CN102219808A - Method for extracting fructooligosaccharides from yacon - Google Patents
Method for extracting fructooligosaccharides from yacon Download PDFInfo
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- CN102219808A CN102219808A CN2011100984721A CN201110098472A CN102219808A CN 102219808 A CN102219808 A CN 102219808A CN 2011100984721 A CN2011100984721 A CN 2011100984721A CN 201110098472 A CN201110098472 A CN 201110098472A CN 102219808 A CN102219808 A CN 102219808A
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Abstract
The invention which relates to the oligosaccharide extraction field concretely relates to a method for extracting fructooligosaccharides from yacon. The method comprises the following steps: 1, peeling and cutting yacon, immersing in a leaching agent solution with a concentration of 1 to 3 wt% and a mass-volume ratio of yacon to the leaching agent solution of 50 to 300 g/L, and leaching at a constant temperature; (2) carrying out solid-liquid separation on a leachate, filtering out large-size solid residues, and removing short grained suspended substances through further centrifugation processing to obtain the leachate; and 3, adding a polar organic solvent mutually soluble with water to the leachate, oscillating to mix, standing for phase separation at a temperature of 0 to 10 DEG C, taking out an organic layer, and removing the polar organic solvent to obtain fructooligosaccharides. The method has the advantages that the cost is low, the technology is simple and easy to operate, the production period of products is short, and the purity of fructooligosaccharides is high.
Description
Technical field
The present invention relates to oligose and extract the field, particularly, the present invention relates to a kind of method that from yacon, extracts oligofructose.
Background technology
Contain multiple human body essential amino acid and abundant mineral substance in the yacon, particularly glucide content reaches more than 90% in its fruit butt, mainly form by oligosaccharides such as oligofructose, sucrose, fructose, glucose and monose material, not starch-containing, wherein oligofructose is main functional oligose class material, and its content accounts for 45%～65% of its fruit butt.
Oligofructose is a kind of ideal functional additive, has extensive use, it is a kind of good water-soluble dietary fibre mainly as human beings'health food, has characteristics such as the enteric microorganism of adjusting colony balance, preventing constipation, promotion mineral substance absorb, anti-ageing, prevention of dental caries; Can improve body immunity, take the effect that can play fat-reducing for a long time.In addition, oligofructose can also part substitute microbiotic, is a kind of " green " fodder additives, and its application prospect is boundless.
From the yacon vat liquor, extract oligofructose, need remove the interference of impurity such as sucrose, fructose, glucose.The key step of purification oligofructose comprises from yacon at present: lixiviate, and--decolouring--deproteinated--nanofiltration separation obtains the oligofructose product, this technology exists cost height, technology very complicated, the oligofructose product purity is lower, is doped with problems such as glucose, fructose.
In recent years, some are emerging, separating and purifying technology develops rapidly efficiently, have been used to separate from various natural products the purification useful component.Comparatively typically comprise two big classes: 1) under the situation that strong electrolyte salt (as oxymuriate, nitrate or the vitriol of basic metal or alkaline-earth metal) exists, come together and added a kind of polar organic solvent in the aqueous solution of thing to containing target, the control certain condition, the polar organic solvent aqueous solution that causes homogeneous originally to dissolve each other splits into two immiscible liquid phases, and the thing that come together of the target in the initial aqueous solution can produce the selective difference distribution along with the two-phase division in two-phase; 2) under the situation that strong electrolyte salt exists, come together and added a kind of high molecular weight water soluble polymer in the aqueous solution of thing to containing target, the control certain condition, the aqueous solutions of polymers that causes homogeneous originally to dissolve each other splits into two immiscible liquid phases.This two-phase system is also referred to as aqueous two-phase extraction because of two-phase water-content height, and is effective especially for the extracting and separating natural active matter; But, because the formation of above-mentioned two kinds of extraction systems all needs to add the salt of higher concentration, tend to cause taking place some unpredictable side reactions in the extraction process in the high salt concentration medium, the final form of extraction product is restive, even can destroy product activity to be separated.In addition, high salt concn also is a difficult problem to the corrosion of extraction equipment, and needs the higher macromolecular water-soluble polymkeric substance of use cost in the polymkeric substance double-aqueous phase system, and polymkeric substance how economical and effective reclaims and recycling utilization is still waiting solution.
Summary of the invention
The objective of the invention is in order to overcome the problems referred to above, a kind of method that extracts oligofructose from yacon is provided.
According to the method that from yacon, extracts oligofructose provided by the invention, said method comprising the steps of:
1) with the yacon peeling, stripping and slicing, being immersed in concentration is in the leaching agent solution of 1wt%～3wt%, wherein the mass volume ratio of yacon and leaching agent solution is 50g/L～300g/L, carries out lixiviate under the constant temperature;
2) with the vat liquor solid-liquid separation, filter out the macrobead solid residue, centrifugal treating further removes small granular suspended matters then, obtains leach liquor;
3) add the polar organic solvent that dissolves each other with water in leach liquor, vibration mixes, and leaves standstill phase-splitting under 0～10 ℃, gets the solution of organic layer, removes polar organic solvent, obtains oligofructose.
According to the method that extracts oligofructose from yacon of the present invention, the leaching agent in the described step 1) comprises xitix.
According to the method that extracts oligofructose from yacon of the present invention, described step 3) Semi-polarity organic solvent is selected from acetonitrile, acetone, tetrahydrofuran (THF), 1-propyl alcohol and/or 2-propyl alcohol, is preferably acetonitrile.
According to of the present invention from yacon the method for extraction oligofructose, the concentration of the described ascorbic acid solution of step 1) is 1%wt～3%wt, and is preferred 2%～2.5%, extraction temperature is 40 ℃～70 ℃, is preferably 50 ℃～60 ℃, extraction time 2～3 hours.
According to the method that from yacon, extracts oligofructose of the present invention, the organic solvent that adds in the step 3) (pure acetonitrile) volume and step 2) volume ratio of the vat liquor supernatant liquor that obtains is 2: 3～7: 3, the temperature that leaves standstill phase-splitting is 0 ℃～10 ℃, the time of leaving standstill phase-splitting is 6～12 hours, wherein, preferred 1: 1～2: 1 of the volume ratio of acetonitrile and vat liquor leaves standstill preferred 0 ℃～4 ℃ of the temperature of phase-splitting, leaves standstill preferred 8～10 hours of the time of phase-splitting.
According to the method that from yacon, extracts oligofructose of the present invention, the method that removes polar organic solvent in the step 3) is a distillation under vacuum, in still-process, allow the system environmental stress remain on below the normal atmosphere, distillation temperature is 30 ℃～60 ℃, the environmental stress of preferred distillation under vacuum is 0MPa～0.05MPa, and distillation temperature is 40 ℃～50 ℃.
One embodiment of the invention, what method of the present invention was concrete may further comprise the steps:
(1) with the yacon peeling of certain mass, stripping and slicing is immersed in the certain density ascorbic acid solution constant temperature water bath lixiviate at a certain temperature;
(2) the vat liquor solid-liquid separation filters out the macrobead solid residue, and centrifugal treating further removes small granular suspended matters then, collects centrifugal back supernatant liquor;
(3) get the centrifugal back of certain volume supernatant liquor, add the pure acetonitrile of certain volume, vibration mixes, and controls suitable temperature and makes mixture leave standstill phase-splitting;
(4) after the mixture phase-splitting, get and carry out underpressure distillation mutually, obtain highly purified oligofructose product to remove lower boiling acetonitrile solvent.
A kind of method that from yacon, extracts oligofructose of the present invention, utilize the monosaccharide concentration in the yacon vat liquor higher, phase-splitting can take place in the supernatant liquor after vat liquor is centrifugal and the mixing solutions of acetonitrile at low temperatures, complete when phase-splitting, reach balance after, most oligofructose all is enriched in phase, glucose is enriched in down mutually with carbohydrates such as fructose, contain oligofructose on pass through underpressure distillation mutually, can obtain highly purified oligofructose, acetonitrile can realize the recycling.
Of the present invention a kind of from yacon the extraction oligofructose method in, phase-splitting can take place in not all organic solvent, therefore to being applicable to that polar organic solvent of the present invention screens, preferred acetonitrile among the present invention, and in the process of extracting oligose, need yacon is carried out lixiviate, make the concentration of oligose wherein reach certain concentration, just can make after adding organic solvent effective, phase-splitting fast, therefore among the present invention with the ascorbic acid solution of 1wt%～3wt% as infusion solution, the mass volume ratio of yacon and leach liquor is 50g/L～300g/L in the strict control solution, and strict controlled temperature is 0～10 ℃, thereby realized phase-splitting fast, obtain the higher oligose of purity, organic solution also realizes recycling simultaneously.
The invention has the advantages that and effectively avoided existing cost height, the technology very complicated that the oligofructose method exists that from the yacon vat liquor, extract, problem such as life cycle of the product is long, and oligofructose purity is low.
Description of drawings
Fig. 1 is the method flow diagram of extraction oligofructose from yacon.
Embodiment
Embodiment 1
With the yacon peeling of certain mass, stripping and slicing is got 80g and is immersed in 2wt%, and in the ascorbic acid solution of 400mL, wherein the mass volume ratio of yacon and leaching agent solution is 200g/L, and 60 ℃ of following constant temperature water bath lixiviates, extraction time is 2 hours; The vat liquor solid-liquid separation filters out the macrobead solid residue, and centrifugal treating further removes small granular suspended matters then, collects centrifugal back supernatant liquor; The centrifugal back of every 4mL supernatant liquor adds the pure acetonitrile of 6mL, and vibration mixes, and makes mixture leave standstill phase-splitting 8 hours under 1 ℃; After the mixture phase-splitting, get and carry out underpressure distillation mutually to remove lower boiling acetonitrile solvent, obtain 0.195g oligofructose product, separating its purity of check through liquid chromatography is 96.7%.
Embodiment 2
With the yacon peeling of certain mass, stripping and slicing is got 86g and is immersed in 2.5wt%, and in the ascorbic acid solution of 400mL, wherein the mass volume ratio of yacon and leaching agent solution is 215g/L, and 60 ℃ of following constant temperature water bath lixiviates, extraction time is 3 hours; The vat liquor solid-liquid separation filters out the macrobead solid residue, and centrifugal treating further removes small granular suspended matters then, collects centrifugal back supernatant liquor; The centrifugal back of every 5mL supernatant liquor adds the pure acetonitrile of 5mL, and vibration mixes, and makes mixture leave standstill phase-splitting 10 hours under 4 ℃; After the mixture phase-splitting, get and carry out underpressure distillation mutually to remove lower boiling acetonitrile solvent, obtain 0.174g oligofructose product, separating its purity of check through liquid chromatography is 96.7%.
Embodiment 3
With the yacon peeling of certain mass, stripping and slicing is got 80g and is immersed in 2wt%, and in the ascorbic acid solution of 400mL, wherein the mass volume ratio of yacon and leaching agent solution is 200g/L, and 60 ℃ of following constant temperature water bath lixiviates, extraction time is 2 hours; The vat liquor solid-liquid separation filters out the macrobead solid residue, and centrifugal treating further removes small granular suspended matters then, collects centrifugal back supernatant liquor; The centrifugal back of every 4mL supernatant liquor adds the pure acetonitrile of 6mL, and vibration mixes, and makes mixture leave standstill phase-splitting 10 hours under 2 ℃; After the mixture phase-splitting, get and carry out underpressure distillation mutually to remove lower boiling acetonitrile solvent, obtain 0.189g oligofructose product, separating its purity of check through liquid chromatography is 96.7%.
The present inventor has investigated the embodiment that the oligose in the yacon under the different condition extracts, its leaching process reference example 1, and the result is as shown in table 1.
Under table 1 different experimental conditions oligose in the yacon is extracted experimental result
By table 1 as seen, as long as guarantee the concentration of xitix to oligose in the yacon leach liquor, and strict controlled temperature is 0～10 ℃, just can be implemented in subsequently organic solvent to the phase-splitting effectively and rapidly of oligofructose, thereby obtains the higher oligofructose of purity.
Claims (9)
- One kind from yacon the extraction oligofructose method, it is characterized in that described method may further comprise the steps:1) with the yacon peeling, stripping and slicing, being immersed in concentration is in the leaching agent solution of 1wt%～3wt%, wherein the mass volume ratio of yacon and leaching agent solution is 50g/L～300g/L, carries out lixiviate under the constant temperature;2) with the vat liquor solid-liquid separation, filter out the macrobead solid residue, centrifugal treating further removes small granular suspended matters then, obtains leach liquor;3) add the polar organic solvent that dissolves each other with water in leach liquor, vibration mixes, and leaves standstill phase-splitting under 0～10 ℃, gets the solution of organic layer, removes polar organic solvent, obtains oligofructose.
- 2. the method that extracts oligofructose from yacon according to claim 1 is characterized in that the leaching agent in the described step 1) comprises xitix.
- 3. the method that extracts oligofructose from yacon according to claim 2 is characterized in that the concentration of xitix is 2wt%～2.5wt% in the described step 1), and extraction temperature is 40 ℃～70 ℃, extraction time 2～3 hours.
- 4. the method that extracts oligofructose from yacon according to claim 3 is characterized in that described step 1) extraction temperature is 50 ℃～60 ℃.
- 5. the method that extracts oligofructose from yacon according to claim 1 is characterized in that described step 3) Semi-polarity organic solvent is selected from acetonitrile, acetone, tetrahydrofuran (THF), 1-propyl alcohol and/or 2-propyl alcohol.
- 6. the method that extracts oligofructose from yacon according to claim 5 is characterized in that described step 3) Semi-polarity organic solvent is an acetonitrile.
- 7. according to claim 1 from yacon the method for extraction oligofructose, it is characterized in that the polar organic solvent and the step 2 that add in the described step 3)) volume ratio of the leach liquor that obtains is 2～7: 3, the time of leaving standstill phase-splitting is 6～12 hours.
- 8. according to claim 7 from yacon the method for extraction oligofructose, it is characterized in that the polar organic solvent and the step 2 that add in the described step 3)) volume ratio of the leach liquor that obtains is 1～2: 1, the time of leaving standstill phase-splitting is 8～10 hours.
- 9. the method that extracts oligofructose from yacon according to claim 1 is characterized in that the method that removes polar organic solvent in the described step 3) is underpressure distillation, the environmental stress≤0.05MPa of distillation under vacuum.
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| CN201110098472.1A CN102219808B (en) | 2011-04-20 | 2011-04-20 | Method for extracting fructooligosaccharides from yacon |
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| CN201110098472.1A CN102219808B (en) | 2011-04-20 | 2011-04-20 | Method for extracting fructooligosaccharides from yacon |
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| CN103288888A (en) * | 2013-06-09 | 2013-09-11 | 中国科学院昆明植物研究所 | Production method of smallanthus sonchifolius oligosaccharide |
| CN103355412A (en) * | 2013-08-09 | 2013-10-23 | 戴君程 | Nutrition powder (compound protein milk powder) and preparation method thereof |
| CN104592317A (en) * | 2014-12-09 | 2015-05-06 | 承德医学院中药研究所 | Yacon fructooligosaccharide and preparation method thereof |
| CN105002309A (en) * | 2015-07-08 | 2015-10-28 | 杨君 | Method for extracting fructose by using apple pomace |
| CN106749715A (en) * | 2016-11-23 | 2017-05-31 | 贵州大学 | A kind of decolouring preparation method of Smallantus sonchifolium extract solution |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288888A (en) * | 2013-06-09 | 2013-09-11 | 中国科学院昆明植物研究所 | Production method of smallanthus sonchifolius oligosaccharide |
| CN103355412A (en) * | 2013-08-09 | 2013-10-23 | 戴君程 | Nutrition powder (compound protein milk powder) and preparation method thereof |
| CN103355412B (en) * | 2013-08-09 | 2014-11-12 | 戴君程 | Nutrition powder (compound protein milk powder) and preparation method thereof |
| CN104592317A (en) * | 2014-12-09 | 2015-05-06 | 承德医学院中药研究所 | Yacon fructooligosaccharide and preparation method thereof |
| CN104592317B (en) * | 2014-12-09 | 2017-08-22 | 承德医学院 | A kind of yacon FOS and preparation method thereof |
| CN105002309A (en) * | 2015-07-08 | 2015-10-28 | 杨君 | Method for extracting fructose by using apple pomace |
| CN106749715A (en) * | 2016-11-23 | 2017-05-31 | 贵州大学 | A kind of decolouring preparation method of Smallantus sonchifolium extract solution |
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| CN102219808B (en) | 2014-04-02 |
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