CN1386764A - Process for decolouring and refining oleaster gum polyose - Google Patents

Process for decolouring and refining oleaster gum polyose Download PDF

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Publication number
CN1386764A
CN1386764A CN 02117954 CN02117954A CN1386764A CN 1386764 A CN1386764 A CN 1386764A CN 02117954 CN02117954 CN 02117954 CN 02117954 A CN02117954 A CN 02117954A CN 1386764 A CN1386764 A CN 1386764A
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China
Prior art keywords
ethanol
polyose
elaeagni angustifoliae
colloidal sol
water
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CN 02117954
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CN1243024C (en
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苏为平
杨宇明
董丽松
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Publication of CN1243024C publication Critical patent/CN1243024C/en
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Abstract

A refining process for decolouring oleaster gum polyose includes dissolving oleaster gum in water, filtering, vacuum concentrating, stirring while slowely adding alcohol, detecting the polyose liquid/alcohol sol with red laser, stopping adding alcohol when the conic angle of laser beam is 90 deg.C, standing for 20-30 hr, stirring while adding it to alcohol to generate oleaster gum polyose particles, filtering, washing the precipitate with alcohol, and vacuum drying. Its advantage is high effect on removing polyphenol (85-95%).

Description

Process for decolouring and refining oleaster gum polyose
Technical field: the invention belongs to process for decolouring and refining oleaster gum polyose.
Background technology: Gummi Elaeagni Angustifoliae is that narrow-leaved oleaster does effusive a kind of polysaccharide that can be used in food and the medicine, and physicochemical property and gum arabic are close.Contain mechanical impurity and impurity atom in the Gummi Elaeagni Angustifoliae virgin rubber.But the method report that does not still have the purifying Gummi Elaeagni Angustifoliae at present.Oleaster gum polyose is through removing mechanical impurity.Can not effectively slough foreign pigment wherein after the filtration.Foreign pigment mainly is a polyphenols, is unhelpful for use these polyphenols of Gummi Elaeagni Angustifoliae in medicament.
The Sudan Gum-arabic of similar Gummi Elaeagni Angustifoliae with make the aqueous solution after filtration then spraying drying powder-forming in food and medicine, use (seeing chemical industry macropaedia V14 (1032)), the foreign pigment in the polysaccharide generally removes with the alcohol method of washing.Foreign pigment in the Gummi Elaeagni Angustifoliae is difficult to removing of higher degree with the general pure precipitator method, mainly be because add after a certain amount of alcohol, continuous sedimentary polysaccharide can form doughy micelle, bring polyphenols in micelle, form the pink colour micelle, so not only can not a high proportion ofly remove coloring matter, micelle aftertreatment dehydration is also difficult.And the hard agglomerate of dehydration back formation, be inconvenient to use.
The water dissolvable polysaccharide, comprise semi-synthetic polysaccharide such as natural water soluble polysaccharides such as Sargassum polysaccharides, gummy polysaccharide, mucopolysaccharide and carboxymethyl cellulose in water/ethanol double solvent, ascending with alcohol concn, change colloidal sol into from solution, sol particles is constantly grown, to becoming visible particles, concerning a kind of polysaccharide, in water/ethanol, adjust the alcoholic acid ratio, the polysaccharide that molecular weight is big, it is faster that particle is grown up, and to precipitation occurring, this is a kind of common methods of polysaccharide molecule with molecular-weight gradation.But in the polysaccharide purification process, polysaccharide colloidal sol has a phase inversion point when adjusting proportion of ethanol, and in this point, higher proportion of ethanol can make the sudden contraction of polysaccharide colloidal sol, forms high moisture micelle, is unfavorable for removing impurity.It is a critical technological point of polysaccharide purification.
Summary of the invention: the purpose of this invention is to provide a kind of process for decolouring and refining oleaster gum polyose.
By a branch of red laser monitoring polysaccharide water/ethanol colloidal sol, measure the point of instability of polysaccharide colloidal sol in polysaccharide water/ethanol double solvents.When only with water being solvent and low ratio ethanol double solvents, laser beam becomes the visible light beam of wire in solution.When polysaccharide soln begins to form colloidal sol, light beam has low scattering, this moment solution in the polysaccharide polymer particle less than 33nm, rising with proportion of ethanol in water/ethanol double solvents, the polysaccharide polymer particle is constantly grown up, and the laser light beam begins to become taper by Strahlungseintritt, and proportion of ethanol is high more, angle of taper is big more, can measure unstable stagnation point by laser post angle of taper.After bevel angle was greater than certain angle, solution began to occur suspended particles by even colloidal sol.At this moment colloidal sol becomes labile state.Further the polysaccharide particle can precipitate suddenly and form high moisture solid-state micelle and carry a large amount of impurity, makes subsequent purification work trouble.In most polysaccharide water/ethanol colloidal sol, hot laser light beam coning angle is lower than 90 ° of ∠ when spending, and colloidal sol is stable, greater than 90 ° of ∠, colloidal sol instability.Therefore, red laser light beam coning angle is most polysaccharide water/unsettled stagnation point of ethanol colloidal sol at 90 ° of degree of ∠.This moment, the part oleaster gum polyose formed the particle of about 0.5-1 μ m.
The present invention with Gummi Elaeagni Angustifoliae through water dissolution, filter after, through vacuum concentration, form weight concentration 20%-40% Gummi Elaeagni Angustifoliae solution, under agitation add ethanol gradually, Gummi Elaeagni Angustifoliae solution and alcoholic acid volume ratio are 0.7-1: 1 o'clock, with a branch of red laser monitoring polysaccharide water/ethanol colloidal sol, when the laser light beam becomes taper by Strahlungseintritt, laser light beam coning angle is oleaster gum polyose water/unsettled stagnation point of ethanol colloidal sol at 90 ° of degree of ∠, stops to add ethanol, and this colloidal sol was placed 20-30 hour; Join gradually in the ethanol this colloidal sol is under agitation anti-phase, form the particulate deposits of oleaster gum polyose, water and volumes of aqueous ethanol are than being 0.1-0.2: 1, with sedimentation and filtration, with the ethanol washing and precipitating, can obtain white oleaster gum polyose fine powder, vacuum-drying must be made with extra care Gummi Elaeagni Angustifoliae.
Process for purification of the present invention once removes polyphenol colored substance efficient can reach 85-95%.In decolorization, measure the point of instability of oleaster gum polyose water/ethanol colloidal sol with red laser beam, can effectively remove the polyphenol in the Gummi Elaeagni Angustifoliae, do not introduce other Harmful chemicals, and what form is the meal of polysaccharide, aftertreatment technology is simple.
Embodiment is as follows:
Embodiment 1: get 30g Gummi Elaeagni Angustifoliae virgin rubber, be dissolved in the 300ml water, be heated to 85 ℃, the deactivation oxydase filters this solution, is concentrated to 90ml, add ethanol gradually under stirring, be added to liquor capacity and be about 300ml, stop adding ethanol during with light scattering determining the best amount of alcohol added, solution was placed 20 hours, to join gradually under this solution stirring in the 500ml ethanol, Gummi Elaeagni Angustifoliae becomes powder shape precipitation, filters, with 30ml ethanol washing and precipitating, vacuum-drying gets white refining arrow-leaved oleaster rubber powder 27g.Spectrographic determination removes polyphenol impurity 85%.
Embodiment 2: get 10g Gummi Elaeagni Angustifoliae virgin rubber, be dissolved in the 300ml water, be heated to 85 ℃, the deactivation oxydase filters this solution, is concentrated to 90ml, add ethanol gradually under stirring, be added to liquor capacity and be about 500ml, stop adding ethanol during with light scattering determining the best amount of alcohol added, solution was placed 24 hours, to join gradually under this solution stirring in the 700ml ethanol, Gummi Elaeagni Angustifoliae becomes powder shape precipitation, filters, with 30ml ethanol washing and precipitating, vacuum-drying gets white refining arrow-leaved oleaster rubber powder 6g.Spectrographic determination removes polyphenol impurity 85%.
Embodiment 3: get 50g Gummi Elaeagni Angustifoliae virgin rubber, be dissolved in the 300ml water, be heated to 85 ℃, the deactivation oxydase filters this solution, is concentrated to 90ml, add ethanol under the high-power stirring gradually, being added to liquor capacity is 300ml, stops adding ethanol during with light scattering determining the best amount of alcohol added, solution was placed 30 hours, to join gradually under this solution stirring in the 500ml ethanol, Gummi Elaeagni Angustifoliae becomes powder shape precipitation, filters, with 30ml ethanol washing and precipitating, vacuum-drying gets white refining arrow-leaved oleaster rubber powder 45g.Spectrographic determination removes polyphenol impurity 85%.

Claims (1)

1. a Gummi Elaeagni Angustifoliae is made with extra care the method for decolouring, it is characterized in that Gummi Elaeagni Angustifoliae after water dissolution, filtration, through vacuum concentration, form weight concentration 20%-40% Gummi Elaeagni Angustifoliae solution, under agitation add ethanol gradually, Gummi Elaeagni Angustifoliae solution and alcoholic acid volume ratio are 0.7-1: 1 o'clock, with a branch of red laser monitoring polysaccharide water/ethanol colloidal sol, when the laser light beam becomes taper by Strahlungseintritt, when laser light beam coning angle is spent 90 ° of ∠, stop to add ethanol, this colloidal sol was placed 20-30 hour; Join gradually in the ethanol this colloidal sol is under agitation anti-phase, form the particulate deposits of oleaster gum polyose, water and volumes of aqueous ethanol are than being 0.1-0.2: 1, with sedimentation and filtration, with the ethanol washing and precipitating, obtain white oleaster gum polyose fine powder, vacuum-drying must be made with extra care Gummi Elaeagni Angustifoliae.
CN 02117954 2002-05-27 2002-05-27 Process for decolouring and refining oleaster gum polyose Expired - Fee Related CN1243024C (en)

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Application Number Priority Date Filing Date Title
CN 02117954 CN1243024C (en) 2002-05-27 2002-05-27 Process for decolouring and refining oleaster gum polyose

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Application Number Priority Date Filing Date Title
CN 02117954 CN1243024C (en) 2002-05-27 2002-05-27 Process for decolouring and refining oleaster gum polyose

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CN1386764A true CN1386764A (en) 2002-12-25
CN1243024C CN1243024C (en) 2006-02-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105622773A (en) * 2016-02-22 2016-06-01 中国科学院新疆理化技术研究所 Method for preparing elaeagnus angustifolia gum polysaccharide

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105622773A (en) * 2016-02-22 2016-06-01 中国科学院新疆理化技术研究所 Method for preparing elaeagnus angustifolia gum polysaccharide
CN105622773B (en) * 2016-02-22 2017-08-22 中国科学院新疆理化技术研究所 A kind of preparation method of oleaster gum polyose

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