CN106674367A - Method for purifying and preparing isomalto-oligosaccharide and application - Google Patents

Method for purifying and preparing isomalto-oligosaccharide and application Download PDF

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Publication number
CN106674367A
CN106674367A CN201611182342.5A CN201611182342A CN106674367A CN 106674367 A CN106674367 A CN 106674367A CN 201611182342 A CN201611182342 A CN 201611182342A CN 106674367 A CN106674367 A CN 106674367A
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China
Prior art keywords
molecular weight
average molecular
ethanol
oligomeric isomaltose
oligosaccharide
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CN201611182342.5A
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Chinese (zh)
Inventor
王相玉
刘兆贵
曹红光
仰振球
吕慧忠
由守谊
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YANTAI DONGCHENG PHARMACEUTICAL GROUP Co Ltd
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YANTAI DONGCHENG PHARMACEUTICAL GROUP Co Ltd
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Priority to CN201611182342.5A priority Critical patent/CN106674367A/en
Publication of CN106674367A publication Critical patent/CN106674367A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H3/00Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
    • C07H3/06Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Biotechnology (AREA)
  • Genetics & Genomics (AREA)
  • Sustainable Development (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention relates to a method for purifying and preparing isomalto-oligosaccharide and an application. The isomalto-oligosaccharide, with the weight-average molecular weight from 800-3000Da and the number-average molecular weight from 600-2800Da, preferably, the weight-average molecular weight from 1000-2000Da and the number-average molecular weight from 800-2000Da, is appointed as the product; and the monosaccharide can be effectively removed (to below an appointed value). The method specifically comprises the following steps: adopting a repeated alcohol precipitation grading method for centrifuging a hydrolyzed solution containing an isomalto-oligosaccharide mixed component, and then drying, thereby acquiring an isomalto-oligosaccharide solid with the appointed molecular weight. The isomalto-oligosaccharide purified and prepared according to the invention is widely applied to the fields of food additives, medicinal chemical engineering, and the like.

Description

A kind of purification prepares the method for oligomeric isomaltose and application
Technical field
The present invention relates to food, medicine field, a kind of purification prepares the method for oligomeric isomaltose and application, and which is average Molecular weight within the specified range, and can effectively remove monosaccharide.Specifically by after hydrolysis containing oligomeric isomaltose blending ingredients Solution, the method being classified by multiple precipitate with ethanol, centrifugation are dried, obtain mean molecule quantity oligomeric Isomalt within the specified range Sugared solid.Oligomeric isomaltose according to the present invention is in food additive (glucose/fructose/sucrose succedaneum etc.), medicineization It is widely used in the fields such as work (preparing injection stage iron supplementary).
Background technology
Oligomeric isomaltose has powerful proliferation function to bacillus bifiduss beneficial in human body, purifies intestinal, promotes intestinal compacted It is dynamic, prevent and constipation relieving and diarrhoea, suppress the breeding of internal harmful bacteria and the generation of poisonous corrupt substance etc..It is oligomeric different in addition Maltose plays more and more extensive effect in medication chemistry, such as prepares iron supplementary etc..
The method for preparing oligomeric isomaltose at present is mainly degraded by acid system, and enzymic degradation etc., technics comparing are ripe.It is pure Chemical industry skill then by the methods such as membrane filter method, (glucosan) gel column method, zwitterion post method or several method use cooperatively into Row purification.
There are patent report (WO948533) in foreign countries by certain films purification, can obtain mean molecule quantity within the specified range Qualifying object product.But the specificity of various filter membranes is limited to, at present the filtration membrane matrix of each manufacturer production, model be not also Can be unified, dragons and fishes jumbled together for properties of product, irregular to differ.Through the multiple trial of our early stage, also fail to obtain by the method Up-to-standard product.
At home and abroad producer is applied for gel column method, zwitterion post method, but defect is gel, zwitterion resin Service life is limited, and process time is long, per resin disposal ability limited (solution concentration is low), in addition spray drying method energy consumption It is very high.
The method that current exploitation alcohol deposition method prepares oligomeric isomaltose is also little.In the method reported, precipitate with ethanol is only made A wherein step in for purifying process can not effectively remove monosaccharide and directly obtain finger removing inorganic salt and other impurities Determine the oligosaccharide of molecular weight ranges.
Such as, it is related to a kind of oligosaccharide method for preparing purified in CN105949335A, is after polysaccharide solution precipitate with ethanol, by (Portugal Polysaccharide) gel column method purification obtains target oligosaccharide.
Oligose preparing process disclosed in CN103172759A is after precipitate with ethanol to obtain target product by membrane filtration.
Said method prepares target product by precipitate with ethanol and other purification process, and its complex steps is relatively costly, no Beneficial to amplification production operation.
Solution containing oligomeric isomaltose blending ingredients, the method being classified by multiple precipitate with ethanol are centrifuged, directly by the present invention Connect and remove inorganic salt, enzyme and monosaccharide, be centrifuged, be dried, mean molecule quantity oligomeric isomaltose within the specified range can be obtained Solid.
The alcohol precipitating method of the present invention is with respect to said method, the effective control monosaccharide in the oligomeric isomaltose for preparing, ethanol Can have the advantages that timeliness height, the three wastes are few, and mean molecule quantity medicine within the specified range can be obtained with effective recycling Injection stage oligomeric isomaltose solid.
The content of the invention
For the deficiencies in the prior art, the present invention relates to a kind of purification prepares the oligomeric isomaltose solid for specifying molecular weight Method, the solution containing oligomeric isomaltose blending ingredients after acid system or enzymatic hydrolysises is added into purified water specifically, is configured to Certain density solution, in the ethanol of Deca respective amount, alcohol analysis, stands centrifugation, and incline supernatant, obtains solid.Again through many Secondary alcohol deposition method, removes inorganic salt, enzyme and monosaccharide, centrifugation, is dried, and finally gives mean molecule quantity within the specified range oligomeric Dextrinose solid.
Mean molecule quantity according to the present invention oligomeric isomaltose within the specified range is mainly used in food additive, doctor The fields such as medicine chemical industry, such as glucose/fructose/sucrose succedaneum, prepare the multiple uses such as iron supplementary.For example, using this Bright oligomeric isomaltose and iron containing compoundses carry out complexation, can effectively produce the injection stage iron supplementary of specified molecular weight.
Experiment shows:Can effectively replace membrane filter method of the present invention, (glucosan) gel column method, zwitterion post method prepare life Oligomeric isomaltose is produced, on the premise of quality is guaranteed, reduces cost is more suitable for industrialized production.
Specific embodiment
Embodiment 1
Precipitate with ethanol classification
To contain in the four-hole bottle of solution input 10L of oligomeric isomaltose blending ingredients 10g (inventory), mend in solution Fill purified water to make sugar juice concentration is 2%, and Deca 4.5L ethanol carries out alcohol analysis under agitation, stands after completion of dropwise addition, and centrifugation is inclined Supernatant is removed, solid is obtained, the 2.73g that weighs is dried, contents of monosaccharides is 11.3%, and yield is 27.3%, and weight average molecular weight is 786, number-average molecular weight is 552.
Secondary precipitate with ethanol classification
By solid dissolving obtained by a precipitate with ethanol in 250mL purified water, and Deca 2.3L ethanol carries out alcohol analysis under agitation, Stand after completion of dropwise addition, centrifugation, incline supernatant, obtain solid, dry the 1.65g that weighs, contents of monosaccharides is 0.34%, and yield is 16.5%, weight average molecular weight is 1551, and number-average molecular weight is 1396.
Three precipitate with ethanol classifications
By solid dissolving obtained by secondary precipitate with ethanol in 130mL purified water, and Deca 1.20L ethanol carries out alcohol under agitation Analysis, stands after completion of dropwise addition, centrifugation, and incline supernatant, and the drying of gained solid is weighed as 0.94g, and contents of monosaccharides is 0.02%, receives Rate is 9.4%, and weight average molecular weight is 2096, and number-average molecular weight is 1812.
Embodiment 2- embodiment 8 using as above processing step, (is thrown using the 10g of blending ingredients containing oligomeric isomaltose Doses) solution carry out precipitate with ethanol classification, the sugar juice concentration only prepared is different with amount of alcohol parameter values, and yield, list Sugared content, average molecular weight value are different, therefore are presented with list mode.
Note:Embodiment 8 is operated according to patent CN105949335A
Through experimental verification, the present invention directly by hydrolysis after sugared mixed salt solution pass through multiple precipitate with ethanol grading purification, can To obtain specifying weight average molecular weight in 800~3000Da, number-average molecular weight is in 600~2800Da, wherein preferably Weight-average molecular 1000~2000Da of amount, oligomeric isomaltose of the number-average molecular weight in 800~2000Da, and it is (extremely specified effectively to remove monosaccharide Under numerical value).

Claims (11)

1. a kind of method for preparing oligomeric isomaltose for purification, its mean molecule quantity within the specified range, and effectively can be gone Except monosaccharide.Specifically by the solution containing oligomeric isomaltose blending ingredients after hydrolysis, the method being classified by multiple precipitate with ethanol, from The heart, is dried, obtains mean molecule quantity oligomeric isomaltose solid within the specified range.
2. advantage of the invention is that being capable of selective removal monosaccharide, that is to say, that while ensureing to reach mean molecule quantity, Contents of monosaccharides can be reduced to below specified content.
3. method according to claim 1, wherein oligomeric isomaltose blending ingredients are referred to containing monosaccharide (glucose, fruit Sugar etc.), disaccharide ((different) maltose etc.), trisaccharide etc. is until the mixture of 18 oligosaccharide, wherein contents of monosaccharides are 25%~35%.
4. method according to claim 2, the specified content of wherein monosaccharide refer to 1%.
5. method according to claim 1, wherein solution are referred to and may contain the salt such as sodium sulfate, Sodium Chloride, sodium nitrate Aqueous solution.
6. method according to claim 1, wherein the ethanol for adding is the ethanol that water content is 93.0-99.5%.
7. method according to claim 1, wherein repeatedly referring to 2-4 time.
8. the classification of method according to claim 1, wherein precipitate with ethanol is referred to containing the molten of oligomeric isomaltose blending ingredients In liquid, suitable quantity of water is added, add enough ethanol, stand centrifugation, be dried, the method for obtaining solid.
9. method according to claim 1, the specified molecular weight ranges of wherein oligomeric isomaltose refer to weight average molecular weight (800-3000) Da, number-average molecular weight (600-2800).1000~2000Da of weight average molecular weight, number-average molecular weight are preferably wherein (800-2000) the specified numerical value in the range of Da.
10. 2~100 times for oligomeric isomaltose quality of method according to claim 8, the wherein volume of water.
11. methods according to claim 8, wherein enough ethanol is 8: 1 to 10 with the volume ratio of suitable quantity of water: 1.
CN201611182342.5A 2016-12-14 2016-12-14 Method for purifying and preparing isomalto-oligosaccharide and application Pending CN106674367A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215338A (en) * 2007-01-05 2008-07-09 庄茅 Iron isomaltum oligosaccharide and preparing method thereof
CN101215337A (en) * 2007-01-05 2008-07-09 庄茅 Method for preparing copper isomaltum oligosaccharide
CN105949335A (en) * 2015-12-31 2016-09-21 牡丹江友搏药业股份有限公司 Oligosaccharide components with anti-platelet aggregation activity, and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215338A (en) * 2007-01-05 2008-07-09 庄茅 Iron isomaltum oligosaccharide and preparing method thereof
CN101215337A (en) * 2007-01-05 2008-07-09 庄茅 Method for preparing copper isomaltum oligosaccharide
CN105949335A (en) * 2015-12-31 2016-09-21 牡丹江友搏药业股份有限公司 Oligosaccharide components with anti-platelet aggregation activity, and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张举贤等: "《高分子科学实验(第1版)》", 28 February 1997, 河南大学出版社 *
金学浩: "《兽用中草药剂的制备与剂型改革(第1版)》", 31 March 1983, 福建科学技术出版社 *

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Application publication date: 20170517