CN102153679B - Method for grading inulin - Google Patents

Method for grading inulin Download PDF

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Publication number
CN102153679B
CN102153679B CN2011100376834A CN201110037683A CN102153679B CN 102153679 B CN102153679 B CN 102153679B CN 2011100376834 A CN2011100376834 A CN 2011100376834A CN 201110037683 A CN201110037683 A CN 201110037683A CN 102153679 B CN102153679 B CN 102153679B
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supernatant
inulin
alcohol
deposit
polymerization degree
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CN102153679A (en
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芦明春
郑晓丽
邹东旭
王应妮
韩璐
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Dalian Polytechnic University
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Dalian Polytechnic University
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Abstract

The invention relates to a method for grading inulin, comprising the following steps: (1) adding alcohol to the inulin to form alcohol solution of the inulin, wherein the concentration of the alcohol in the alcohol solution is 5-95% (V/V), processing the alcohol solution of the inulin with ultrasonic waves at 10-50 DEG C, and centrifuging to obtain a supernatant Y1 and a precipitate D1; (2) continuously adding alcohol to the supernatant Y1 and the precipitate D1, processing and centrifuging the supernatant Y1 and the precipitate D1 like the operation in the step (1), processing the supernatant Y1 to obtain a supernatant Y2 and a precipitate D2, and processing the precipitate D1 to obtain a supernatant Y3 and a precipitate D3; and (3) repeating the operation in sequence to finally obtain a supernatant and a precipitate by grading in each step, and drying the supernatant and the precipitate obtained by grading in each step to obtain the product which is the inulin with a certain range of polymerization degree or specific polymerization degree. The invention has the advantages of high grading efficiency, short time, low power consumption and the like. The produced product which is the inulin with a certain range of polymerization degree has good application values.

Description

A kind of stage division of inulin
Technical field
The invention belongs to the separation method field of natural phant powder, relate to solvent and carry out ultrasonic separation, fractionated technology.
Background technology
The inulin general molecular formula is GFn, is to be linked through β-2,1 glycosidic link and the terminal polysaccharide that is connected with the glucose saccharide residue by a plurality of fructose residual sugar base Fn, and the polymerization degree is generally 2~60, and mean polymerisation degree is 10.Inulin has many-sided physiological function as a kind of functional Polylevulosan, and it is the somatomedin of bifidus bacillus, also can be used as the protective foods batching and the medicine of anti-curing oncoma, coronary heart disease, colorectal carcinoma, constipation etc.Inulin also has the technic character that is fit to processing, is widely used in fields such as food, medicine, chemical industry.
According to the different inulin that form different chain length of the polymerization degree of Polylevulosan, the inulin that the polymerization degree is different there are differences on functional and manufacturability.As: the inulin of high-polymerization degree has excellent viscometric properties and high gel-strength than the low polymerization degree inulin; And the low polymerization degree inulin has stronger beneficial natural disposition matter, and the high-polymerization degree inulin then is more suitable for as pharmaceutical carrier and treatment distal colorectal intestinal disease.Mostly the application of inulin at present is its blending ingredients; Be difficult to the technology or the functional effect that reach required to a certain extent; With inulin refinement classification, produce the inulin product that has certain polymerization degree scope or have the specific aggregation degree, have great importance for the selectivity application that realizes inulin.Publication number is the method that the direct film of the Chinese patent of CN1389468A is produced inulin, oligofructose; This method production process cleaning; Non-pollutant discharge, the product purity that obtains is high, and production process is easy to control; But the polymerization degree range spans of the inulin that this method makes is big, is difficult to obtain the narrower inulin product of distribution of polymerization degree.Publication number is the extraction process of a kind of inulin of Chinese patent of CN1634997A; A kind of technology of producing the inulin of different polymerization degree scope is provided; The inulin product of producing is various, but the distribution of polymerization degree of the inulin that stage division wherein makes is also than broad, and length consuming time; Energy consumption is big, is difficult to realize suitability for industrialized production.
Summary of the invention
The present invention is directed to above-mentioned inulin current situation of classification, adopt ultrasonic supplementary classification technology, produce the inulin product that has certain polymerization degree scope or have the specific aggregation degree, using for the selectivity that realizes inulin provides a kind of feasible effective means.
Technical scheme of the present invention is following: utilize organic solvent that different polymerization degree raw material inulin is had different solubilities; Through UW supplementary classification processing carrying out polymerization degree classification; Then, make the inulin product that has certain polymerization degree scope or have the specific aggregation degree respectively respectively through centrifugal and dry.
Described classification, it is to adopt pure classification, used alcohol is methyl alcohol or ethanol.
Described raw material inulin is the inulin of burdock, witloof, jerusalem artichoke plant origin.Described UW supplementary classification is handled, its be stage solution in 10~50 ℃, under ultrasonic frequency 21~50kHz, ultrasonic 10~30min.Described centrifugal, it is in 2000~10000rmp/min, centrifugal 5~20min.Described drying, it is that liquid adopts spraying drying to dust, deposition adopts high levels of organic solvents washing back negative pressure drying powder process.
Operation steps of the present invention is:
(1) adds alcohol in the inulin, form the alcoholic solution of inulin, make in the solution determining alcohol be 5~95% (V/V, down with), use ultrasonication in 10~50 ℃,, obtain supernatant Y through centrifugal 1And deposit D 1
(2) supernatant Y 1And deposit D 1Proceed respectively to add alcohol, supersound process and centrifugal treating like step (1), supernatant Y 1The treated supernatant Y that obtains 2And deposit D 2Deposit D 1The treated supernatant Y that obtains 3And deposit D 3
Wherein: supernatant Y 1Adding in the solution of alcohol back the determining alcohol value exceeds than (1) step determining alcohol value and is no less than 5%, deposit D 1Determining alcohol value behind the adding alcohol is hanged down than determining alcohol value described in (1) step and to be no less than 5%;
(3) repetitive operation successively, finally each classification all obtains supernatant and deposition;
Supernatant after each stage treatment and/or deposition are through the dry inulin product that has certain polymerization degree scope or have the specific aggregation degree that makes;
The invention has the advantages that: the inventive method adopts the auxiliary organic solvent classification technique of UW without any chemistry or biological action, produces the inulin product that has certain polymerization degree scope or have the specific aggregation degree.The present invention is applied to the inulin classification with ultrasonic technology; Has the fractional efficiency height; Weak point consuming time; The advantage of less energy-consumption etc., the inulin product with certain polymerization degree scope of production has good application: the polymerization degree has better oligofructose performance at the product below 10, is particularly suitable for being applied in functional food and the protective foods as prebiotics; The polymerization degree is suitable for as fat-replacer then having better processability ability and food fibre performance more than 10, the medicine of treatment such as intestinal tract disease and constipation; The polymerization degree can be used as segmented intestine targeted location pharmaceutical carrier at the product more than 25; The product of producing with specific aggregation degree is expected to use as a kind of inulin standard substance.The inventive method can also have vital role for the selective use of realization polysaccharide, the using value of raising polysaccharide as a kind of polysaccharide Retreatment method simultaneously.
Embodiment
Embodiment 1
Dry jerusalem artichoke inulin 2.0kg, adding 10.0L concentration is 5% ethanolic soln, and in 10 ℃, ultrasonic 20min under the 50kHz, solution are in 4000rpm/min, and centrifugal 10min obtains supernatant Y and deposit D; Spraying drying made dry powder F after supernatant Y was concentrated into 40% concentration 1, deposit D is through absolute ethanol washing, and in 40 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 2The inulin product F that this instance makes 1, F 2The polymerization degree is respectively: 1~41 and 42~44.
Embodiment 2
Dry jerusalem artichoke inulin 2.0kg, adding 10.0L concentration is 50% ethanolic soln, and in 20 ℃, ultrasonic 15min under the 50kHz, solution are in 4000rpm/min, and centrifugal 10min obtains supernatant Y and deposit D; Spraying drying made dry powder F after supernatant Y was concentrated into 40% concentration 1, deposit D is through absolute ethanol washing, and in 40 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 2The inulin product F that this instance makes 1, F 2The polymerization degree is respectively: 1~24 and 25~44.
Embodiment 3
Dry jerusalem artichoke inulin 2.0kg, adding 6.0L concentration is 95% ethanolic soln, and in 30 ℃, ultrasonic 15min under the 45kHz, solution are in 8000rpm/min, and centrifugal 5min obtains supernatant Y and deposit D; Supernatant Y is concentrated into the spray-dried dry powder F that makes after 40% concentration 1, deposit D is through absolute ethanol washing, and in 50 ℃, vacuum tightness makes dry powder F for the 0.09MPa drying 2The inulin product F that this instance makes 1, F 2The polymerization degree is respectively: 1~2 and 3~44.
Embodiment 4
Dry witloof inulin 2.0kg, adding 10.0L concentration is 10% ethanolic soln, and in 40 ℃, ultrasonic 20min under the 30kHz, solution are in 2000rpm/min, and centrifugal 20min obtains supernatant Y 1And deposit D 1Supernatant Y 1Continue to add alcohol and reach that determining alcohol is 15% in the solution, deposit D 1Adding concentration by solid-to-liquid ratio 1: 5 is 5% ethanolic soln, all repeats ultrasound procedure.Supernatant Y 1The treated supernatant Y that obtains 2And deposit D 2, deposit D 1The treated supernatant Y that obtains 3And deposit D 3Supernatant Y 2, Y 3Spraying drying makes dry powder F after being concentrated into 40% concentration respectively 1, F 3, deposit D 2, D 3Through absolute ethanol washing, in 40 ℃, vacuum tightness makes dry powder F for the 0.09MPa drying 2, F 4The inulin product F that this instance makes 1, F 2, F 3, F 4The polymerization degree is respectively: 1~35,36~39,40~42 and 43~56.
Embodiment 5
Dry jerusalem artichoke inulin 2.0kg, adding 8.0L concentration is 90% ethanolic soln, and in 30 ℃, ultrasonic 10min under the 45kHz, solution are in 10000rpm/min, and centrifugal 5min obtains supernatant Y 1And deposit D 1Supernatant Y 1Continue to add alcohol and reach that determining alcohol is 95% in the solution, deposit D 1Adding concentration by solid-to-liquid ratio 1: 4 is 85% ethanolic soln, all repeats ultrasound procedure.Supernatant Y 1The treated supernatant Y that obtains 2And deposit D 2, deposit D 1The treated supernatant Y that obtains 3And deposit D 3Supernatant Y 2, Y 3Spraying drying makes dry powder F after being concentrated into 40% concentration respectively 1, F 3, deposit D 2, D 3Through absolute ethanol washing, in 40 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 2, F 4The inulin product F that this instance makes 1, F 2, F 3, F 4The polymerization degree is respectively: 1~2,3,4~10 and 11~44.
Embodiment 6
Dry burdock inulin 2.0kg, adding 10.0L concentration is 50% ethanolic soln, and in 40 ℃, ultrasonic 30min under the 21kHz, solution are in 8000rpm/min, and centrifugal 5min obtains supernatant Y 1And deposit D 1Supernatant Y 1Continue to add alcohol and reach that determining alcohol is 80% in the solution, deposit D 1Adding concentration by solid-to-liquid ratio 1: 6 is 30% ethanolic soln, all repeats ultrasound procedure.Supernatant Y 1The treated supernatant Y that obtains 2And deposit D 2, deposit D 1The treated supernatant Y that obtains 3And deposit D 3Supernatant Y 2, Y 3Spraying drying makes dry powder F after being concentrated into 40% concentration respectively 1, F 3, deposit D 2, D 3Through washing with acetone, in 50 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 2, F 4The inulin product F that this instance makes 1, F 2, F 3, F 4The polymerization degree is respectively: 1~12,13~25,26~32 and 33~41.
Embodiment 7
Dry burdock inulin 2.0kg, adding 8.0L concentration is 5% methanol solution, and in 50 ℃, ultrasonic 15min under the 25kHz, solution are in 3000rpm/min, and centrifugal 15min obtains supernatant Y 1And deposit D 1Supernatant Y 1Continue to add methyl alcohol and reach that determining alcohol is 50% in the solution, repeat ultrasound procedure, obtain supernatant Y 2And deposit D 2Supernatant Y 2Be concentrated into the spray-dried dry powder F that makes after 40% concentration 1, deposit D 1, D 2Through washing with acetone, in 40 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 3, F 2The inulin product F that this instance makes 1, F 2, F 3The polymerization degree is respectively: 1~26,27~38,39~41.
Embodiment 8
Dry burdock inulin 2.0kg, adding 10.0L concentration is 70% methanol solution, and in 40 ℃, ultrasonic 20min under the 30kHz, solution are in 4000rmp/min, and centrifugal 10min obtains supernatant Y 1And deposit D 1Deposit D 1Add 5% ethanolic soln, repeat ultrasound procedure, obtain supernatant Y 2And deposit D 2Supernatant Y 1Be concentrated into the spray-dried dry powder F that makes after 40% concentration 1Supernatant Y 2Be concentrated into the spray-dried dry powder F that makes after 40% concentration 2Deposit D 2Through absolute ethanol washing, in 50 ℃, vacuum tightness is that drying makes dry powder F under the 0.09MPa 3The inulin product F that this instance makes 1, F 2, F 3The polymerization degree be respectively: 1~16,12~37,38~41.

Claims (1)

1. the stage division of an inulin is characterized in that with organic solvent to the classification of the raw material inulin polymerization degree, its operation steps is:
(1) adds alcohol in the inulin, form the alcoholic solution of inulin, make that determining alcohol is 5~95%V/V in the solution, use ultrasonication,, obtain supernatant Y through centrifugal 1And deposit D 1
(2) supernatant Y 1And deposit D 1Proceed respectively to add alcohol, ultrasonication and centrifugal treating like step (1), supernatant Y 1The treated supernatant Y that obtains 2And deposit D 2Deposit D 1The treated supernatant Y that obtains 3And deposit D 3
Wherein: supernatant Y 1Adding in the solution of alcohol back the determining alcohol value exceeds than (1) step determining alcohol value and is no less than 5%, deposit D 1Determining alcohol value behind the adding alcohol is hanged down than determining alcohol value described in (1) step and to be no less than 5%;
(3) repetitive operation successively, finally each classification all obtains supernatant and deposition;
Supernatant after each stage treatment adopts spraying drying to dust, and it is 1~24 and 25~44 jerusalem artichoke inulin product that deposition makes polymerization degree scope through the absolute ethyl alcohol drying, and polymerization degree scope is 1~35,36~39,40~42 and 43~56 witloof inulin product; Supernatant after each stage treatment adopts spraying drying to dust, and it is 1~12,13~25 that deposition makes polymerization degree scope through acetone drying, 26~32,33~41 burdock inulin product;
Above-mentioned in steps in: used alcohol is ethanol, and said determining alcohol is: V/V; Described ultrasonication is: 10~50 ℃, under ultrasonic frequency 21~50kHz, handle 10~30min; Said spinning is: 2000-10000rpm, centrifugal 5~20min.
CN2011100376834A 2011-02-14 2011-02-14 Method for grading inulin Expired - Fee Related CN102153679B (en)

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Publication number Priority date Publication date Assignee Title
US6399142B1 (en) * 1998-08-27 2002-06-04 Barnard Stewart Silver Liquid food products
CN1285615C (en) * 2004-12-02 2006-11-22 西北农林科技大学 Inulin extraction process
CN101432314B (en) * 2006-04-28 2011-10-12 拜尔作物科学股份公司 Inulin of very high chain length

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