the step 2.
Further, chromatographic column stationary phase is polyacrylamide, sephadex or macroporous absorbent resin in the step 3)
One of.
Further, chromatographic column stationary phase is macroporous absorbent resin in the step 3).
Further, eluent is distilled water or 5%~10% acid solution in the step 3).
Further, acid solution is dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid solution in the step 3).
Further, eluent is distilled water in the step 3).
Further, the temperature being concentrated in the step 1), step 2 and step 3) is 40~60 DEG C.
Compared with the existing technology, the present invention has the advantage that and effect:
The method of the invention improves the comprehensive utilization value of acer truncatum by the extraction to tannic acid.The present invention, which uses, to be divided
Grade is extracted and can effectively be extracted the tannic acid of the degree of polymerization various in acer truncatum, opposed polarity, and extraction efficiency is higher.The present invention
Method and process is simple, and process is short, and strong operability is at low cost.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus for the art conventional reagent, method and apparatus,
Unless stated otherwise, agents useful for same and material of the present invention are commercially available.
Embodiment 1:
1, it slightly mentions: weighing the 50g acer truncatum seed dregs of rice, successively use 40% acetone of 250mL, 60% acetone of 250mL and 250mL 100% the third
Ketone is extracted respectively on shaking bath, wherein the solid-liquid ratio of each acer truncatum seed dregs of rice and each concentration acetone is 1:5, and temperature is
60 DEG C, pH=2 are filtered after being repeated 3 times, are concentrated after merging filtrate, obtain tannic acid crude extract；
2, the ethyl acetate of 1 times of volume, water, wherein acetic acid impurity elimination: are sequentially added in the tannic acid crude extract into step 1)
The volume ratio of ethyl ester and water is 1:1.Then fractional extraction, filtering, merging filtrate are carried out using the methanol solution containing 4% hydrochloric acid
After be concentrated, obtain tannic acid extracting solution；
3, purify: it is 0.1g/mL that the tannic acid extracting solution that step 2 obtains, which is diluted to tannin acid concentration with distilled water, will be measured
PH=4, while NKA-Macroporous absorbent resin fills out column, then with the distillation water balance of pH=4, and diluted tannic acid extracting solution is pressed
20mL/min loading, then eluted with the distilled water of pH=4, rate of flow in rinse 50mL/min, until leacheate transparent clear,
It is finally eluted with 100% acetone 20mL/min, collects eluent and obtain tannic acid refined solution, be concentrated and dried to obtain tannic acid 12.1g.
Embodiment 2:
1, it slightly mentions: weighing the 50g acer truncatum seed dregs of rice, successively use 40% ethyl alcohol of 400mL, 100% second of 60% ethyl alcohol of 400mL and 400mL
Alcohol is extracted 2 times respectively on shaking bath, wherein the solid-liquid ratio of each acer truncatum seed dregs of rice and each concentration acetone is 1:7, temperature
It is 65 DEG C, pH=3 are filtered after being repeated 3 times, are concentrated after merging filtrate, and tannic acid crude extract is obtained；
2, impurity elimination: sequentially adding the ethyl acetate of 1 times of volume in the tannic acid crude extract into step 1), the water of 1 times of volume,
Then fractional extraction is carried out using the methanol solution containing 4% hydrochloric acid of 1 times of volume, filtered, be concentrated after merging filtrate, obtain tannin
Sour extracting solution；
3, purify: it is 0.3g/mL that the tannic acid extracting solution that step 2 obtains, which is diluted to tannin acid concentration with distilled water, will be measured
PH=2, while NKA-Macroporous absorbent resin fills out column, then with the distillation water balance of pH=2, and diluted tannic acid extracting solution is pressed
20mL/min loading, then eluted with the distilled water of pH=2, rate of flow in rinse 30mL/min, until leacheate transparent clear,
It is finally eluted with 100% acetone 20mL/min, collects eluent and obtain tannic acid refined solution, be concentrated and dried to obtain tannic acid 14.3g.
Claims (10)
1. a kind of method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice, which comprises the following steps:
1) it slightly mentions: weighing the acer truncatum seed dregs of rice, adjust pH to 2~4, extracted 3 ~ 4 times in 60~65 DEG C of gradients, press solid-liquid ratio 1 every time:
5~10 are added extractant, are concentrated after merging filtrate after extraction, obtain tannic acid crude extract；2) impurity elimination: the tannin into step 1)
The extractant that 1~2 times of volume is sequentially added in sour crude extract carries out fractional extraction, filters, and is concentrated after merging filtrate, obtains tannin
Sour extracting solution；3) purify: it is 0.1~0.5g/mL that the tannic acid extracting solution that step 2 obtains, which is diluted with water tannin acid concentration,
Loading in chromatographic column after survey pH value, the flow velocity of the loading are 20 mL/min hereinafter, then being eluted using eluent, elution
Flow velocity is 30~50 mL/min, and elution is eluted to transparent, then using 100% acetone, the flow velocity of elution be 50 mL/min hereinafter,
Eluent is collected, tannic acid is concentrated and dried to obtain.
2. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
1) extractant is acetone or alcohol in, and wherein the concentration of acetone or alcohol is 40%~100%.
3. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
1) gradient is extracted as in the concentration gradient of extractant in, and each gradient spacing is greater than 20%.
4. recycling according to claim 1 or from the acer truncatum seed dregs of rice methods for extracting tannic acid described in 3, it is characterised in that: described
Gradient is extracted as successively using 40% acetone, 60% acetone, 100% acetone extraction in step 1).
5. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
2) extractant of the fractional extraction in is followed successively by the methanol of ethyl acetate, water and content of hydrochloric acid 1%~10%.
6. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
3) chromatographic column stationary phase is one of polyacrylamide, sephadex or macroporous absorbent resin in.
7. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 6, it is characterised in that: the chromatography
Column stationary phase is macroporous absorbent resin.
8. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
3) eluent in is the acid solution of distilled water or 5%~10%.
9. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 8, it is characterised in that: the acidity
Solution is one of dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid solution.
10. the method that tannic acid is extracted in recycling from the acer truncatum seed dregs of rice according to claim 1, it is characterised in that: the step
The rapid temperature 1), in step 2 and step 3) being concentrated is 40~60 DEG C.
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| CN201811094107.1A CN109053826A (en) | 2018-09-19 | 2018-09-19 | A method of tannic acid is extracted in recycling from the acer truncatum seed dregs of rice |
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| CN201811094107.1A CN109053826A (en) | 2018-09-19 | 2018-09-19 | A method of tannic acid is extracted in recycling from the acer truncatum seed dregs of rice |
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Citations (5)
| 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 |
| CN101134766A (en) * | 2006-08-30 | 2008-03-05 | 上海康文医药中间体有限公司 | Method for preparing high-purity maple tannin by acer ginnala leaf |
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN104311676A (en) * | 2014-10-15 | 2015-01-28 | 贵州绿农生物科技有限公司 | Method for extracting edible starch from oak seeds and obtaining byproduct tannin |
| CN105694733A (en) * | 2016-02-16 | 2016-06-22 | 山东永春堂集团有限公司 | Method for extracting tannin extract in seed coats of acer truncatum |
-
2018
- 2018-09-19 CN CN201811094107.1A patent/CN109053826A/en not_active Withdrawn
Patent Citations (5)
| 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 |
| CN101134766A (en) * | 2006-08-30 | 2008-03-05 | 上海康文医药中间体有限公司 | Method for preparing high-purity maple tannin by acer ginnala leaf |
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN104311676A (en) * | 2014-10-15 | 2015-01-28 | 贵州绿农生物科技有限公司 | Method for extracting edible starch from oak seeds and obtaining byproduct tannin |
| CN105694733A (en) * | 2016-02-16 | 2016-06-22 | 山东永春堂集团有限公司 | Method for extracting tannin extract in seed coats of acer truncatum |
Non-Patent Citations (5)
| Title |
|---|
| 吴谋成 等: ""油菜籽中单宁的提取、组成及性质的研究"", 《华中农业大学百年校庆校友学术论文》 * |
| 张燕 等: ""油菜籽饼中单宁的提取、分离与纯化制备"", 《华中农业大学学报》 * |
| 杨连利 等: ""元宝枫单宁类化合物的提取研究"", 《皮革化工》 * |
| 段久芳 主编: "《天然高分子材料》", 30 September 2016, 华中科技大学出版社 * |
| 王磊 等: ""植物单宁的提取纯化方法及其发展"", 《西部皮革》 * |
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