CN104592317A - Yacon fructooligosaccharide and preparation method thereof - Google Patents
Yacon fructooligosaccharide and preparation method thereof Download PDFInfo
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Abstract
The invention relates to yacon fructooligosaccharide and a preparation method thereof, and the method comprises steps of pretreatment, extraction, flocculation, extraction and concentration. The fructooligosaccharide content of the yacon fructooligosaccharide accounts for 90% or more by weight of the total yacon fructooligosaccharide. The yacon fructooligosaccharide extraction method is lower in solvent total consumption compared with the prior art, the yacon fructooligosaccharide extraction rate is high, and the content of yacon fructooligosaccharide obtained by using the method is high. Therefore, the method is extremely beneficial for industrialized large-scale production because of relatively small solvent consumption, high efficiency, high content and simple and practicable operation.
Description
[technical field]
The invention belongs to and extract oligose technical field from plant.More specifically, the present invention relates to a kind of yacon oligofructose, also relate to the preparation method of described yacon oligofructose.
[background technology]
Yacon (Smallanthus sonchifolius [Poepp. & Endl.] H.Robinson), have another name called Ya Gong (Yacon), for a member of composite family (Compositae orAsteraceae) plant families, originating in South America Andes, is live in the traditional tuberous foodstuffs of the aboriginal Indian of alpine region, Andes.Yacon pulp mouthfeel is the spitting image of water pears, juice is many and glittering and translucent, fragrant and sweet crisp and refreshing, containing more than 20 kinds of essential amino acids and enrich mineral substance and great amount of soluble fiber, comprising oligofructose, belong to low calorific food, but its carbohydrate is not absorption of human body, therefore, be well suited for diabetics and slimmer to eat.In South America, often by the protective foods as diabetic, various digestive function or kidney disorder patient.
Yacon dry-matter (Dry matter, DM) main component is oligofructose, oligofructose (fructooligo-saccharides, be called for short FOS) be again fructooligosaccharide or Polylevulosan, molecular formula is G-F-Fn, (G is glucosyl group, F is fructosyl, n=1 ~ 3), it is the linear oligosacchardides that fructose and glucose are formed, be the fructosyl of sucrose be combined into β-1,2 glycosidic link and 1 ~ 3 fructosyl kestose (GF2), GF3 (GF3), GF4 (GF4) mixture.Oligofructose has and improves flora in body, toxin-expelling intestine-cleaning, improves lipid metabolism, reduces blood fat, regulates body immune system, improve immunizing power, promote the biological activitys such as mineral absorption.
At present, CN 102219808A discloses a kind of method extracting oligofructose from yacon, and it comprises yacon and is immersed in leaching agent (xitix) solution, extracting at constant temperature; Solid-liquid separation, obtains leach liquor; In leach liquor, add the polar organic solvent dissolved each other with water, vibration mixing, removes polar organic solvent and obtains the steps such as oligofructose.The people such as You Yi are being entitled as " yacon oligofructose extraction and isolation and analysis and research ", " Institutes Of Technology Of Changsha's master thesis ", describe in 2011 and utilize water-bath restricted-access media oligofructose, carry out protecting look with xitix, use cation polypropylene amides gel to carry out flocculation purifying and with desolventing technology etc. such as D941 resins.The technological deficiency that these prior aries exist is as follows: A, be easier to brown stain with the infusion of water-bath microwave leaching technology and the squeezeding juice ratio extracting yacon oligofructose of squeezing the juice, and be difficult to process, treating processes is loaded down with trivial details; B, hot water bath lixiviate access method temperature are high, and side reaction is many and oligofructose is oxidizable, and the oligofructose in yacon is oxidizable, and extraction yield is low, be not as abundant as supersound extraction; C, colour protecting agent are very important in its leaching process, if it is too large to Influence on test result to go wrong.
The present inventor, for prior art defect, on the basis of summing up prior art, by a large amount of experimental studies, finally solves these technical problems, completes the present invention.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of yacon oligofructose.
Another object of the present invention is to provide the preparation method of described yacon oligofructose.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of extracting method of yacon oligofructose.
The step of this extracting method is as follows:
A, pre-treatment
Cleaned by fresh yacon, then cut into slices, it is by weight less than 5% that this saussurea involucrata chankings is dried to water-content again under the condition of temperature 50 ~ 60 DEG C, obtains a kind of yacon dry-matter;
B, extraction
The yacon dry-matter using pulverizer steps A to be obtained is ground into yacon powder, be 1:10 ~ 80 according to the volume ratio of yacon powder and aqueous citric acid solution again, aqueous citric acid solution extraction agent is added in described yacon powder, then ultrasonic device is used to carry out supersound extraction 2 ~ 4 times under the condition of frequency 40KHz and power 500W, all supersound extraction liquid merges, and obtains a kind of yacon extracting solution;
C, flocculation
The yacon extracting solution that step B obtains mixes according to volume ratio 0.5 ~ 2.5 with cation polypropylene amides gel solution, then uses ammoniacal liquor and aqueous acetic acid by its pH regulator to 5.0 ~ 7.0, then flocculates, suction filtration, obtain a kind of clear solution;
D, extraction
According to volume ratio 1:10 ~ 30 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:2 ~ 10, then removing emulsification and extraction liquid is separated, this extraction step repeats 3 ~ 6 times, the raffinate aqueous phase obtained merges, then at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume, obtain the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 90 ~ 98% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the supernatant liquor obtained is concentrated into 1/2 of described supernatant volume again at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, the throw out obtained is yacon oligofructose.
In step, described saussurea involucrata chankings first uses water rinse 0.4 ~ 0.6h to a preferred embodiment of the invention, and then dries under the condition of temperature 50 ~ 60 DEG C, obtains yacon dry-matter; Or
Described saussurea involucrata chankings first uses 0.2%NaHSO
3aqueous solution rinsing 0.4 ~ 0.6h, and then dry under the condition of temperature 50 ~ 60 DEG C, obtain yacon dry-matter; Or
Described saussurea involucrata chankings first uses water rinse 0.4 ~ 0.6h, and then lyophilize at temperature 50 ~ 60 DEG C with the condition of vacuum tightness 1 ~ 10Pa, obtains yacon dry-matter.
In step, the thickness of described saussurea involucrata chankings is 0.4 ~ 1.0cm to a preferred embodiment of the invention.
A preferred embodiment of the invention, in stepb, the granularity of described yacon powder is 60 ~ 120 orders.
A preferred embodiment of the invention, in stepb, the concentration of described aqueous citric acid solution is by weight 0.1 ~ 0.6%.
A preferred embodiment of the invention, in stepb, the time of each supersound extraction is 0.5 ~ 3.0h.
A preferred embodiment of the invention, in step C, the concentration of the described cation polypropylene amides gel aqueous solution is by weight 0.01 ~ 0.20%.
A preferred embodiment of the invention, in step C, the time of carrying out flocculating is 1.0 ~ 4.0h.
The invention still further relates to the yacon oligofructose adopting described method to obtain.
A preferred embodiment of the invention, the oligofructose content of described yacon oligofructose is with described yacon oligofructose total weight more than 90%.
In more detail the present invention will be described below.
The present invention relates to a kind of extracting method of yacon oligofructose.
The step of this extracting method is as follows:
A, pre-treatment
Cleaned by fresh yacon, then cut into slices, it is by weight less than 5% that this saussurea involucrata chankings is dried to water-content again under the condition of temperature 50 ~ 60 DEG C, obtains a kind of yacon dry-matter.
Fresh yacon clear water washes away the silt be attached on fruit, foreign material, is then used in normally used slicing machine in food processing technology field and cuts into slices.Preferably, the thickness of described saussurea involucrata chankings is 0.4 ~ 1.0cm, and more preferably, the thickness of described saussurea involucrata chankings is 0.6 ~ 0.8cm.
In this step, the object of this saussurea involucrata chankings drying and processing is its water-content to be reduced to by weight less than 5% because, if its water-content higher than 5% time, then can not easily preserve perishable.
In this step, the equipment that this saussurea involucrata chankings drying and processing uses is normally used drying plant in food processing technology field, the dryer such as sold with trade(brand)name digital display air dry oven by Shanghai Boxun Industrial Co., Ltd..
In the present invention, this saussurea involucrata chankings can also process in the following manner:
The saussurea involucrata chankings obtained first uses water rinse 0.4 ~ 0.6h, and then dries under the condition of temperature 50 ~ 60 DEG C, obtains yacon dry-matter.
In this step, be removal of impurities with the effect of water rinse.
Or
The saussurea involucrata chankings obtained first uses 0.2%NaHSO
3aqueous solution rinsing 0.4 ~ 0.6h, and then dry under the condition of temperature 50 ~ 60 DEG C, obtain yacon dry-matter.
In this step, 0.2%NaHSO is used
3the effect of the aqueous solution is anti-oxidant.
Or
Described saussurea involucrata chankings first uses water rinse 0.4 ~ 0.6h, and then lyophilize at temperature 50 ~ 60 DEG C with the condition of vacuum tightness 1 ~ 10Pa, obtains yacon dry-matter.
In this step, the equipment that this saussurea involucrata chankings lyophilize process uses is normally used freeze drying equipment in food processing technology field, the freeze drier such as sold with trade(brand)name CHRIST Laboratary type freeze drier by German MARTINCHRIST company.
B, extraction
The yacon dry-matter using pulverizer steps A to be obtained is ground into yacon powder, be 1:10 ~ 80 according to the volume ratio of yacon powder and aqueous citric acid solution again, aqueous citric acid solution extraction agent is added in described yacon powder, then ultrasonic device is used to carry out supersound extraction 2 ~ 4 times under the condition of frequency 40KHz and power 500W, all supersound extraction liquid merges, and obtains a kind of yacon extracting solution;
In this step, normally used disintegrating apparatus in food processing technology field can be used in, the pulverizer such as sold with trade(brand)name high-speed multifunctional pulverizer by Yongkang City Jiu Pin Trade Co., Ltd., yacon dry-matter steps A obtained is ground into yacon powder.If desired, be used in normally used screening plant in food processing technology field, the sieve such as sold with trade(brand)name sub-sieve by the first sifter device factory on the qian of Shangyu sieves, and collects granularity 60 ~ 120 object yacon powder, preferably collects granularity 80 ~ 100 object yacon powder.
In this step, use aqueous citric acid solution extraction agent to extract yacon oligofructose in yacon powder, the mechanism of action of its citric acid extraction agent anti-oxidantly prevents extracting solution brown stain.
According to the present invention; except citric acid extraction agent, everyly can extract yacon oligofructose from yacon powder, but dysgenic material can not be produced to yacon oligofructose quality and may be used to the present invention; also all in the scope of protection of present invention, such as xitix or NaHSO
3the aqueous solution etc.
In the present invention, if when the volume ratio of yacon powder and aqueous citric acid solution is more than 1:10, then can lose time and reagent because extraction efficiency is low; If when the volume ratio of yacon powder and aqueous citric acid solution is below 1:80, then understands low and next step flocculation of oligofructose extraction yield because yacon powder can not fully contact with extracting solution and badly to do.Therefore, the volume ratio of yacon powder and aqueous citric acid solution is 1:10 ~ 80 is rational, preferably 1:25 ~ 65, more preferably 1:36 ~ 52.
In the present invention, the concentration of described aqueous citric acid solution is by weight 0.1 ~ 0.6%, if aqueous citric acid solution concentration exceedes this scope, then understands oligofructose extraction yield because extracting solution acidity is large low; Preferably 0.2 ~ 0.5%, more preferably 0.2 ~ 0.4%.
In this step, the effect using ultrasonic device to carry out supersound process is from yacon powder, to extract oligofructose fully.
The ultrasonic device that the present invention uses is normally used ultrasonic device in food processing technology field, the ultrasonic apparatus of such as being sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd..
In the present invention, such as use the ultrasonic apparatus of being sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd., under the condition at frequency 40KHz and power 500W, carry out supersound extraction 2 ~ 4 times, the time of each supersound extraction is 0.5 ~ 3.0h.Certainly, when actual supersound process, its ultrasonic frequency, ultrasonic power, supersound extraction number of times and supersound extraction time suitably can adjust according to the actual effect reached.
C, flocculation
The yacon extracting solution that step B obtains mixes according to volume ratio 0.5 ~ 2.5 with cation polypropylene amides gel solution, then uses ammoniacal liquor and aqueous acetic acid by its pH regulator to 5.0 ~ 7.0, then flocculates, suction filtration, obtain a kind of clear solution;
Cation polypropylene amides gel is all in the electricity positive in acid or alkaline medium, and therefore it can negative charge particle in adsorbent solution, and such as protein, polysaccharide etc., form floc settlement because making its particle electric neutrality and get off.Many particulates in adsorbent solution can also couple together by cation polypropylene amides gel, form floc sedimentation sedimentation, thus make solution become clarification.
The cation polypropylene amides gel that the present invention uses should have following performance:
Flocculence: cation polypropylene amides gel can make suspended matter by charge neutrality, bridge formation adsorption, plays throwing out.
Binding property: cation polypropylene amides gel by machinery, physics, chemistry effect, rise adhesive effect.
Fall resistive: cation polypropylene amides gel can reduce the friction resistance of fluid effectively, add trace P AM in water and just can fall resistance 50-80%.
The cation polypropylene amides gel that the present invention uses reaches the limited public affairs of auspicious fine chemicals with trade(brand)name cation polypropylene amides gel product sold by Shanghai.
In the present invention, the concentration of the cation polypropylene amides gel aqueous solution and the pH of yacon extracting solution and cation polypropylene amides gel solution mixture are vital.If the concentration of the described cation polypropylene amides gel aqueous solution is lower than 0.01%, then understand magazine in extracting solution because flocculation is not thorough many; If the concentration of the cation polypropylene amides gel aqueous solution is higher than 0.20%, then can reduce oligofructose extraction yield because flocculation agent is too many; Therefore, the concentration of the cation polypropylene amides gel aqueous solution is 0.01 ~ 0.20% is appropriate, preferably 0.05 ~ 0.15%, more preferably 0.08 ~ 0.12%.
When regulating pH, institute uses the concentration of ammoniacal liquor and aqueous acetic acid to be not critical, but the rare or overrich of mistake is all worthless.
In this step, the time using the cation polypropylene amides gel aqueous solution to carry out flocculating is 1.0 ~ 4.0h, if flocculation time is too short or long is all not all right, this is because in general, the time of flocculation is longer, can make flocculation purification more fully but caused by wadding a quilt with cotton after can finding out 3h by experiment and substantially reaching capacity.
In this step, suction filtration should reach solids content in the clear solution obtained lower than 10%, otherwise subsequent disposal is bad does.The pumping and filtering device used during suction filtration is normally used pumping and filtering device in chemical technology field, such as, use Büchner funnel suction filtration.
D, extraction
According to volume ratio 1:10 ~ 30 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:2 ~ 10, then removing emulsification and extraction liquid is separated, this extraction step repeats 3 ~ 6 times, the raffinate aqueous phase obtained merges, then at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume, obtain the raffinate aqueous phase concentrated.
The object of this extraction step removes protein.
In this step, if the volume ratio of clear solution and extraction agent is greater than 1:10, then can protein etc. remove unclean; If the volume ratio of clear solution and extraction agent is less than 1:30, then reagent can be wasted; Therefore, the volume ratio of clear solution and extraction agent is 1:10 ~ 30 is appropriate, and preferably, the volume ratio of clear solution and extraction agent is 1:14 ~ 26, and more preferably, the volume ratio of clear solution and extraction agent is 1:18 ~ 22.
It is normally used extraction equipment in chemical technology field that the present invention extracts the equipment used, such as, by separating funnel.
The equipment that vacuum concentration of the present invention uses is normally used vacuum concentration equipment in food processing technology field, the vacuum concentration equipment such as sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant.
Determine according to HPLC-ELSD analytical procedure, institute's concentrated raffinate aqueous phase that obtains is mainly containing oligofructose.
E, concentrated
The aqueous ethanolic solution that concentration is by volume 90 ~ 98% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the supernatant liquor obtained is concentrated into 1/2 of described supernatant volume again at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, the throw out obtained is yacon oligofructose.
In this step, the object of alcohol precipitation is removing polysaccharide macro-molecular material for the first time.
The object of second time alcohol precipitation is that precipitation obtains oligofructose.
The equipment that vacuum concentration of the present invention uses is normally used vacuum concentration equipment in food processing technology field, such as, by the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant.
Following analysis has been carried out to yacon oligofructose throw out:
According to GB/T 23528-2009 oligofructose national standard analytical procedure, HPLC ELSD detection method (HPLC-ELSD) is carried out to yacon oligofructose, its measurement result is shown in accompanying drawing 1, can determine throw out mainly containing yacon oligofructose by accompanying drawing 1 according to contrast reference substance color atlas.This measuring method is determined, oligofructose content is by weight more than 90%.
The extraction yield that can calculate the inventive method according to following formula by yacon raw material and the yacon oligofructose that obtains is 56-45%.
Yacon oligofructose extraction yield (%)=oligofructose/yacon powder × 100%.
The invention still further relates to the yacon oligofructose adopting described method to obtain.
The oligofructose content of described yacon oligofructose is with described yacon oligofructose total weight more than 90%.
Yacon oligofructose extracting method of the present invention has following feature:
1, the extraction efficiency of the inventive method is high.The extraction yield of prior art is 45%, and the inventive method yacon oligofructose extraction yield is 56%, and therefore the inventive method is higher than prior art by 11%.
2, the yacon oligofructose content of the inventive method acquisition is high.The yacon oligofructose content that prior art obtains is 80%, and the yacon oligofructose content that the inventive method obtains is more than 90%, and therefore the inventive method is higher than prior art by more than 10%.
3, the inventive method due to solvent-oil ratio less, efficiency is high, and content is high, and operation is simple and be very beneficial for industrialized production, and prior art then efficiency is low, and content is low and operation is loaded down with trivial details.
[beneficial effect]
The invention has the beneficial effects as follows:
The oligofructose content of yacon oligofructose of the present invention is with described yacon oligofructose total weight more than 90%.The inventive method yacon oligofructose extraction yield is higher than prior art by 11%; The yacon oligofructose content that the inventive method obtains is high by more than 10%; Therefore, the inventive method due to due to solvent-oil ratio less, efficiency is high, and content is high, and operation is simple and be very beneficial for industrialized production.
[accompanying drawing explanation]
Fig. 1: the yacon oligofructose sample HPLC-ELSD that the inventive method obtains schemes.
[embodiment]
The present invention can be understood better by following embodiment.
Embodiment 1: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 0.6cm, it is by weight less than 5% that this saussurea involucrata chankings is dried to water-content again under the condition of temperature 60 C, obtains a kind of yacon dry-matter;
B, extraction
Yacon dry-matter steps A obtained with the pulverizer that the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold is sold by Yongkang City Jiu Pin Trade Co., Ltd. is used to be ground into granularity 80 object yacon powder, be 1:36 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.3% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 2 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 1.4h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.01% reach by Shanghai the cation polypropylene amides gel solution that the limited public affairs of auspicious fine chemicals sell with trade(brand)name cation polypropylene amides gel and mix according to volume ratio 1.8 by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 5.0, then flocculation 1.0h is carried out, carry out suction filtration with Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:10 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:8, then removing emulsification and extraction liquid is separated, this extraction step repeats 3 times, the raffinate aqueous phase obtained merges, then the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant carries out vacuum concentration to 1/4 of former raffinate aqueous phase volume under the condition of temperature 50 C and vacuum tightness 0.90Pa, obtains the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 94% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the supernatant liquor obtained re-uses the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant and be concentrated into 1/2 of described supernatant volume under the condition of temperature 50 C and vacuum tightness 0.90Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 93%.
Embodiment 2: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 0.4cm, described saussurea involucrata chankings first uses water rinse 0.4h, and then dries under the condition of temperature 50 C, obtains yacon dry-matter.
B, extraction
Yacon dry-matter steps A obtained with the pulverizer that the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold is sold by Yongkang City Jiu Pin Trade Co., Ltd. is used to be ground into granularity 100 object yacon powder, be 1:10 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.5% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 3 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 0.5h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.20% reach the limited public affairs of auspicious fine chemicals by Shanghai and mix according to volume ratio 0.5 with the cation polypropylene amides gel solution of trade(brand)name cation polypropylene amides gel by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 6.5, then flocculation 2.0h is carried out, carry out suction filtration with Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:30 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:2, then removing emulsification and extraction liquid is separated, this extraction step repeats 5 times, the raffinate aqueous phase obtained merges, then at temperature 55 DEG C with the condition of vacuum tightness 0.80Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume by Shanghai Yarong Biochemical Instrument Plant with the vacuum concentration equipment that trade(brand)name RE-52AA Rotary Evaporators is sold, obtain the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 90% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the vacuum concentration equipment that the supernatant liquor obtained is sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant is again concentrated into 1/2 of described supernatant volume at temperature 55 DEG C with the condition of vacuum tightness 0.80Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 92%.
Embodiment 3: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 1.0cm, this saussurea involucrata chankings first uses 0.2%NaHSO
3aqueous solution rinsing 0.3h, and then dry under the condition of temperature 54 DEG C, obtain yacon dry-matter.
B, extraction
Use and be ground into granularity 60 object yacon powder by Yongkang City Jiu Pin Trade Co., Ltd. with the yacon dry-matter that steps A obtains by the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold, be 1:52 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.6% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 4 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 3.0h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.08% mix according to volume ratio 1.2 by being reached the cation polypropylene amides gel solution that the limited public affairs of auspicious fine chemicals sell with trade(brand)name cation polypropylene amides gel by Shanghai by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 7.0, then flocculation 4.0h is carried out, carry out suction filtration by Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:18 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:10, then removing emulsification and extraction liquid is separated, this extraction step repeats 4 times, the raffinate aqueous phase obtained merges, then the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant carries out vacuum concentration to 1/4 of former raffinate aqueous phase volume under the condition of temperature 60 C and vacuum tightness 0.95Pa, obtains the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 98% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant again of the supernatant liquor obtained is concentrated into 1/2 of described supernatant volume under the condition of temperature 60 C and vacuum tightness 0.95Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 92%.
Embodiment 4: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 0.8cm, this saussurea involucrata chankings first uses water rinse 0.6h, and then lyophilize obtains yacon dry-matter.
B, extraction
Use and be ground into granularity 120 object yacon powder by Yongkang City Jiu Pin Trade Co., Ltd. with the yacon dry-matter that steps A obtains by the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold, be 1:80 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.1% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 3 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 2.2h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.12% mix according to volume ratio 2.5 by being reached the cation polypropylene amides gel solution that the limited public affairs of auspicious fine chemicals sell with trade(brand)name cation polypropylene amides gel by Shanghai by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 5.6, then flocculation 3.0h is carried out, carry out suction filtration by Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:22 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:5, then removing emulsification and extraction liquid is separated, this extraction step repeats 6 times, the raffinate aqueous phase obtained merges, then at temperature 65 DEG C with the condition of vacuum tightness 0.90Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume by Shanghai Yarong Biochemical Instrument Plant with the vacuum concentration equipment that trade(brand)name RE-52AA Rotary Evaporators is sold, obtain the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 96% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the vacuum concentration equipment that the supernatant liquor obtained is sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant is again concentrated into 1/2 of described supernatant volume at temperature 65 DEG C with the condition of vacuum tightness 0.90Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 93%.
Embodiment 5: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 0.6, it is by weight less than 5% that this saussurea involucrata chankings is dried to water-content again under the condition of temperature 50 C, obtains a kind of yacon dry-matter.
B, extraction
Use and be ground into granularity 80 object yacon powder by Yongkang City Jiu Pin Trade Co., Ltd. with the yacon dry-matter that steps A obtains by the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold, be 1:10 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.6% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 3 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 1.4h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.20% mix according to volume ratio 1.2 by being reached the cation polypropylene amides gel solution that the limited public affairs of auspicious fine chemicals sell with trade(brand)name cation polypropylene amides gel by Shanghai by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 5.6, then flocculation 1.0h is carried out, carry out suction filtration by Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:30 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:10, then removing emulsification and extraction liquid is separated, this extraction step repeats 6 times, the raffinate aqueous phase obtained merges, then the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant carries out vacuum concentration to 1/4 of former raffinate aqueous phase volume under the condition of temperature 60 C and vacuum tightness 0.80Pa, obtains the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 98% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the vacuum concentration equipment that the supernatant liquor obtained is sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant is again concentrated into 1/2 of described supernatant volume at temperature 65 DEG C with the condition of vacuum tightness 0.70Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 90%.
Embodiment 6: the extraction of yacon oligofructose
The implementation step of this embodiment is as follows:
A, pre-treatment
Cleaned by fresh yacon clear water, then saussurea involucrata chankings is cut into the sheet of thickness 1.0cm, this saussurea involucrata chankings first uses 0.2%NaHSO
3aqueous solution rinsing 0.6h, and then dry under the condition of temperature 54 DEG C, obtain yacon dry-matter.
B, extraction
Use and be ground into granularity 120 object yacon powder by Yongkang City Jiu Pin Trade Co., Ltd. with the yacon dry-matter that steps A obtains by the pulverizer that trade(brand)name high-speed multifunctional pulverizer is sold, be 1:36 according to the volume ratio of yacon powder and aqueous citric acid solution again, the aqueous citric acid solution extraction agent that concentration is by weight 0.5% is added in described yacon powder, then the ultrasonic device sold with trade(brand)name KQ-100E ultrasonic cleaner by Kunshan Ultrasonic Instruments Co., Ltd. is used to carry out supersound extraction 4 times under the condition of frequency 40KHz and power 500W, the time of each supersound extraction is 2.2h, all supersound extraction liquid merges, obtain a kind of yacon extracting solution,
C, flocculation
The yacon extracting solution that step B obtains and concentration are 0.01% reach by Shanghai the cation polypropylene amides gel solution that the limited public affairs of auspicious fine chemicals sell with trade(brand)name cation polypropylene amides gel and mix according to volume ratio 0.5 by weight, then use by volume 30% ammoniacal liquor and 28% aqueous acetic acid by weight by its pH regulator to 7.0, then flocculation 3.0h is carried out, carry out suction filtration by Büchner funnel, obtain a kind of clear solution;
D, extraction
According to the volume ratio 1:10 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:2, then removing emulsification and extraction liquid is separated, this extraction step repeats 4 times, the raffinate aqueous phase obtained merges, then at temperature 65 DEG C with the condition of vacuum tightness 0.70Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume by Shanghai Yarong Biochemical Instrument Plant with the vacuum concentration equipment that trade(brand)name RE-52AA Rotary Evaporators is sold, obtain the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 90% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the vacuum concentration equipment sold with trade(brand)name RE-52AA Rotary Evaporators by Shanghai Yarong Biochemical Instrument Plant again of the supernatant liquor obtained is concentrated into 1/2 of described supernatant volume under the condition of temperature 60 C and vacuum tightness 0.90Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, obtain yacon oligofructose extract.
Adopt the method described in present specification to measure, the yacon oligofructose content of described extract is with described extract total weight 91%.
Claims (10)
1. an extracting method for yacon oligofructose, is characterized in that the step of the method is as follows:
A, pre-treatment
Cleaned by fresh yacon, then cut into slices, it is by weight less than 5% that this saussurea involucrata chankings is dried to water-content again under the condition of temperature 50 ~ 60 DEG C, obtains a kind of yacon dry-matter;
B, extraction
The yacon dry-matter using pulverizer steps A to be obtained is ground into yacon powder, be 1:10 ~ 80 according to the volume ratio of yacon powder and aqueous citric acid solution again, aqueous citric acid solution extraction agent is added in described yacon powder, then ultrasonic device is used to carry out supersound extraction 2 ~ 4 times under the condition of frequency 40KHz and power 500W, all supersound extraction liquid merges, and obtains a kind of yacon extracting solution;
C, flocculation
The yacon extracting solution that step B obtains mixes according to volume ratio 0.5 ~ 2.5 with cation polypropylene amides gel solution, then uses ammoniacal liquor and aqueous acetic acid by its pH regulator to 5.0 ~ 7.0, then flocculates, suction filtration, obtain a kind of clear solution;
D, extraction
According to volume ratio 1:10 ~ 30 of clear solution and extraction agent, the clear solution that step C obtains uses chloroform to extract with the extraction agent that propyl carbinol mixes according to volume ratio 1:2 ~ 10, then removing emulsification and extraction liquid is separated, this extraction step repeats 3 ~ 6 times, the raffinate aqueous phase obtained merges, then at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, carry out vacuum concentration to 1/4 of former raffinate aqueous phase volume, obtain the raffinate aqueous phase concentrated;
E, concentrated
The aqueous ethanolic solution that concentration is by volume 90 ~ 98% is added in the concentrated raffinate aqueous phase that step D obtains, stir, until the alcohol concn in concentrated raffinate aqueous phase reaches by volume 70%, leave standstill, allow polysaccharide precipitation in concentrated raffinate aqueous phase, centrifugation, disgorging, the supernatant liquor obtained is concentrated into 1/2 of described supernatant volume again at temperature 55 ~ 65 DEG C with the condition of vacuum tightness 0.70 ~ 0.95Pa, then add dehydrated alcohol and reach its concentration for by volume 90%, stir, centrifugation, the throw out obtained is yacon oligofructose.
2. method according to claim 1, is characterized in that in step, and described saussurea involucrata chankings first uses water rinse 0.4 ~ 0.6h, and then dries under the condition of temperature 50 ~ 60 DEG C, obtains yacon dry-matter; Or
Described saussurea involucrata chankings first uses 0.2% NaHSO
3aqueous solution rinsing 0.4 ~ 0.6h, and then dry under the condition of temperature 50 ~ 60 DEG C, obtain yacon dry-matter; Or
Described saussurea involucrata chankings first uses water rinse 0.4 ~ 0.6h, and then lyophilize at temperature 50 ~ 60 DEG C with the condition of vacuum tightness 1 ~ 10Pa, obtains yacon dry-matter.
3. method according to claim 1, is characterized in that in step, and the thickness of described saussurea involucrata chankings is 0.4 ~ 1.0cm.
4. method according to claim 1, is characterized in that in stepb, and the granularity of described yacon powder is 60 ~ 120 orders.
5. method according to claim 1, is characterized in that in stepb, and the concentration of described aqueous citric acid solution is by weight 0.1 ~ 0.6%.
6. method according to claim 1, is characterized in that in stepb, and the time of each supersound extraction is 0.5 ~ 3.0h.
7. method according to claim 1, is characterized in that in step C, and the concentration of the described cation polypropylene amides gel aqueous solution is by weight 0.01 ~ 0.20%.
8. method according to claim 1, is characterized in that in step D, and the time of carrying out flocculating is 1.0 ~ 4.0h.
9. the yacon oligofructose that method obtains according to claim arbitrary in claim 1-9.
10. yacon oligofructose according to claim 9, is characterized in that its oligofructose content is with described yacon oligofructose total weight more than 90%.
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