CN105646727A - Method for extracting high-activity corncob polysaccharide - Google Patents
Method for extracting high-activity corncob polysaccharide Download PDFInfo
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
The invention discloses a method for extracting high-activity corncob polysaccharide and belongs to the field of corncob polysaccharide. According to the method, dried corncobs are smashed, hot water adding is conducted, supernatant liquid is extracted in an ultrasonic immersion mode, concentration and alcohol precipitation are conducted, then, centrifugation is conducted, and crude polysaccharide is obtained; then, protein is removed through a Sevag method, purification is conducted through chromatography, ethyl alcohol precipitation separation, low-temperature drying and smashing are conducted, and sterling polysaccharide is obtained. The preparing process is environmentally friendly, acid and alkali waste water can not be produced greatly, and environment pollution can not occur; the active components of the corncob polysaccharide can be completely stored, the extracted corncob polysaccharide is high in purity and yield, production of by-products is reduced, and the method has wide application prospects.
Description
Technical field
The invention discloses the extracting method of a kind of high activity corn-cob polysaccharide, belong to corn-cob polysaccharide field.
Background technology
Semen Maydis is big in the cultivated area of China, distribution is wide, and annual production, up to hundred billion kilograms, occupies the 2nd, the world, and corn cob is the by-product of Maize Production and processing, and its yield reaches more than ten million ton, and corn cob is used in paper-making pulping except small part! The aspects such as biological sugaring and feed stripped, all the other major parts are dropped or burn, and cause serious waste of resources, and " in recent years, the exploitation of corn cob have been carried out big quantity research by domestic and international many researchers.
The main component of corn cob is based on cellulose, hemicellulose, lignin and xylan. Corn cob also has other compositions, such as crude protein, crude fat, saccharide, mineral etc. Corn cob can produce important industrial chemicals after treatment, such as high value added products such as reducing sugar, xylose, xylan, polyphenol, polysaccharide, furfural, xanthan gum, activated carbon from activated sludge, lignin, modified corn cores.
Bioactive polysaccharide participates in various vital movements, has various biological function. As body is had immunoregulation effect by polysaccharide, there is the aspects such as enhancing immunity, antitumor, blood sugar lowering, antiviral, anticoagulation, slow down aging
Function. In recent years, to the biological activity of corn-cob polysaccharide and pharmacological effect, there are reports, but the research of its extraction process is also less, and is generally adopted alkaline process and acid system. But, general acid carries, alkali puies forward technique and can destroy its molecular structure to a certain extent, thus affecting its biological activity, function, and uses a large amount of acid-base pair equipment requirements high in production, it is easy to cause environmental pollution.
Summary of the invention
The technical problem that present invention mainly solves: be generally adopted alkaline process and acid system for extracting corn-cob polysaccharide at present, but acid carries, alkali puies forward technique and can destroy its molecular structure to a certain extent, affect its biological activity, limit its function to use, and in producing, use a large amount of acid, alkali that equipment requirements is high, the problem easily causing environmental pollution, it is provided that the extracting method of a kind of high activity corn-cob polysaccharide, the present invention is pulverized by dry corn cob, heating
The ultrasonic lixiviate of water take supernatant carry out concentrating, precipitate with ethanol, more centrifugal to obtain crude polysaccharides, then with Sevag method isolating protein, then through purification by chromatography, ethanol precipitating separates, cold drying, pulverize, obtain polysaccharide sterling, preparation process environmental protection of the present invention, a large amount of acid, alkali waste water will not be produced, free from environmental pollution, and also the active component obtaining corn-cob polysaccharide can be saved completely, the corn-cob polysaccharide purity extracted is high, yield is high, and reduces the generation of by-product, is with a wide range of applications.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) 100��200g corn cob dried is taken, pulverized, cross 60��70 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 40��60 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 60��70 DEG C, extract 30��50min, and repeat extraction 2��3 times, feed the mixture into after extraction and centrifugal separator separates 10��15min under 5000��7000r/min rotating speed, take supernatant;
(2) above-mentioned supernatant is put in vacuum concentration pot under 0.085��0.091MPa, carry out concentrating under reduced pressure, until being concentrated into the 8��10% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 50��60 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides;
(3) above-mentioned prepared Corn Crude polysaccharide is added distilled water by solid-to-liquid ratio 1:6, stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 8000��9000r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.3��1:1.5 addition by volume in supernatant, 10��12h is stood after stirring mixing, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol;
(4) by corn-cob polysaccharide liquid bag filter dialysis treatment 10��12h obtained above, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 5��10% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed;
(5) by the dehydrated alcohol of 1:4 addition by volume in above-mentioned mixed liquor, it is sufficiently stirred for, at room temperature stand 5��6h, remove upper strata mixed liquor, taking precipitate, freezes precipitate freezing, puts into lyophilization in vacuum freeze drier, crushed after being dried crosses 85��95 mesh sieves, obtains corn-cob polysaccharide sterling.
The corn-cob polysaccharide that the present invention prepares is light tan powder, easy moisture absorption, soluble in water, it is insoluble in the organic solvents such as alcohol, ketone, ether, chloroform, purity reaches 88.9��92.2%, the composition of corn-cob polysaccharide is mainly xylose, Arabinose and glucose, has the multiple biological activity such as immunologic function improving human body.
The invention has the beneficial effects as follows:
(1) preparation process environmental protection of the present invention, will not produce a large amount of acid, alkali waste water, free from environmental pollution;
(2) active component of the corn-cob polysaccharide that the present invention prepares can be saved completely, and the corn-cob polysaccharide purity of extraction is high, and yield is high, is with a wide range of applications.
Detailed description of the invention
First 100��200g corn cob dried is taken, pulverized, cross 60��70 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 40��60 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 60��70 DEG C, extract 30��50min, and repeat extraction 2��3 times, feed the mixture into after extraction and centrifugal separator separates 10��15min under 5000��7000r/min rotating speed, take supernatant; Supernatant is put into vacuum concentration pot carries out concentrating under reduced pressure under 0.085��0.091MPa, until being concentrated into the 8��10% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 50��60 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides; Prepared Corn Crude polysaccharide is added distilled water by solid-to-liquid ratio 1:6, stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 8000��9000r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.3��1:1.5 addition by volume in supernatant, 10��12h is stood after stirring mixing, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol;The corn-cob polysaccharide liquid bag filter dialysis treatment 10��12h that will obtain, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 5��10% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed; By the dehydrated alcohol of 1:4 addition by volume in mixed liquor, it is sufficiently stirred for, at room temperature stands 5��6h, remove upper strata mixed liquor, taking precipitate, precipitate freezing is frozen, putting into lyophilization in vacuum freeze drier, crushed after being dried crosses 85��95 mesh sieves, obtains corn-cob polysaccharide sterling.
Example 1
First the 100g corn cob dried is taken, pulverized, cross 60 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 40 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 60 DEG C, extract 30min, and repeat to extract 2 times, feed the mixture into after extraction and centrifugal separator separates 10min under 5000r/min rotating speed, take supernatant; Supernatant is put into vacuum concentration pot carries out concentrating under reduced pressure under 0.085MPa, until being concentrated into the 8% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 50 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides; By solid-to-liquid ratio 1:6, prepared Corn Crude polysaccharide is added distilled water, and stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 8000r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.3 addition by volume in supernatant, after stirring mixing, stand 10h, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol; The corn-cob polysaccharide liquid bag filter dialysis treatment 10h that will obtain, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 5% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed; By the dehydrated alcohol of 1:4 addition by volume in mixed liquor, it is sufficiently stirred for, at room temperature stands 5h, remove upper strata mixed liquor, taking precipitate, precipitate freezing is frozen, putting into lyophilization in vacuum freeze drier, crushed after being dried crosses 85 mesh sieves, obtains corn-cob polysaccharide sterling.
The corn-cob polysaccharide that the present invention prepares is light tan powder, easy moisture absorption, soluble in water, it is insoluble in the organic solvents such as alcohol, ketone, ether, chloroform, purity reaches 88.9%, the composition of corn-cob polysaccharide is mainly xylose, Arabinose and glucose, has the multiple biological activity such as immunologic function improving human body.
Example 2
First the 150g corn cob dried is taken, pulverized, cross 65 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 50 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 65 DEG C, extract 40min, and repeat to extract 2 times, feed the mixture into after extraction and centrifugal separator separates 13min under 6000r/min rotating speed, take supernatant; Supernatant is put into vacuum concentration pot carries out concentrating under reduced pressure under 0.089MPa, until being concentrated into the 9% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 55 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides;By solid-to-liquid ratio 1:6, prepared Corn Crude polysaccharide is added distilled water, and stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 8500r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.4 addition by volume in supernatant, after stirring mixing, stand 11h, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol; The corn-cob polysaccharide liquid bag filter dialysis treatment 11h that will obtain, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 8% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed; By the dehydrated alcohol of 1:4 addition by volume in mixed liquor, it is sufficiently stirred for, at room temperature stands 5.5h, remove upper strata mixed liquor, taking precipitate, precipitate freezing is frozen, putting into lyophilization in vacuum freeze drier, crushed after being dried crosses 90 mesh sieves, obtains corn-cob polysaccharide sterling.
The corn-cob polysaccharide that the present invention prepares is light tan powder, easy moisture absorption, soluble in water, it is insoluble in the organic solvents such as alcohol, ketone, ether, chloroform, purity reaches 90.8%, the composition of corn-cob polysaccharide is mainly xylose, Arabinose and glucose, has the multiple biological activity such as immunologic function improving human body.
Example 3
First the 200g corn cob dried is taken, pulverized, cross 70 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 60 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 70 DEG C, extract 50min, and repeat to extract 3 times, feed the mixture into after extraction and centrifugal separator separates 15min under 7000r/min rotating speed, take supernatant; Supernatant is put into vacuum concentration pot carries out concentrating under reduced pressure under 0.091MPa, until being concentrated into the 10% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 60 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides; By solid-to-liquid ratio 1:6, prepared Corn Crude polysaccharide is added distilled water, and stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 9000r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.5 addition by volume in supernatant, after stirring mixing, stand 12h, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol; The corn-cob polysaccharide liquid bag filter dialysis treatment 12h that will obtain, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 10% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed; By the dehydrated alcohol of 1:4 addition by volume in mixed liquor, it is sufficiently stirred for, at room temperature stands 6h, remove upper strata mixed liquor, taking precipitate, precipitate freezing is frozen, putting into lyophilization in vacuum freeze drier, crushed after being dried crosses 95 mesh sieves, obtains corn-cob polysaccharide sterling.
The corn-cob polysaccharide that the present invention prepares is light tan powder, easy moisture absorption, soluble in water, it is insoluble in the organic solvents such as alcohol, ketone, ether, chloroform, purity reaches 92.2%, the composition of corn-cob polysaccharide is mainly xylose, Arabinose and glucose, has the multiple biological activity such as immunologic function improving human body.
Claims (1)
1. the extracting method of a high activity corn-cob polysaccharide, it is characterised in that concrete extraction step is:
(1) 100��200g corn cob dried is taken, pulverized, cross 60��70 mesh sieves and obtain corncob powder, by solid-to-liquid ratio 1:3 by corncob powder and 40��60 DEG C of hot water mixing, being extracted by mixture ultrasound wave, Extracting temperature is 60��70 DEG C, extract 30��50min, and repeat extraction 2��3 times, feed the mixture into after extraction and centrifugal separator separates 10��15min under 5000��7000r/min rotating speed, take supernatant;
(2) above-mentioned supernatant is put in vacuum concentration pot under 0.085��0.091MPa, carry out concentrating under reduced pressure, until being concentrated into the 8��10% of original volume, concentrated solution 1:4 by volume is joined in dehydrated alcohol, until deposit-free precipitates out, filter, with mass concentration 95% alcoholic solution washing leaching cake, filter cake after rinsing is put in baking oven, at 50��60 DEG C dry, crushed after being dried, sieve, obtain corn cob crude polysaccharides;
(3) above-mentioned prepared Corn Crude polysaccharide is added distilled water by solid-to-liquid ratio 1:6, stirring makes it dissolve, with in high speed centrifuge after dissolving, separate under 8000��9000r/min rotating speed, collect supernatant, by the Sevag reagent of 1:1.3��1:1.5 addition by volume in supernatant, 10��12h is stood after stirring mixing, zonal centrifugation after standing is separated, obtain supernatant, then supernatant is stood to layering, reclaim organic facies, collecting aqueous phase and be corn-cob polysaccharide liquid, in described Sevag reagent, chloroform is 4:1 with the volume ratio of n-butyl alcohol;
(4) by corn-cob polysaccharide liquid bag filter dialysis treatment 10��12h obtained above, by the liquid after dialysis again with porous resin chromatography column purification, and use sodium-chloride water solution eluting, obtain polysaccharide chromatographic solution, and collect the eluent containing polysaccharide, the eluent of polysaccharide is concentrated into the 5��10% of original volume, concentrated solution and polysaccharide chromatographic solution is mixed;
(5) by the dehydrated alcohol of 1:4 addition by volume in above-mentioned mixed liquor, it is sufficiently stirred for, at room temperature stand 5��6h, remove upper strata mixed liquor, taking precipitate, freezes precipitate freezing, puts into lyophilization in vacuum freeze drier, crushed after being dried crosses 85��95 mesh sieves, obtains corn-cob polysaccharide sterling.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325996A (en) * | 2017-12-23 | 2018-07-27 | 佛山科学技术学院 | A kind of method that abandoned biomass multi-direction synthetic utilizes |
| CN109987690A (en) * | 2019-04-02 | 2019-07-09 | 江苏师范大学 | A kind of algal polysaccharides base composite water disposal agent and the preparation method and application thereof |
-
2016
- 2016-02-04 CN CN201610078591.3A patent/CN105646727A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325996A (en) * | 2017-12-23 | 2018-07-27 | 佛山科学技术学院 | A kind of method that abandoned biomass multi-direction synthetic utilizes |
| CN109987690A (en) * | 2019-04-02 | 2019-07-09 | 江苏师范大学 | A kind of algal polysaccharides base composite water disposal agent and the preparation method and application thereof |
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