CN106967128A - A kind of extracting method of raffinose - Google Patents
A kind of extracting method of raffinose Download PDFInfo
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- CN106967128A CN106967128A CN201710180125.0A CN201710180125A CN106967128A CN 106967128 A CN106967128 A CN 106967128A CN 201710180125 A CN201710180125 A CN 201710180125A CN 106967128 A CN106967128 A CN 106967128A
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- raffinose
- light wave
- eluent
- extracting method
- exchange resin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
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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
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- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of extracting method of raffinose, comprise the following steps：1）Cottonseed Meal is chosen and crushed；2）Light wave extraction is carried out to the Cottonseed Meal after crushing, Extraction solvent is ethanol, and light wave power is set to 400 600w, and extraction time is 30 60min；3）Ceramic membrane filter is carried out to Cottonseed Meal extract solution and is concentrated under reduced pressure；4）Concentrate is passed sequentially through into macropore faintly acid styrene series anion exchange resin and macroporous acrylic system weak basic anion exchange resin is adsorbed and elution processing, eluent is obtained；5）Heating concentration is carried out to eluent, then handled with ethanol purification, raffinose finished product is finally made.Extraction efficiency of the present invention is high, and raffinose processes purity up to more than 95%, and device therefor instrument and solvent meet the standard of safety in production and environmental protection, production cost is low, suitable for large-scale industrialized production without obvious dangerous matter sources and murder by poisoning.
Description
Technical field
The present invention relates to raffinose extractive technique field, more particularly, to a kind of extracting method of raffinose.
Background technology
Raffinose (Raffinose) is also known as melitriose (Melitriose), gossypose, by galactolipin, glucose and fructose
It is combined into, belongs to oligosaccharide, be non-reducing sugar.It has been investigated that, raffinose is Bifidobacterium, acidophilus lactic acid bar in human body intestinal canal
The fabulous nutrient source of the beneficial bacteriums such as bacterium, can promote their propagation, so as to suppress the growth of spoilage organisms in enteron aisle, and reduce poisonous
The formation of tunning.Bifidobacterium fermentation raffinose produces substantial amounts of short chain fatty acids, can stimulate intestines peristalsis, increase excrement
Degree of wetting simultaneously keeps certain osmotic pressure, so as to prevent the generation of constipation.In addition, raffinose can improve the digestive function of human body,
Promote absorption of the human body to calcium, so as to strengthen body immunity, there is positive effect to prevention disease and anti-aging.Gossypose is also
The organ transplant protection that can be lived as human body and animal conveys the main component of liquid and extends viable bacteria body survival period at normal temperatures
Synergist.Raffinose it is acidproof, heat-resist, under 90% relative humidity also will not moisture absorption caking, itself can as food
Product additive is used, and improves the processing characteristics of food, prevents product brown stain, improves product quality, extends the shelf-life of product.Cotton
Seed sugar because with excellent physicochemical property and physiologically active, having been widely used for the industries such as food, medicine and cosmetics at present.
Raffinose is very wide in the distribution of nature, is to be distributed most wide oligosaccharide in plant in addition to sucrose, it is deposited extensively
It is in beet, cottonseed, honey, cabbage, yeast, potato, grape, wheat class, corn and the seed of legume, wherein
Content highest in cottonseed, about 4~9%.Cotton Seed produces substantial amounts of byproduct after cottonseed oil is extracted --- degreasing
The content of raffinose is held essentially constant in Cottonseed Meal, degreased cottonseed meal, therefore, and degreased cottonseed meal cake is industrial production cottonseed
The splendid raw material of sugar.
But under prior art conditions, the technological process of raffinose is extracted from degreased cottonseed meal in industrialized production
There are the deficiencies such as high cost, low yield, numerous and diverse flow.Therefore, it is the art to update and improve raffinose extraction process
The target of personnel's research and development.
The content of the invention
The purpose of the present invention is that in view of the shortcomings of the prior art there is provided a kind of extracting method of raffinose, prepared by this method
It is simple and the raffinose of high-purity can be obtained.
In order to achieve the above object, the present invention is achieved by the following technical solutions：
A kind of extracting method of raffinose, is followed the steps below：
（1）The selection and processing of raw material：Dry Cottonseed Meal is chosen, pulverizer is put into and carries out pulverization process；
（2）Light wave is extracted：Cottonseed Meal powder after crushing is subjected to light wave extraction with organic solvent, extract solution is filtered to obtain；
（3）Extract solution removal of impurities：By step（2）Extract solution is obtained through ceramic membrane filter, filtrate is obtained, it is then that the filtrate decompression is dense
Contracting filtrate obtains rough cottonseed liquid glucose to the 1/3 of original volume；
（4）Upper prop is adsorbed：Macropore faintly acid styrene series anion exchange resin on the rough cottonseed liquid glucose is adsorbed,
Gradient elution is carried out for 20%, 30%, 40% and 50% ethanol solution using volumetric concentration afterwards, collected volume concentration is
The eluent A of 50% ethanol solution；Again by eluent A by macroporous acrylic system weak basic anion exchange resin, after the completion of absorption
Eluted with eluting solvent, eluant, eluent is with extracting solution proportion=0.5L:1L, collects eluent B；
（5）Secondary concentration, purifying and crystallization：By step（4）Gained eluent B is depressurized under the conditions of heating-up temperature is 60-80 DEG C
Concentration, is concentrated into the 1/3 of original volume, then is purified with ethanol, and purifying obtains raffinose finished product after drying.
Preferably, the organic solvent during the light wave is extracted is that volumetric concentration is 75% ethanol solution.
Further, the light wave extraction time is set as 30-60min, and light wave power is 400-600w.
Further, ratio=5.5L of organic solvent and Cottonseed Meal during the light wave is extracted:1kg.
Further, the adsorption flow rate of the macropore faintly acid styrene series anion exchange resin is 1.5-3BV/hr,
Elution flow rate is 1.5-3BV/hr.
Further, the adsorption flow rate of macroporous acrylic system weak basic anion exchange resin is 2-4BV/hr, elution
Flow velocity is 2-4BV/hr.
Preferably, the eluting solvent is the acetone soln of volumetric concentration 75%.
Further, the ethanol and volume of concentrate ratio=0.3-0.5L:1L.
Beneficial effects of the present invention：
（1）By two kinds of different polymeric adsorbents, eluent and the resin of setting blade diameter length ratio and absorb-elute flow velocity, make product
Purity be greatly improved, purity can reach more than 95%；
（2）Solvent used in the present invention is nontoxic, cheap, volume production organic solvent, reduces organic solvent to health
The extent of injury and production cost, reduce the degree to environmental emission discarded object, meet green production and environmental protection standard；
（3）Cottonseed Meal is tentatively extracted using light wave, extraction efficiency is greatly accelerated, carrying for raffinose in raw material is improved
Rate is taken, industrial-scale production is adapted to, with good economic benefit.
Embodiment
With reference to embodiment and comparative example, the invention will be further described, so that those skilled in the art knows more about
The present invention, but and it is not so limited the present invention.
Embodiment 1
A kind of extracting method of raffinose, its step is performed as follows：
（1）The selection and processing of raw material：Dry Cottonseed Meal is chosen, pulverizer is put into and carries out pulverization process；
（2）Light wave is extracted：Cottonseed Meal powder after crushing is subjected to light wave extraction with volumetric concentration for 75% ethanol solution, the process
In, light wave extraction time is set as 30min, and light wave power is 600w, and ratio=5.5L of above-mentioned ethanol solution and Cottonseed Meal:
1kg, filters to obtain extract solution afterwards；
（3）Extract solution removal of impurities：By step（2）Extract solution is obtained through ceramic membrane filter, filtrate is obtained, it is then that the filtrate decompression is dense
Contracting filtrate obtains rough cottonseed liquid glucose to the 1/3 of original volume；
（4）Upper prop is adsorbed：By macropore faintly acid styrene series anion exchange resin on the rough cottonseed liquid glucose（Model
D301-G）Adsorbed, carry out gradient elution using volumetric concentration for 20%, 30%, 40% and 50% ethanol solution afterwards,
Collected volume concentration is the eluent A of 50% ethanol solution, during being somebody's turn to do, macropore faintly acid styrene series anion exchange resin
Adsorption flow rate be 1.5BV/hr, elution flow rate is 1.5BV/hr；Eluent A is passed through into macroporous acrylic system weak base anion again
Exchanger resin is adsorbed（Model D311）, eluted after the completion of absorption with the acetone soln of volumetric concentration 75%, eluant, eluent is with extracting
Solution proportion=0.5L:1L, collects eluent B, during being somebody's turn to do, the absorption stream of macroporous acrylic system weak basic anion exchange resin
Speed is 2BV/hr, and elution flow rate is 2BV/hr；
（5）Secondary concentration, purifying and crystallization：By step（4）Gained eluent B depressurizes dense under the conditions of heating-up temperature is 60 DEG C
Contracting, is concentrated into the 1/3 of original volume, then is purified with volumetric concentration for 75% ethanol solution, and ethanol solution and the volume of concentrate
Ratio=0.3L:1L, purifying obtains raffinose finished product after drying.
Embodiment 2
A kind of extracting method of raffinose, its step is performed as follows：
（1）The selection and processing of raw material：Dry Cottonseed Meal is chosen, pulverizer is put into and carries out pulverization process；
（2）Light wave is extracted：Cottonseed Meal powder after crushing is subjected to light wave extraction with volumetric concentration for 75% ethanol solution, the process
In, light wave extraction time is set as 45min, and light wave power is 500w, and ratio=5.5L of above-mentioned ethanol solution and Cottonseed Meal:
1kg, filters to obtain extract solution afterwards；
（3）Extract solution removal of impurities：By step（2）Extract solution is obtained through ceramic membrane filter, filtrate is obtained, it is then that the filtrate decompression is dense
Contracting filtrate obtains rough cottonseed liquid glucose to the 1/3 of original volume；
（4）Upper prop is adsorbed：By macropore faintly acid styrene series anion exchange resin on the rough cottonseed liquid glucose（Model
D301-G）Adsorbed, carry out gradient elution using volumetric concentration for 20%, 30%, 40% and 50% ethanol solution afterwards,
Collected volume concentration is the eluent A of 50% ethanol solution, during being somebody's turn to do, macropore faintly acid styrene series anion exchange resin
Adsorption flow rate be 2BV/hr, elution flow rate is 2BV/hr；Eluent A is exchanged by macroporous acrylic system weak base anion again
Resin is adsorbed（Model D311）, eluted after the completion of absorption with the acetone soln of volumetric concentration 75%, eluant, eluent is with extracting solution
Ratio=0.5L:1L, collects eluent B, and during being somebody's turn to do, the adsorption flow rate of macroporous acrylic system weak basic anion exchange resin is
3BV/hr, elution flow rate is 3BV/hr；
（5）Secondary concentration, purifying and crystallization：By step（4）Gained eluent B depressurizes dense under the conditions of heating-up temperature is 70 DEG C
Contracting, is concentrated into the 1/3 of original volume, then is purified with volumetric concentration for 75% ethanol solution, and ethanol solution and the volume of concentrate
Ratio=0.4L:1L, purifying obtains raffinose finished product after drying.
Embodiment 3
A kind of extracting method of raffinose, its step is performed as follows：
（1）The selection and processing of raw material：Dry Cottonseed Meal is chosen, pulverizer is put into and carries out pulverization process；
（2）Light wave is extracted：Cottonseed Meal powder after crushing is subjected to light wave extraction with volumetric concentration for 75% ethanol solution, the process
In, light wave extraction time is set as 60min, and light wave power is 400w, and ratio=5.5L of above-mentioned ethanol solution and Cottonseed Meal:
1kg, filters to obtain extract solution afterwards；
（3）Extract solution removal of impurities：By step（2）Extract solution is obtained through ceramic membrane filter, filtrate is obtained, it is then that the filtrate decompression is dense
Contracting filtrate obtains rough cottonseed liquid glucose to the 1/3 of original volume；
（4）Upper prop is adsorbed：By macropore faintly acid styrene series anion exchange resin on the rough cottonseed liquid glucose（Model
D301-G）Adsorbed, carry out gradient elution using volumetric concentration for 20%, 30%, 40% and 50% ethanol solution afterwards,
Collected volume concentration is the eluent A of 50% ethanol solution, during being somebody's turn to do, macropore faintly acid styrene series anion exchange resin
Adsorption flow rate be 3BV/hr, elution flow rate is 3BV/hr；Eluent A is exchanged by macroporous acrylic system weak base anion again
Resin is adsorbed（Model D311）, eluted after the completion of absorption with the acetone soln of volumetric concentration 75%, eluant, eluent is with extracting solution
Ratio=0.5L:1L, collects eluent B, and during being somebody's turn to do, the adsorption flow rate of macroporous acrylic system weak basic anion exchange resin is
4BV/hr, elution flow rate is 4BV/hr；
（5）Secondary concentration, purifying and crystallization：By step（4）Gained eluent B depressurizes dense under the conditions of heating-up temperature is 80 DEG C
Contracting, is concentrated into the 1/3 of original volume, then is purified with volumetric concentration for 75% ethanol solution, and ethanol solution and the volume of concentrate
Ratio=0.5L:1L, purifying obtains raffinose finished product after drying.
Comparative example
Original technique
（1）Drying and crushing：Cottonseed Meal is dried, particle diameter≤2mm is crushed to, Cottonseed Meal powder is obtained；
（2）Acid solution is extracted：By step（1）It is 8% hydrochloric acid solution extraction to obtain Cottonseed Meal powder and add volumetric concentration, and matter is used afterwards
Amount concentration is that 8% sodium hydroxide solution is neutralized, and filters to obtain filter residue and extract solution；
（3）Concentration centrifugation：By extract solution through being concentrated under reduced pressure into the 1/3 of original volume, then after centrifugation, filtering, filtrate is collected, is obtained
Cottonseed liquid glucose crude product, wherein, centrifugal rotational speed is 500r/min, and centrifugation time is 15min；
（4）Refining and concentrating：Cottonseed liquid glucose crude product is passed through into macroporous acrylic system weak basic anion exchange resin（Model D311）
Adsorption treatment is carried out, then is eluted with volumetric concentration for 75% ethanol solution, raffinose eluent is obtained；
（5）Dry：Above-mentioned raffinose eluent is dried after processing, raffinose finished product is obtained.
Experiment detection
Using Polyose extraction in raffinose finished product made from phend-sulphuric acid and colorimetric method for determining embodiment 1-3 and comparative example
Rate and purity, experimental result data such as table 1 below.
Table 1
| Group | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Recovery rate % | 20.45 | 22.63 | 21.20 | 10.16 |
| Purity % | 95.19 | 97.32 | 95.55 | 78.84 |
【Recovery rate %=（Polysaccharide quality/raw material gross mass in raffinose finished product）×100%】
【Purity %=（Polysaccharide quality/finished product gross mass in raffinose finished product）×100%】
The new technology of the present invention compares the pure of the raffinose finished product that original existing technique productions come out it can be seen from upper table 1
Raffinose recovery rate is obviously improved in degree and raw material.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvement can also be made, these improvement also should be regarded as the present invention's
Protection domain.
Claims (8)
1. a kind of extracting method of raffinose, it is characterised in that comprise the following steps：
（1）The selection and processing of raw material：Dry Cottonseed Meal is chosen, pulverizer is put into and carries out pulverization process；
（2）Light wave is extracted：Cottonseed Meal powder after crushing is subjected to light wave extraction with organic solvent, extract solution is filtered to obtain；
（3）Extract solution removal of impurities：By step（2）Extract solution is obtained through ceramic membrane filter, filtrate is obtained, it is then that the filtrate decompression is dense
Contracting filtrate obtains rough cottonseed liquid glucose to the 1/3 of original volume；
（4）Upper prop is adsorbed：Macropore faintly acid styrene series anion exchange resin on the rough cottonseed liquid glucose is adsorbed,
Gradient elution is carried out for 20%, 30%, 40% and 50% ethanol solution using volumetric concentration afterwards, collected volume concentration is
The eluent A of 50% ethanol solution；Again by eluent A by macroporous acrylic system weak basic anion exchange resin, after the completion of absorption
Eluted with eluting solvent, eluant, eluent is with extracting solution proportion=0.5L:1L, collects eluent B；
（5）Secondary concentration, purifying and crystallization：By step（4）Gained eluent B is depressurized under the conditions of heating-up temperature is 60-80 DEG C
Concentration, is concentrated into the 1/3 of original volume, then is purified with ethanol, and purifying obtains raffinose finished product after drying.
2. the extracting method of a kind of raffinose according to claim 1, it is characterised in that organic in the light wave extraction
Solvent is that volumetric concentration is 75% ethanol solution.
3. a kind of extracting method of raffinose according to claim 1, it is characterised in that the light wave extraction time setting
For 30-60min, light wave power is 400-600w.
4. the extracting method of a kind of raffinose according to claim 1, it is characterised in that the light wave is organic molten in extracting
Agent and ratio=5.5L of Cottonseed Meal:1kg.
5. a kind of extracting method of raffinose according to claim 1, it is characterised in that the macropore faintly acid styrene
The adsorption flow rate of series anion exchange resin is 1.5-3BV/hr, and elution flow rate is 1.5-3BV/hr.
6. a kind of extracting method of raffinose according to claim 1, it is characterised in that macroporous acrylic system weak base
The adsorption flow rate of anion exchange resin is 2-4BV/hr, and elution flow rate is 2-4BV/hr.
7. the extracting method of a kind of raffinose according to claim 1, it is characterised in that the eluting solvent is that volume is dense
Spend 75% acetone soln.
8. the extracting method of a kind of raffinose according to claim 1, it is characterised in that the ethanol and the volume of concentrate
Ratio=0.3-0.5L:1L.
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| CN201710180125.0A CN106967128A (en) | 2017-03-24 | 2017-03-24 | A kind of extracting method of raffinose |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527377A (en) * | 2021-08-09 | 2021-10-22 | 内蒙古泓兴生物科技有限公司 | Method for preparing raffinose from raffinose oligosaccharide and raffinose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372498A (en) * | 2008-09-27 | 2009-02-25 | 浙江大学 | Process for preparing high-purity raffinose from degreased cottonseed meal |
| CN101376666A (en) * | 2008-09-27 | 2009-03-04 | 浙江大学 | Method for improving purity of raffinose |
| CN102351917A (en) * | 2011-09-14 | 2012-02-15 | 北京科技大学 | Method for extracting raffinose from cotton seed meal |
| CN102675317A (en) * | 2012-05-29 | 2012-09-19 | 福建省安溪县南洋茶厂 | Method for extracting a plurality of kinds of active ingredients from tea leaves simultaneously |
-
2017
- 2017-03-24 CN CN201710180125.0A patent/CN106967128A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372498A (en) * | 2008-09-27 | 2009-02-25 | 浙江大学 | Process for preparing high-purity raffinose from degreased cottonseed meal |
| CN101376666A (en) * | 2008-09-27 | 2009-03-04 | 浙江大学 | Method for improving purity of raffinose |
| CN102351917A (en) * | 2011-09-14 | 2012-02-15 | 北京科技大学 | Method for extracting raffinose from cotton seed meal |
| CN102675317A (en) * | 2012-05-29 | 2012-09-19 | 福建省安溪县南洋茶厂 | Method for extracting a plurality of kinds of active ingredients from tea leaves simultaneously |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527377A (en) * | 2021-08-09 | 2021-10-22 | 内蒙古泓兴生物科技有限公司 | Method for preparing raffinose from raffinose oligosaccharide and raffinose |
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Application publication date: 20170721 |