CN102219808B - Method for extracting fructooligosaccharides from yacon - Google Patents
Method for extracting fructooligosaccharides from yacon Download PDFInfo
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- CN102219808B CN102219808B CN201110098472.1A CN201110098472A CN102219808B CN 102219808 B CN102219808 B CN 102219808B CN 201110098472 A CN201110098472 A CN 201110098472A CN 102219808 B CN102219808 B CN 102219808B
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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 field, particularly, the present invention relates to a kind of method that extracts oligofructose from yacon.
Background technology
In yacon, contain multiple human body essential amino acid and abundant mineral substance, particularly in its fruit butt, glucide content reaches more than 90%, mainly by the oligosaccharides such as oligofructose, sucrose, fructose, glucose and monose material, formed, 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 desirable functional additive, there is extensive use, it, as the mankind's heath food, is mainly a kind of good water-soluble dietary fibre, has the characteristics such as regulating intestinal canal microorganism species balance, preventing constipation, promotion mineral absorption, anti-ageing, prevention of dental caries; Can improve body immunity, long-term taking can play the effect of fat-reducing.In addition, all right part substitute antibiotics of oligofructose, is a kind of " green " fodder additives, and its application prospect is boundless.
From yacon vat liquor, extract oligofructose, need remove the interference of the impurity such as sucrose, fructose, glucose.The key step of the current oligofructose of purifying from yacon comprises: lixiviate, and--decolouring--deproteinated--nanofiltration separation obtains oligofructose product, this technique exists that cost is high, technique very complicated, oligofructose product purity is lower, doped with problems such as glucose, fructose.
In recent years, some emerging, efficient separating and purifying technologies develop rapidly, have been used to separating-purifying useful component from various natural products.Comparatively typically comprise two large classes: 1) in the situation that strong electrolyte salt (as the oxymuriate of basic metal or alkaline-earth metal, nitrate or vitriol) existence, to containing target and extracted in the aqueous solution of thing, add a kind of polar organic solvent, control certain condition, cause the polar organic solvent aqueous solution that originally homogeneous dissolves each other to split into two immiscible liquid phases, and target in initial aqueous solution is extracted thing and is distributed along with two-phase division can produce selective difference in two-phase; 2) in the situation that strong electrolyte salt exists, to containing target and extracted in the aqueous solution of thing, add a kind of high molecular weight water soluble polymer, control certain condition, cause the aqueous solutions of polymers that homogeneous dissolves each other originally to split into two immiscible liquid phases.This two-phase system because of two-phase water-content high, also referred to as aqueous two-phase extraction, effective especially for 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, in extraction process in high salt concentration medium, tend to cause occurring some unpredictable side reactions, the final form of extraction product is restive, even can destroy the activity of product to be separated.In addition, high salt concn is also a difficult problem to the corrosion of extraction equipment, and in polymkeric substance double-aqueous phase system, needs the macromolecular water-soluble polymkeric substance that use cost is higher, and polymkeric substance how economical and effective reclaims and recycling utilization need solution.
Summary of the invention
The object of the invention is to, in order to overcome the problems referred to above, provides a kind of method that extracts oligofructose from yacon.
According to the method that extracts oligofructose from yacon provided by the invention, said method comprising the steps of:
1) by 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 constant temperature;
2) by vat liquor solid-liquid separation, filter out macrobead solid residue, then centrifugal treating further removes small granular suspended matters, obtains leach liquor;
3) in leach liquor, add the polar organic solvent dissolving each other with water, vibration mixes, and the solution of organic layer is got in standing phase-splitting at 0～10 ℃, removes polar organic solvent, obtains oligofructose.
According to the method that extracts oligofructose from yacon of the present invention, described step 1) in leaching agent comprise 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 the method that extracts oligofructose from yacon of the present invention, step 1) concentration of described ascorbic acid solution is 1%wt～3%wt, preferably 2%～2.5%, extraction temperature is 40 ℃～70 ℃, is preferably 50 ℃～60 ℃, extraction time 2～3 hours.
According to the method that extracts oligofructose from yacon of the present invention, step 3) organic solvent adding in (pure acetonitrile) volume and step 2) volume ratio of the vat liquor supernatant liquor that obtains is 2: 3～7: 3, the temperature of standing phase-splitting is 0 ℃～10 ℃, the time of standing phase-splitting is 6～12 hours, wherein, the volume ratio of acetonitrile and vat liquor preferably 1: 1～2: 1, preferably 0 ℃～4 ℃ of the temperature of standing phase-splitting, preferably 8～10 hours time of standing phase-splitting.
According to the method that extracts oligofructose from yacon of the present invention, step 3) method that removes polar organic solvent in is distillation under vacuum, in still-process, allow system environmental stress remain on below 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 comprises the following steps:
(1) by the yacon peeling of certain mass, stripping and slicing, is immersed in certain density ascorbic acid solution constant temperature water bath lixiviate at a certain temperature;
(2) vat liquor solid-liquid separation filters out macrobead solid residue, and then centrifugal treating further removes small granular suspended matters, collects centrifugal rear supernatant liquor;
(3) get the centrifugal rear supernatant liquor of certain volume, add the pure acetonitrile of certain volume, vibration mixes, and controls suitable temperature and makes the standing phase-splitting of mixture;
(4) after mixture phase-splitting, get and carry out mutually underpressure distillation to remove lower boiling acetonitrile solvent, obtain highly purified oligofructose product.
A kind of method that extracts oligofructose from yacon of the present invention, utilize the monosaccharide concentration in yacon vat liquor higher, can there is phase-splitting at low temperatures in the supernatant liquor after vat liquor is centrifugal and the mixing solutions of acetonitrile, complete when phase-splitting, reach after balance, most oligofructose is all enriched in phase, the carbohydrate such as glucose and fructose is enriched in lower phase, what contain oligofructose above passes through underpressure distillation mutually, can obtain highly purified oligofructose, and acetonitrile can be realized recycling.
In a kind of method that extracts oligofructose from yacon of the present invention, can there is phase-splitting in not all organic solvent, therefore to being applicable to polar organic solvent of the present invention, screen, preferred acetonitrile in the present invention, and need yacon to carry out lixiviate in the process of extracting oligose, make the concentration of oligose wherein reach certain concentration, just can make after adding organic solvent effective, phase-splitting fast, therefore in the present invention, using the ascorbic acid solution of 1wt%～3wt% as infusion solution, in strict control solution, the mass volume ratio of yacon and leach liquor is 50g/L～300g/L, and strictly to control temperature be 0～10 ℃, thereby realized phase-splitting fast, obtain the oligose that purity is higher, organic solution also realizes recycling simultaneously.
The invention has the advantages that and effectively avoid the existing problems such as the cost that oligofructose method exists is high, technique very complicated, and life cycle of the product is long, and oligofructose purity is low of extracting from yacon vat liquor.
Accompanying drawing explanation
Fig. 1 for extracting the method flow diagram of oligofructose from yacon.
Embodiment
Embodiment 1
By the yacon peeling of certain mass, stripping and slicing, gets 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, constant temperature water bath lixiviate at 60 ℃, and extraction time is 2 hours; Vat liquor solid-liquid separation filters out macrobead solid residue, and then centrifugal treating further removes small granular suspended matters, collects centrifugal rear supernatant liquor; The centrifugal rear supernatant liquor of every 4mL adds the pure acetonitrile of 6mL, and vibration mixes, and makes the standing phase-splitting of mixture 8 hours at 1 ℃; After mixture phase-splitting, getting and carry out mutually underpressure distillation to remove lower boiling acetonitrile solvent, obtain 0.195g oligofructose product, is 96.7% through its purity of the separated check of liquid chromatography.
Embodiment 2
By the yacon peeling of certain mass, stripping and slicing, gets 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, constant temperature water bath lixiviate at 60 ℃, and extraction time is 3 hours; Vat liquor solid-liquid separation filters out macrobead solid residue, and then centrifugal treating further removes small granular suspended matters, collects centrifugal rear supernatant liquor; The centrifugal rear supernatant liquor of every 5mL adds the pure acetonitrile of 5mL, and vibration mixes, and makes the standing phase-splitting of mixture 10 hours at 4 ℃; After mixture phase-splitting, getting and carry out mutually underpressure distillation to remove lower boiling acetonitrile solvent, obtain 0.174g oligofructose product, is 96.7% through its purity of the separated check of liquid chromatography.
Embodiment 3
By the yacon peeling of certain mass, stripping and slicing, gets 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, constant temperature water bath lixiviate at 60 ℃, and extraction time is 2 hours; Vat liquor solid-liquid separation filters out macrobead solid residue, and then centrifugal treating further removes small granular suspended matters, collects centrifugal rear supernatant liquor; The centrifugal rear supernatant liquor of every 4mL adds the pure acetonitrile of 6mL, and vibration mixes, and makes the standing phase-splitting of mixture 10 hours at 2 ℃; After mixture phase-splitting, getting and carry out mutually underpressure distillation to remove lower boiling acetonitrile solvent, obtain 0.189g oligofructose product, is 96.7% through its purity of the separated check of liquid chromatography.
The present inventor has investigated the embodiment that the oligose in yacon under different condition extracts, its leaching process reference example 1, and result is as shown in table 1.
Under table 1 different experimental conditions, the oligose in yacon is extracted to experimental result
From table 1, as long as guarantee the concentration of xitix to oligose in yacon leach liquor, and strictly to control temperature be 0～10 ℃, just can realize the phase-splitting effectively and rapidly to oligofructose at organic solvent subsequently, thereby obtain the oligofructose that purity is higher.
Claims (7)
1. from yacon, extract a method for oligofructose, it is characterized in that, described method comprises the following steps:
1) by 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 constant temperature;
Wherein, described leaching agent is xitix;
Described extraction temperature is 40 ℃～70 ℃, extraction time 2～3 hours;
2) by vat liquor solid-liquid separation, filter out macrobead solid residue, then centrifugal treating further removes small granular suspended matters, obtains leach liquor;
3) in leach liquor, add the polar organic solvent dissolving each other with water, vibration mixes, and the solution of organic layer is got in standing phase-splitting at 0～10 ℃, removes polar organic solvent, obtains oligofructose;
Wherein, the polar organic solvent and the step 2 that in described step 3), add) volume ratio of the leach liquor that obtains is 2～7:3, the time of standing phase-splitting is 6～12 hours.
2. the method that extracts oligofructose from yacon according to claim 1, is characterized in that, in described step 1), the concentration of xitix is 2wt%～2.5wt%.
3. the method that extracts oligofructose from yacon according to claim 1, is characterized in that, described step 1) extraction temperature is 50 ℃～60 ℃.
4. 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.
5. the method that extracts oligofructose from yacon according to claim 4, is characterized in that, described step 3) Semi-polarity organic solvent is acetonitrile.
6. the method that extracts oligofructose from yacon according to claim 1, is characterized in that, the polar organic solvent and the step 2 that in described step 3), add) volume ratio of the leach liquor that obtains is 1～2:1, the time of standing phase-splitting is 8～10 hours.
7. the method that extracts oligofructose from yacon according to claim 1, is characterized in that, the method that removes polar organic solvent in 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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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN103355412B (en) * | 2013-08-09 | 2014-11-12 | 戴君程 | Nutrition powder (compound protein milk powder) 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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| CN1820643A (en) * | 2006-03-23 | 2006-08-23 | 昆明瑞鹏生态农业科技有限公司 | Process for preparing saussurea involucrata fruit full powder |
| CN1831014A (en) * | 2006-01-19 | 2006-09-13 | 昆明瑞鹏生态农业科技有限公司 | Process for preparing inslin and oligofructose using xuelianguo fruits as raw material |
| CN101283761A (en) * | 2008-05-27 | 2008-10-15 | 昆明理工大学 | Smallanthus sonchifolius fruit extract and extracting method and application |
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| KR20040107611A (en) * | 2003-06-05 | 2004-12-23 | 영숙 김 | A Study of Functional Food Yacon Jam |
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| CN1831014A (en) * | 2006-01-19 | 2006-09-13 | 昆明瑞鹏生态农业科技有限公司 | Process for preparing inslin and oligofructose using xuelianguo fruits as raw material |
| CN1820643A (en) * | 2006-03-23 | 2006-08-23 | 昆明瑞鹏生态农业科技有限公司 | Process for preparing saussurea involucrata fruit full powder |
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