CN109810205A - A kind of compound pectin purification process - Google Patents
A kind of compound pectin purification process Download PDFInfo
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- CN109810205A CN109810205A CN201711159636.0A CN201711159636A CN109810205A CN 109810205 A CN109810205 A CN 109810205A CN 201711159636 A CN201711159636 A CN 201711159636A CN 109810205 A CN109810205 A CN 109810205A
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Abstract
The invention discloses a kind of compound pectin purification process, and be characterized in that: (1) pectin, which is dissolved in deionized water, forms solution；(2) pectin solution carries out micro-filtrate membrane filtration；(3) alkali alumina adsorbent is added in filtered pectin solution to be adsorbed；Successively by centrifugation and filtering removal adsorbent after absorption；(4) HCl solution that 1M is added in pectin solution is adjusted, and quickly gel is smashed in stirring, and carries out gel cleaning；Decompression, which filters, after cleaning removes moisture removal, and NaOH solution tune pH is added and dissolves gel-forming concentrated solution；(5) pectin solution is added dehydrated alcohol and is precipitated；(6) 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 compound pectin purification process.
Background technique
Pectin is a kind of containing several hundred linear polysaccharides to thousands of a structural units, average molecular weight 5-30 ten thousand it
Between.Pectin be mainly galacturonic acid and rhamnose, arabinose and galactolipin etc. as made of α -1,4- glucosides key connecting its
The polymer that his neutral sugar is linked, main chain be D- galacturonic acid formed backbone, side chain be by rhamnose, I
The short-chain structure of the compositions such as uncle's sugar, galactolipin and xylose.Pectin is white to Red-brown powder, has colorless and odorless, without fixation
The properties such as fusing point and solubility are dissolved in hot water, are slightly soluble in cold water insoluble in organic solvents such as ethyl alcohol.Pectin is a kind of thickener
With stabilizer, it has been widely used in food industry at present, pectin is added in jam, fruit juice can make it during transportation
It is indeformable, while can also tart up and reduce syneresis；Pectin is added when producing fruit drink, extract to be stablized
Suspension oiliness lactic acid in solution makes fruit juice have fresh flavor；Addition pectin can play stable and fresh-keeping in milk product
Effect, coagulation of casein can also be prevented and extend acid dairy produce drinks the time limit.The food fiber of pectin is to maintain people
The important substance of body health, having the function of, which enhances gastrointestinal peristalsis, promotes nutrient absorption, to prevention and treatment hypertension, intestinal cancer, urine disease, fertilizer
The illnesss such as fat disease have good curative effect, while being the antidotes of pectin or heavy metal.
Current market sales of commercialization pectin is apple pectin and citrus pectin, they are all food-grade pectin, pure
Spend not high, impurity is more, due to impurity it is more cannot directly in field of medicaments application, need to carry out after purification could in medicine and
Field of tissue engineering technology application.Apple pectin is extracted from apple pomace, and the ingredient of apple pomace is extremely complex, including protein,
Polypeptide, amino acid, monosaccharide, polysaccharide, cellulose, hemicellulose, volatile oil and grease, organic acid, polyphenol, lactone, flavones, dimension life
Element 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 the complicated component of impurity in pectin, it is larger to purify difficulty.Pectin purification process is mainly that ethanol purification and resin are pure at present
To change, ethanol purification method can only remove oil-soluble impurities, and water-solubility impurity cannot remove, and the big higher cost of ethanol consumption,
And purifying resin method treating capacity is smaller, and higher cost.Due to apple pectin complicated component, single method is difficult impurity
It completely removes, therefore the present invention purifies pectin using absorption attached gel ablution, it is desirable to provide one kind is easy to operate, product is pure
Degree 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 compound 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 successively carries out the micro-filtrate membrane filtration that aperture is 0.8,0.45 and 0.22 μm after being completely dissolved, filtration temperature is
20-80 DEG C, solution ph 2.5-9.
(3) adsorbent adsorbs
Adsorbent is added in filtered pectin solution to be adsorbed, adsorbent amount and pectin dry weight ratio are 0.5-4:1,
Adsorption temp is 20-60 DEG C, and adsorption operations number is 1-4 times, adsorption time 0.5-4h.Successively by centrifugation after absorption
Adsorbent is removed with filtering.
(4) 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.
(5) ethanol precipitation
Pectin solution is added dehydrated alcohol and is precipitated, and ethyl alcohol volumetric concentration is 50-90%, and alcohol precipitation temperature is 4-30 DEG C.
(6) product drying
Pectin precipitating carries out constant pressure and dry, and drying temperature is 30-80 DEG C.
In above-mentioned pectin purification process step (1) pectin mass concentration be 1-4%, speed of agitator 500-1500rpm,
Temperature is 20-80 DEG C, mixing time 1-4h.
Further, above-mentioned pectin purification process step (2) is pectin solution micro-filtration, and pectin solution successively carries out aperture
For 0.8,0.45 and 0.22 μm of micro-filtrate membrane filtration, filtration temperature is 20-80 DEG C, solution ph 2.5-9.
Further, above-mentioned pectin purification process step (3) is adsorbent Adsorption impurity, and selected adsorbent is alkali
The one of property alumina adsorbant, molecular sieve, silica gel, active carbon, atlapulgite, macroreticular resin XDA-7, macroreticular resin D3520 etc.
Kind is two or more, and absorbent particles size is 100-300 mesh, and adsorbent amount and pectin dry weight ratio are 0.5-4:1, and absorption is warm
Degree is 20-60 DEG C, and absorption number is 1-4 times, adsorption time 0.5-4h.Successively by centrifugation and filtering removal after absorption
Adsorbent.Further, above-mentioned pectin purification process step (4) is gel ablution removal impurity, is added in pectin solution
Acid solution adjusts pH to 1-2 and forms acid gel, and acid solutions are that acid used in 0.5M-2M is hydrochloric acid, acetic acid, citric acid, sulfuric acid
Deng one or more；Quickly gel is smashed in stirring, and the stirring and washing time is 1-4h, and temperature is 20-60 DEG C, cleaning time
Number is 1-4 times；Decompression filters the moisture of removal 70-90% volume after cleaning, and aqueous slkali tune pH to 6-7 is added and dissolves gel
Concentrated solution, alkaline concentration 0.5M-2M are formed, alkali used is sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide etc.
It is one or more kinds of.
Further, above-mentioned pectin purification process step (5) is ethanol precipitation, and pectin solution concentration ratio is original solution
The 10-30% of volume, ethyl alcohol volumetric concentration are 50-90%, and alcohol precipitation temperature is 2-30 DEG C.
Technical solution provided by the invention has following technological merit:
(1) technical solution provided by the invention develops a kind of compound pectin purification process, with single purification process phase
Than impurity-eliminating effect is more preferable, and pectin purity is higher.
(2) technical solution simple process provided by the invention, step is less, 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 1500rpm, temperature are 30 DEG C, mixing time 2h.
(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 4.5.
(3) adsorbent adsorbs
Alkali alumina adsorbent is added in filtered pectin solution to be adsorbed, absorbent particles size is 300 mesh,
Pectin dry weight ratio is 2:1 in adsorbent amount and step (1), and adsorption temp is 30 DEG C, adsorption time 2h.After absorption according to
Secondary to remove adsorbent by centrifugation and filtering, repeating this step absorption centrifugal filtration number of operations is 4 times.
(4) 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 wash number is 3 times.Decompression filters 90% volume of removal after cleaning
Moisture, the NaOH solution tune pH to 6 that 1M is added dissolve gel-forming concentrated solution.
(5) ethanol precipitation
Pectin solution carries out ethanol precipitation after vacuum distillation concentration, and concentration ratio is 10% addition nothing of original solution volume
Extremely, ethyl alcohol volume final concentration of 70%, alcohol precipitation temperature is 10 DEG C to water-ethanol.
(6) 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 99.5%, yield 41.9%.
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 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 2h.
(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 4.5.
(3) adsorbent adsorbs
Alkali alumina adsorbent is added in filtered pectin solution to be adsorbed, absorbent particles size is 300 mesh,
Pectin dry weight ratio is 2:1 in adsorbent amount and step (1), and adsorption temp is 30 DEG C, and adsorption operations number is 1 time, when absorption
Between be 1h.Successively by centrifugation and filtering removal adsorbent after absorption.
(4) 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 wash number is 2 times.Decompression filters the water of removal 90% after cleaning
Point, the NaOH solution tune pH to 6 that 1M is added dissolves gel-forming concentrated solution.
(5) ethanol precipitation
Pectin solution carries out ethanol precipitation after vacuum distillation concentration, and concentration ratio is 10% addition nothing of original solution volume
Extremely, ethyl alcohol volume final concentration of 60%, alcohol precipitation temperature is 10 DEG C to water-ethanol.
(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 88.3%, yield 42.2%.
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 2.0g is add to deionized water dissolution under agitation, and pectin mass concentration is 2%,
Speed of agitator is 1500rpm, and temperature is 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 9.
(3) adsorbent adsorbs
Alkali alumina adsorbent is added in filtered pectin solution to be adsorbed, absorbent particles size is 100-
300 mesh, adsorbent amount are 4:1 with pectin dry weight ratio in step (1), and adsorption temp is 60 DEG C, and adsorption operations number is 1 time,
Adsorption time is 1h.Successively by centrifugation and filtering removal adsorbent after absorption.
(4) gel cleans
The HCl solution that 1M is added in filtered pectin solution adjusts pH to 1.0 and forms acid gel, quickly stirs gel
It smashes, the stirring and washing time is 1h, and temperature is 30 DEG C, and wash number is 2 times.Decompression filters 90% volume of removal after cleaning
Moisture, be added 1M NaOH solution tune pH to 7 dissolve gel-forming concentrated solution.
(5) ethanol precipitation
Pectin solution carries out ethanol precipitation after vacuum distillation concentration, and concentration ratio is 20% addition nothing of original solution volume
Extremely, ethyl alcohol volume final concentration of 70%, alcohol precipitation temperature is 4 DEG C to water-ethanol.
(6) 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 90.7%, yield 43.2%.
Claims (5)
1. a kind of compound pectin purification process, 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) adsorbent adsorbs
Adsorbent is added in filtered pectin solution to be adsorbed, adsorbent amount is with pectin dry weight ratio in step (1)
0.5-4:1, adsorption temp are 20-60 DEG C, adsorption time 0.5-4h；It is successively inhaled by centrifugation and filtering removal after absorption
Attached dose, repeating this step operation number is 0-4 times；
(4) 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；
(5) ethanol precipitation
Dehydrated alcohol is added in pectin concentrated solution in step (4) 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；
(6) 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. a kind of pectin purification process that one kind described in claim 1 is compound, it is characterised in that: pectin described in step 2
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 compound pectin purification process of one kind according to claim 1, it is characterised in that: absorption described in step 3
Agent is alkali alumina adsorbent, molecular sieve, silica gel, active carbon, atlapulgite, macroreticular resin XDA-7, macroreticular resin D3520
Deng one or more, absorbent particles size be 100 mesh~300 mesh.
4. the compound pectin purification process of one kind according to claim 1, it is characterised in that: acid described in step 4 is molten
Liquid is that 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, the preferably one or more of the sodium hydroxide of 1M, sodium carbonate, sodium bicarbonate, potassium hydroxide etc..
5. the method for gel ablution purifying pectin according to claim 1, it is characterised in that: fruit described in step 5
Glue concentrated solution mass concentration is 5-20%.
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|---|---|---|---|---|
| CN1184818A (en) * | 1997-12-16 | 1998-06-17 | 张文沂 | Method for purifying sun-flower seed low-ester pectine |
| CN1279286A (en) * | 2000-05-17 | 2001-01-10 | 华南农业大学 | Process for preparing gel medium of lysozyme affinity chromatography |
| CN102911288A (en) * | 2012-10-23 | 2013-02-06 | 陕西科技大学 | Method for decolouring and purifying pectin |
| CN103641929A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from persimmon peels |
| US20170073433A1 (en) * | 2015-09-10 | 2017-03-16 | The United States Of America, As Represented By The Secretary Of Agriculture | Processes to Produce Unpurified Polygalacturonic Acids from Plant Tissue Using Calcium Sequestering Compounds |
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2017
- 2017-11-20 CN CN201711159636.0A patent/CN109810205A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1184818A (en) * | 1997-12-16 | 1998-06-17 | 张文沂 | Method for purifying sun-flower seed low-ester pectine |
| CN1279286A (en) * | 2000-05-17 | 2001-01-10 | 华南农业大学 | Process for preparing gel medium of lysozyme affinity chromatography |
| CN102911288A (en) * | 2012-10-23 | 2013-02-06 | 陕西科技大学 | Method for decolouring and purifying pectin |
| CN103641929A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from persimmon peels |
| US20170073433A1 (en) * | 2015-09-10 | 2017-03-16 | The United States Of America, As Represented By The Secretary Of Agriculture | Processes to Produce Unpurified Polygalacturonic Acids from Plant Tissue Using Calcium Sequestering Compounds |
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Application publication date: 20190528 |