CN102351917A - Method for extracting raffinose from cotton seed meal - Google Patents
Method for extracting raffinose from cotton seed meal Download PDFInfo
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- CN102351917A CN102351917A CN2011102704265A CN201110270426A CN102351917A CN 102351917 A CN102351917 A CN 102351917A CN 2011102704265 A CN2011102704265 A CN 2011102704265A CN 201110270426 A CN201110270426 A CN 201110270426A CN 102351917 A CN102351917 A CN 102351917A
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Abstract
The invention belongs to the field of plant extraction, and relates to a method for extracting raffinose from cotton seed meal. The method comprises the following steps of: extracting the cotton seed meal by using water to obtain crude raffinose solution; removing macromolecular substances from the crude raffinose solution by adding a flocculating agent or using an ultrafiltration membrane to obtain primarily purified raffinose solution; adsorbing the raffinose in the primarily purified raffinose solution by using an adsorbent; eluting the raffinose from the adsorbent by using ethanol or methanol, and collecting eluent to obtain recovered raffinose solution; and concentrating the recovered raffinose solution, adding ethanol solution, adding raffinose crystal seeds for crystallizing, and separating and drying crystals to obtain purified raffinose. Compared with the conventional alcohol extraction method, the method has the advantages that the method is clean, low in energy consumption and cost, easy to operate, high in recovery rate and the like.
Description
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Technical field
The invention belongs to field of plant extraction, relate to a kind of method of from cottonseed meal, extracting raffinose.
Background technology
Raffinose is claimed raffinose again, is the oligose that content is only second to sucrose in the oligose that exists in the vegitabilia, and raffinose has plurality of health care functions to human body; Has the bifidus bacillus of making had significant proliferation; Significantly improve intestinal microflora, improve the just property of constipation and diarrhea patient, different physiological roles such as anticancer; On March 9th, 2010; China Ministry of Health has announced that 7 kinds of article that comprise the cottonseed oligose are new resource food (Bao Shuyun, Guangzhou chemical industry, 2011; 3,20).In addition, raffinose is also having certain application aspect medicine and the microorganism, can also synthesize glycolipid as the surrogate of anakinetomer, as the stabilizing component of emulsion system etc.
China is one of maximum in the world cotton state of product, and cotton gross annual output amount is 600-700 ten thousand t, and the cottonseed annual production is 960-1100 ten thousand t (Zhou Dongli etc., grain and grease, 2010,12,39).Contain a large amount of raffinoses in the cottonseed meal; Its content is approximately 4%-9%; Yet now domesticly but cottonseed meal directly is used for animal feed; Bioavailability is extremely low; Change the situation that the direct as fertilizer sources of present cottonseed meal uses; It is carried out deep processing, and the extraction functionality oligose has huge economic benefit and social benefit.
At present, the research of in cottonseed meal, extracting raffinose is less, generally all uses methyl alcohol or ethanolic soln extraction method to extract raffinose (Dai Weidong etc. for example, foodstuffs industry science and technology, 2009,4,208; And CN200710121866.8).The shortcoming that the method for using alcohol directly from cottonseed meal, to extract raffinose exists is: 1) use a large amount of alcohol, these alcohol need distill recovery after use, make cost improve; With 2) when using alcohol from cottonseed meal, to extract raffinose, can make later separation complex steps and cost high deleterious gossypol stripping in the cottonseed meal, also caused the rate of recovery of raffinose low simultaneously.
Summary of the invention
The object of the invention provides a kind of new extraction raffinose method, big, the shortcomings such as the raffinose rate of recovery is low, industrial cost's height of the usage quantity that this method can overcome alcohol in the existing ethanol-extracted method.
A kind of method of from cottonseed meal, extracting raffinose comprises the steps:
[1], (1) water under 30 ~ 80 ℃ of temperature carries out lixiviate to cottonseed meal, separates then and removes solid, obtains thick raffinose solution, wherein the mass volume ratio of cottonseed meal and water is 1:3 g/mL ~ 1:10 g/mL;
(2) add flocculation agent and perhaps use ultra-filtration membrane to remove the macromolecular substance in the said thick raffinose solution, obtain the raffinose solution of preliminary purification, said macromolecular substance comprises protein and polysaccharide;
(3) raffinose in the raffinose solution of the said preliminary purification of use adsorbents adsorb;
(4) under 30～80 ℃ of temperature, to use concentration be 30% ~ 80% ethanol or methyl alcohol with raffinose wash-out from the said sorbent material, collects elutriant and obtain reclaiming raffinose solution;
(5) with said recovery raffinose solution concentration to 1/8 ~ 1/10 of original volume; Add 50% ~ 80% ethanolic soln that concentrates 1 ~ 3 times of volume of liquid glucose; Add the raffinose crystal seed then and carry out crystallization, 0 ~ 4 ℃ of growing the grain 1 ~ 3 day obtains crystal separation and oven dry the raffinose of purifying.
[2], according to [1] described method, wherein said cottonseed meal is the dephenolization cottonseed dregs of rice or the dephenolization cottonseed dregs of rice not.
[3], according to [1]] described method, wherein said water is deionized water.
[4], according to [1] described method, wherein said lixiviate is carried out 1-3 time, each 1 ~ 3h.
[5], according to [1] described method, wherein said ultra-filtration membrane is a hollow fiber ultrafiltration membrane.
[6], according to [1] described method, wherein said flocculation agent is selected from one or more in chitosan, ZTC1+1 finings II type, 101 fruit juice clarifiers, trichoroacetic acid(TCA) (TCA), polyacrylic acid (PAC), the polyacrylamide.
[7], according to [1] described method, it is that polymeric adsorbent, nonpolar gel-type acrylic acid series polymeric adsorbent, bonding have the silica gel of C18 and the silica gel that bonding has C30 that wherein said sorbent material is selected from granulated active carbon, nonpolar macroporous type polystyrene polymeric adsorbent, nonpolar macroporous type acrylic acid series polymeric adsorbent, nonpolar gel type polystyrene.
[8], the described method of root [1], wherein said absorption is carried out Static Adsorption through directly in the raffinose solution of said preliminary purification, adding sorbent material.
[9], according to [1] described method, wherein said absorption is carried out dynamic adsorption through the raffinose solution with said preliminary purification through the adsorption column that sorbent material is housed.
[10], according to [1] each described method, wherein the said wash-out of step (4) washes out up to no raffinose; Wherein said the concentrating of step (5) carried out through underpressure distillation.
Method provided by the invention is utilized the water-fast character of gossypol, with cottonseed meal as raw material with water as the solvent extraction raffinose.Extract after the raffinose technology,, can carry out simple dephenolize again and handle (for example cottonseed meal being handled), can be used as high protein feed then with diluted acid or alcohols etc. for the cottonseed meal that contains gossypol; For the cottonseed meal that does not contain gossypol, can directly be used as high protein feed.Wherein isolated macromolecular substance can be put back in the cottonseed meal as feed again, the nutritive ingredient of cottonseed meal when being used as feed with assurance.Ultra-filtration membrane that uses in the inventive method or sorbent material can be reused after cleaning.
Method of the present invention is followed the example of with alcohol extracting of the prior art and is compared, and has the following advantages:
1,, make the leaching process cleanliness without any pollution, and production cost is than using alcohol to reduce greatly as extracting solvent because what extract that solvent uses is water.
2, because the amount of the alcohol that in technological process, uses significantly reduces, energy consumption and cost that pure recovery causes have been reduced.
3, make water avoid the stripping of gossypol, make that extraction process is more simple and yield raffinose is high as solvent.
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Embodiment
The present invention combines following examples to further specify, but is not restriction the present invention.
Embodiment 1
Taking by weighing 100g cottonseed meal (raffinose content is 5.8%), is that 1:3 (g/mL) adds deionized water by mass volume ratio, and 40 ℃ are extracted 1 hour 3 times, through deposition, filter, centrifugal after, thick raffinose solution.Adopt hollow fiber ultrafiltration tunica fibrosa (molecular weight cut-off is 10000 Dalton) to carry out ultrafiltration, get the raffinose solution of purifying by the 6mL/min flow velocity.Under 40 ℃ of conditions, the employing gac is a sorbent material, is that 1:10 ~ 1:20 carries out Static Adsorption with the mass volume ratio.Under 50 ℃ of conditions,, collect elutriant and obtain reclaiming raffinose solution with 50% ethanolic soln vibration wash-out 30min.Be concentrated into 1/8 of original volume with reclaiming the distillation of raffinose solution decompression; 1:3 adds 60% ethanolic soln by volume; Add mark article raffinose then and carry out crystallization; The add-on of mark article raffinose is 0.05g/L; 0 ℃ of growing the grain 3 days; Separate and dry crystal getting raffinose product 5.18g, purity of raffinose can reach 93%, and extract yield is 83%.
Embodiment 2
Taking by weighing 200g cottonseed meal (raffinose content is 5.6%), is that 1:4 (g/mL) adds deionized water by mass volume ratio, and 60 ℃ are extracted 3 hours 1 time, through deposition, filter, centrifugal after, thick raffinose solution.1% chitosan solution that adds thick raffinose liquor capacity 1/100 flocculates, the centrifuging and taking supernatant, the raffinose solution of purifying.Under 60 ℃ of conditions, employing is filled with nonpolar macroporous type acrylic acid series polymeric adsorbent absorption exchange column and carries out adsorption treatment, and flow velocity is about 4mL/min.Under 50 ℃ of conditions, with 30% methanol solution wash-out resin absorption exchange column, flow velocity 3mL/min does not have raffinose to elutriant, collects elutriant and obtains reclaiming raffinose solution.Be concentrated into 1/9 of original volume with reclaiming the distillation of raffinose solution decompression; 1:1 adds 80% ethanolic soln by volume; Add mark article raffinose then and carry out crystallization; The add-on of mark article raffinose is 0.08g/L; 3 ℃ of growing the grains 2 days; Separate and dry crystal getting raffinose product 10.35g, raffinose content can reach 92%, and extraction yield is 85%.
Embodiment 3
Taking by weighing 200g cottonseed meal (raffinose content is 5.6%), is that 1:5 (g/mL) adds deionized water by mass volume ratio, and 60 ℃ are extracted 1.5 hours 2 times, through deposition, filter, centrifugal after, thick raffinose solution.Adopt hollow fiber ultrafiltration membrane (molecular weight cut-off is 10000 Dalton) to carry out ultrafiltration, get the raffinose solution of purifying by the 8mL/min flow velocity.Under 70 ℃ of conditions, employing is filled with bonding has the silica gel adsorption exchange column of C18 to carry out adsorption treatment, and flow velocity is about 5mL/min.Under 60 ℃ of conditions, with 60% ethanolic soln wash-out resin absorption exchange column, flow velocity 2.5mL/min does not have raffinose to elutriant, collects elutriant and obtains reclaiming raffinose solution.Be concentrated into 1/9 of original volume with reclaiming the distillation of raffinose solution decompression; Add 70% ethanolic soln by 2 times of volumes of concentrated liquid glucose; Add mark article raffinose then and carry out crystallization; The add-on of mark article raffinose is 0.06g/L; 4 ℃ of growing the grains 1 day; Separate and dry crystal getting raffinose product 9.68g, raffinose content can reach 95%, and extraction yield is 82%.
Embodiment 4
Taking by weighing 200g cottonseed meal (raffinose content is 5.6%), is that 1:6 (g/mL) adds deionized water by mass volume ratio, and 80 ℃ are extracted 2.5 hours 2 times, through deposition, filter, centrifugal after, thick raffinose solution.Add 100% trichoroacetic acid(TCA) (TCA) protein precipitation of raffinose liquor capacity 1/9, put 4 ℃ of refrigerator overnight, the centrifuging and taking supernatant, the raffinose solution of purifying.Under 80 ℃ of conditions, adopting and being filled with nonpolar gel type polystyrene is that polymeric adsorbent absorption exchange column carries out adsorption treatment, and flow velocity is about 9mL/min.Under 40 ℃ of conditions, with 30% ethanolic soln wash-out resin absorption exchange column, flow velocity 4.5mL/min does not have raffinose to elutriant, collects elutriant and obtains reclaiming raffinose solution.Be concentrated into 1/10 of original volume with reclaiming the distillation of raffinose solution decompression; Add 50% ethanolic soln by 3 times of volumes of concentrated liquid glucose; Add mark article raffinose then and carry out crystallization; The add-on of mark article raffinose is 0.10g/L; 0 ℃ of growing the grain 3 days; Separate and dry crystal getting raffinose product 9.65g, raffinose content can reach 94%, and extraction yield is 81%.
Embodiment 5
Taking by weighing 200g cottonseed meal (raffinose content is 5.6%), is that 1:7 (g/mL) adds deionized water by mass volume ratio, and 70 ℃ are extracted 1.5 hours 3 times, through deposition, filter, centrifugal after, thick raffinose solution.Adopt hollow fiber ultrafiltration membrane (molecular weight cut-off is 10000 Dalton) to carry out ultrafiltration, get the raffinose solution of purifying by the 10mL/min flow velocity.Under 70 ℃ of conditions, employing is filled with active carbon adsorption column and carries out adsorption treatment, and flow velocity is about 5mL/min.Under 60 ℃ of conditions, with 30% methanol solution wash-out charcoal absorption exchange column, flow velocity 2.5mL/min does not have raffinose to elutriant, collects elutriant and obtains reclaiming raffinose solution.Be concentrated into 1/9 of original volume with reclaiming the distillation of raffinose solution decompression; Add 75% ethanolic soln by 1 times of volume of concentrated liquid glucose; Add mark article raffinose then and carry out crystallization; The add-on of mark article raffinose is 0.09g/L; 3 ℃ of growing the grains 3 days; Separate and dry crystal getting raffinose product 10.26g, raffinose content can reach 95%, and extraction yield is 87%.
Claims (10)
1. method of from cottonseed meal, extracting raffinose is characterized in that may further comprise the steps:
(1) water carries out lixiviate to cottonseed meal under 30 ~ 80 ℃ of temperature, separates then and removes solid, obtains thick raffinose solution, and wherein the mass volume ratio of cottonseed meal and water is 1:3 g/mL ~ 1:10 g/mL;
(2) add flocculation agent and perhaps use ultra-filtration membrane to remove the macromolecular substance in the said thick raffinose solution, obtain the raffinose solution of preliminary purification, said macromolecular substance comprises protein and polysaccharide;
(3) raffinose in the raffinose solution of the said preliminary purification of use adsorbents adsorb;
(4) under 30～80 ℃ of temperature, to use concentration be 30% ~ 80% ethanol or methyl alcohol with raffinose wash-out from the said sorbent material, collects elutriant and obtain reclaiming raffinose solution;
(5) with said recovery raffinose solution concentration to 1/8 ~ 1/10 of original volume; Add 50% ~ 80% ethanolic soln that concentrates 1 ~ 3 times of volume of liquid glucose; Add the raffinose crystal seed then and carry out crystallization, 0 ~ 4 ℃ of growing the grain 1 ~ 3 day obtains crystal separation and oven dry the raffinose of purifying.
2. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said cottonseed meal of step (1) is the dephenolization cottonseed dregs of rice or the dephenolization cottonseed dregs of rice not.
3. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said water of step (1) is deionized water.
4. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein each 1 ~ 3h is carried out in the said lixiviate of step (1) 1-3 time.
5. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said ultra-filtration membrane of step (2) is a hollow fiber ultrafiltration membrane.
6. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said flocculation agent of step (2) is selected from one or more in chitosan, ZTC1+1 finings II type, 101 fruit juice clarifiers, trichoroacetic acid(TCA) (TCA), polyacrylic acid (PAC), the polyacrylamide (PAM).
7. according to the said method of from cottonseed meal, extracting raffinose of claim 1, it is that polymeric adsorbent, nonpolar gel-type acrylic acid series polymeric adsorbent, bonding have the silica gel of C18 and the silica gel that bonding has C30 that wherein said step (3) sorbent material is selected from granulated active carbon, nonpolar macroporous type polystyrene polymeric adsorbent, nonpolar macroporous type acrylic acid series polymeric adsorbent, nonpolar gel type polystyrene.
8. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said absorption of step (3) is carried out Static Adsorption through directly in the raffinose solution of said preliminary purification, adding sorbent material.
9. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein the said absorption of step (3) is carried out dynamic adsorption through the raffinose solution with said preliminary purification through the adsorption column that sorbent material is housed.
10. according to the said method of from cottonseed meal, extracting raffinose of claim 1, wherein carry out the said wash-out of step (4) and wash out up to no raffinose; Said the concentrating of step (5) carried out through underpressure distillation.
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Cited By (10)
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| CN102875607A (en) * | 2012-09-28 | 2013-01-16 | 浙江大学 | Separation and purification method of raffinose |
| CN102898486A (en) * | 2012-09-21 | 2013-01-30 | 晨光生物科技集团股份有限公司 | Comprehensive method for preparation of raffinose and gossypol from cottonseed meal |
| CN103445229A (en) * | 2013-09-09 | 2013-12-18 | 南京农业大学 | Method for simultaneously and effectively removing laver protein and laver polysaccharide from laver extracting solution |
| CN103724379A (en) * | 2013-12-31 | 2014-04-16 | 晨光生物科技集团股份有限公司 | Method for extracting raffinose from cottonseed meal dephenolization solution |
| CN104672343A (en) * | 2015-02-11 | 2015-06-03 | 唐泽光 | Extracting and purifying method of raffino-oligosaccharide |
| CN106866750A (en) * | 2017-03-24 | 2017-06-20 | 合肥云都棉花有限公司 | A kind of method that raffinose is extracted from Cottonseed Meal |
| CN106967128A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of extracting method of raffinose |
| CN106967127A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of method that degreased cottonseed meal extracts raffinose |
| CN106967130A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of method that raffinose is extracted from Cottonseed Meal |
| CN108085424A (en) * | 2017-12-29 | 2018-05-29 | 天圣制药集团股份有限公司 | A kind of preparation method of medical cane sugar |
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Cited By (13)
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| CN102898486B (en) * | 2012-09-21 | 2015-07-22 | 晨光生物科技集团股份有限公司 | Comprehensive method for preparation of raffinose and gossypol from cottonseed meal |
| CN102898486A (en) * | 2012-09-21 | 2013-01-30 | 晨光生物科技集团股份有限公司 | Comprehensive method for preparation of raffinose and gossypol from cottonseed meal |
| CN102875607A (en) * | 2012-09-28 | 2013-01-16 | 浙江大学 | Separation and purification method of raffinose |
| CN102875607B (en) * | 2012-09-28 | 2015-03-04 | 浙江大学 | Separation and purification method of raffinose |
| CN103445229A (en) * | 2013-09-09 | 2013-12-18 | 南京农业大学 | Method for simultaneously and effectively removing laver protein and laver polysaccharide from laver extracting solution |
| CN103724379A (en) * | 2013-12-31 | 2014-04-16 | 晨光生物科技集团股份有限公司 | Method for extracting raffinose from cottonseed meal dephenolization solution |
| CN103724379B (en) * | 2013-12-31 | 2016-03-23 | 晨光生物科技集团股份有限公司 | The method of raffinose is extracted from cotton dregs dephenolizing solution |
| CN104672343A (en) * | 2015-02-11 | 2015-06-03 | 唐泽光 | Extracting and purifying method of raffino-oligosaccharide |
| CN106866750A (en) * | 2017-03-24 | 2017-06-20 | 合肥云都棉花有限公司 | A kind of method that raffinose is extracted from Cottonseed Meal |
| CN106967128A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of extracting method of raffinose |
| CN106967127A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of method that degreased cottonseed meal extracts raffinose |
| CN106967130A (en) * | 2017-03-24 | 2017-07-21 | 合肥云都棉花有限公司 | A kind of method that raffinose is extracted from Cottonseed Meal |
| CN108085424A (en) * | 2017-12-29 | 2018-05-29 | 天圣制药集团股份有限公司 | A kind of preparation method of medical cane sugar |
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Application publication date: 20120215 |