CN109810206A - A kind of method of gel ablution purifying pectin - Google Patents
A kind of method of gel ablution purifying pectin Download PDFInfo
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- CN109810206A CN109810206A CN201711160132.0A CN201711160132A CN109810206A CN 109810206 A CN109810206 A CN 109810206A CN 201711160132 A CN201711160132 A CN 201711160132A CN 109810206 A CN109810206 A CN 109810206A
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Abstract
The invention discloses a kind of methods of gel ablution purifying pectin, it is desirable to provide a kind of pectin purification process easy to operate, product purity is high, easy to industrialized production；Be characterized in that: (1) pectin, which is dissolved in deionized water, forms solution；(2) pectin solution carries out micro-filtrate membrane filtration；(3) acid solution is added in pectin solution and adjusts pH value formation acid gel, quickly gel is smashed and carries out stirring and washing by stirring.Decompression, which filters, after cleaning removes moisture removal, and aqueous slkali tune pH is added to dissolution gel-forming concentrated solution；(4) pectin solution is added dehydrated alcohol and is precipitated；(5) pectin precipitating carries out constant pressure and dry.
Description
Technical field
This technology is related to field of biological pharmacy, and in particular to a kind of pectin purification process.
Background technique
Pectin is a kind of natural polysaccharide high molecular polymer, and for molecular weight between 5-30 ten thousand, main chain is D- galacturonic acid
Through backbone made of α-Isosorbide-5-Nitrae glucosides key connection, side chain is made of rhamnose, arabinose, galactolipin and xylose etc.
Short-chain structure.Pectin is white to Red-brown powder, has colorless and odorless, without the properties such as definite melting point and solubility, does not dissolve in
The organic solvents such as ethyl alcohol, are dissolved in hot water, are slightly soluble in cold water.Pectin is the main component of the seventh-largest nutrient diet fiber of human body,
It is had a wide range of applications with multiple eating and medical value, therefore in food, medicine and other fields.
Current market sales of commercialization pectin is apple pectin and citrus pectin, is food-grade pectin, and purity is not high,
Impurity is more, cannot need progress after purification could be in medicine and group weaver directly in field of medicaments application since impurity is more
The application of journey field.Apple pectin is extracted from apple pomace, and the ingredient of apple pomace is extremely complex, including protein, polypeptide, ammonia
Base acid, monosaccharide, polysaccharide, cellulose, hemicellulose, volatile oil and grease, organic acid, polyphenol, lactone, flavones, vitamin and
Minerals etc., if the removal of these ingredients is not thorough when extracting pectin, it is likely that remain in and form impurity in pectin.Due to fruit
The complicated component of impurity in glue, purifying difficulty are larger.Pectin purification process is mainly ethanol purification and purifying resin, ethyl alcohol at present
Purification process can only remove oil-soluble impurities, and water-solubility impurity cannot remove, and the big higher cost of ethanol consumption, and resin is pure
Change method treating capacity is smaller, and higher cost, therefore the present invention purifies pectin using gel ablution, it is desirable to provide Yi Zhongcao
Make simple, product purity height, pectin purification process easy to industrialized production.
Summary of the invention
The purpose of the present invention is develop a kind of pectin purifying side easy to operate, product purity is high, easy to industrialized production
Method.
A kind of method of gel ablution purifying pectin, which is characterized in that in turn include the following steps:
(1) pectolysis
It weighs a certain amount of apple pectin and is add to deionized water dissolution under agitation, pectin mass concentration is
0.5-4%, speed of agitator 500-1500rpm, temperature are 20-80 DEG C, mixing time 1-4h；
(2) pectin solution micro-filtration
Pectin carries out micro-filtrate membrane filtration after being completely dissolved, filtration temperature is 20-80 DEG C, solution ph 2.5-9；
(3) gel cleans
Acid solution is added in filtered pectin solution and adjusts pH to 1-2 formation acid gel, quickly gel is smashed in stirring,
The stirring and washing time is 1-4h, and temperature is 20-60 DEG C, and wash number is 1-4 times.Decompression filters removal 70- after cleaning
The moisture of 90% volume is added aqueous slkali tune pH to 6-7 and dissolves gel-forming concentrated solution；
(4) ethanol precipitation
Dehydrated alcohol is added in pectin concentrated solution in step (3) to precipitate, the final concentration of 50-90% of ethyl alcohol volume,
Alcohol precipitation temperature is 2-30 DEG C, and preferable temperature is 4-10 DEG C；
(5) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 30-80 DEG C, and preferable temperature is 40-60 DEG C.
Pectin solution micro-filtration described in step 2 is the micro-filtrate membrane filtration for passing sequentially through 3 kinds of apertures, aperture is 0.8 μm,
0.45 μm and 0.22 μm.
Acid solutions described in step 3 are 0.5M-2M, preferably the one of the hydrochloric acid of 1M, acetic acid, citric acid, sulfuric acid etc.
Kind is two or more；It is quickly stirred after addition acid solution and smashes gel, the solable matter in colloidal sol is soluble in water.
The alkaline concentration is 0.5M-2M, the preferably sodium hydroxide of 1M, sodium carbonate, sodium bicarbonate, potassium hydroxide etc.
It is one or more kinds of.
Pectin concentrated solution mass concentration described in step 4 is 5-20%.
Technical solution provided by the invention has following technological merit:
(1) technical solution provided by the invention develops a kind of new pectin purification process, and the purity of pectin can be improved,
Impurity-eliminating effect is preferable.
(2) technical solution provided by the invention is easy to operate, is easy to technique amplification and industrialized production.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but do not constitute any limitation of the invention.Anyone is within the scope of the invention as claimed
Any type of modification made, still within the claims in the present invention protection scope.
Embodiment 1
A kind of pectin purification process provided by the invention, in turn includes the following steps:
(1) pectolysis
The apple pectin for weighing 1.5g is add to deionized water dissolution under agitation, and pectin mass concentration is
1.5%, speed of agitator 1000rpm, temperature are 30 DEG C, mixing time 1h.
(2) pectin solution micro-filtration
The pectin solution being completely dissolved successively carries out the filtering with microporous membrane that aperture is 0.8,0.45 and 0.22 μm, filtering temperature
Degree is 30 DEG C, solution ph 4.
(3) gel cleans
The HCl solution that 1M is added in filtered pectin solution adjusts pH to 1 and forms acid gel, and quickly gel is broken in stirring
Broken, the stirring and washing time is 2h, and temperature is 30 DEG C, and stirring and washing number is 3 times.Decompression filters 90% body of removal after cleaning
Long-pending moisture, the NaOH solution tune pH to 6 that 1M is added dissolve gel-forming concentrated solution.
(4) ethanol precipitation
Dehydrated alcohol is added in pectin solution to be precipitated, pectin solution mass concentration is 15% at this time, to pectin solution
Dehydrated alcohol is added to dehydrated alcohol volume final concentration of 70%, alcohol precipitation temperature is 4 DEG C.
(5) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 60 DEG C.
The pectin finished product removal of impurity that above-mentioned purifying process obtains is 85.1%, yield 45.3%.
Embodiment 2
A kind of pectin purification process provided by the invention, in turn includes the following steps:
(1) pectolysis
The apple pectin for weighing 2.0g is add to deionized water dissolution under agitation, and pectin mass concentration is
2.0%, speed of agitator 1500rpm, temperature are 30 DEG C, mixing time 1h.
(2) pectin solution micro-filtration
The pectin solution being completely dissolved successively carries out the filtering with microporous membrane that aperture is 0.8,0.45 and 0.22 μm, filtering temperature
Degree is 30 DEG C, solution ph 3.
(3) gel cleans
The HCl solution that 1M is added in filtered pectin solution adjusts pH to 1 and forms acid gel, and quickly gel is broken in stirring
Broken, the stirring and washing time is 1h, and temperature is 30 DEG C, and stirring and washing number is 2 times.Decompression filters 90% body of removal after cleaning
Long-pending moisture, the NaOH solution tune pH to 6 that 1M is added dissolve gel-forming concentrated solution.
(4) ethanol precipitation
Dehydrated alcohol is added in pectin solution to be precipitated, pectin solution mass concentration is 15% at this time, to pectin solution
Dehydrated alcohol is added to dehydrated alcohol volume final concentration of 60%, alcohol precipitation temperature is 10 DEG C.
(5) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 60 DEG C.
The pectin finished product removal of impurity that above-mentioned purifying process obtains is 83.2%, yield 44.7%.
Embodiment 3
A kind of pectin purification process provided by the invention, in turn includes the following steps:
(1) pectolysis
The apple pectin for weighing 1.0g is add to deionized water dissolution under agitation, and pectin mass concentration is
1.0%, speed of agitator 1500rpm, temperature are 30 DEG C, mixing time 1h.
(2) pectin solution micro-filtration
The pectin solution being completely dissolved successively carries out the filtering with microporous membrane that aperture is 0.8,0.45 and 0.22 μm, filtering temperature
Degree is 60 DEG C, solution ph 3.
(3) gel cleans
The HCl solution that 1M is added in filtered pectin solution adjusts pH to 2 and forms acid gel, and quickly gel is broken in stirring
Broken, the stirring and washing time is 1h, and temperature is 30 DEG C, and stirring and washing number is 1 time.Decompression filters 80% body of removal after cleaning
Long-pending moisture, the NaOH solution tune pH to 6 that 1M is added dissolve gel-forming concentrated solution.
(4) ethanol precipitation
Dehydrated alcohol is added in pectin solution to be precipitated, pectin solution mass concentration is 15% at this time, to pectin solution
Dehydrated alcohol is added to dehydrated alcohol volume final concentration of 70%, alcohol precipitation temperature is 4 DEG C.
(5) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 30 DEG C.
The pectin finished product removal of impurity that above-mentioned purifying process obtains is 74.2%, yield 42.7%.
Claims (4)
1. a kind of method of gel ablution purifying pectin, which is characterized in that in turn include the following steps:
(1) pectolysis
It weighs a certain amount of apple pectin and is add to deionized water dissolution under agitation, pectin mass concentration is 0.5-
4%, speed of agitator 500-1500rpm, temperature are 20-80 DEG C, mixing time 1-4h；
(2) pectin solution micro-filtration
Pectin carries out micro-filtrate membrane filtration after being completely dissolved, filtration temperature is 20-80 DEG C, solution ph 2.5-9；
(3) gel cleans
Acid solution is added in filtered pectin solution and adjusts pH to 1-2 formation acid gel, quickly gel is smashed in stirring, is stirred
Scavenging period is 1-4h, and temperature is 20-60 DEG C, and wash number is 1-4 times；Decompression filters removal 70-90% body after cleaning
Long-pending moisture is added aqueous slkali tune pH to 6-7 and dissolves gel-forming concentrated solution；
(4) ethanol precipitation
Dehydrated alcohol is added in pectin concentrated solution in step (3) to precipitate, the final concentration of 50-90% of ethyl alcohol volume, alcohol precipitation
Temperature is 2-30 DEG C, and preferable temperature is 4-10 DEG C；
(5) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 30-80 DEG C, and preferable temperature is 40-60 DEG C.
2. the method for gel ablution purifying pectin according to claim 1, it is characterised in that: fruit described in step 2
Sol solution micro-filtration is the micro-filtrate membrane filtration for passing sequentially through 3 kinds of apertures, and aperture is 0.8 μm, 0.45 μm and 0.22 μm.
3. the method for gel ablution purifying pectin according to claim 1, it is characterised in that: acid described in step 3
Solution concentration is 0.5M-2M, preferably the one or more of the hydrochloric acid of 1M, acetic acid, citric acid, sulfuric acid etc.；The aqueous slkali
Concentration is 0.5M-2M, preferably the one or more of the sodium hydroxide of 1M, sodium carbonate, sodium bicarbonate, potassium hydroxide etc..
4. the method for gel ablution purifying pectin according to claim 1, it is characterised in that: fruit described in step 4
Glue concentrated solution mass concentration is 5-20%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111513305A (en) * | 2020-05-27 | 2020-08-11 | 西南大学 | High-fat pectin rapid sugar-free gelling method and product |
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| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN101073384A (en) * | 2006-05-17 | 2007-11-21 | 烟台安德利果胶有限公司 | Production of low-methoxy apple pectin |
| CN103012617A (en) * | 2012-12-19 | 2013-04-03 | 中国农业大学 | Method for quickly and efficiently preparing pectin in energy-saving way |
| CN106317253A (en) * | 2016-09-27 | 2017-01-11 | 中国农业科学院特产研究所 | Ginseng fruit pectin and extraction method thereof |
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2017
- 2017-11-20 CN CN201711160132.0A patent/CN109810206A/en active Pending
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| CN1923853A (en) * | 2005-09-01 | 2007-03-07 | 中南大学 | Extraction and preparation technology for pectin of orange pericarp |
| CN101073384A (en) * | 2006-05-17 | 2007-11-21 | 烟台安德利果胶有限公司 | Production of low-methoxy apple pectin |
| CN103012617A (en) * | 2012-12-19 | 2013-04-03 | 中国农业大学 | Method for quickly and efficiently preparing pectin in energy-saving way |
| CN106810620A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of gingko episperm pectin extraction method |
| CN106317253A (en) * | 2016-09-27 | 2017-01-11 | 中国农业科学院特产研究所 | Ginseng fruit pectin and extraction method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111513305A (en) * | 2020-05-27 | 2020-08-11 | 西南大学 | High-fat pectin rapid sugar-free gelling method and product |
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