CN107556400A - It is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method - Google Patents
It is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method Download PDFInfo
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- CN107556400A CN107556400A CN201710956930.8A CN201710956930A CN107556400A CN 107556400 A CN107556400 A CN 107556400A CN 201710956930 A CN201710956930 A CN 201710956930A CN 107556400 A CN107556400 A CN 107556400A
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Abstract
The invention discloses it is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method, belong to extraction polysaccharide preparation field.The preparation method comprises the following steps：Wintercherry is cleaned, be beaten, dry, 60 mesh sieves are crossed after crushing, obtains wintercherry powder；After the supersound process of different condition, centrifugation, supernatant is polysaccharide extraction liquid.Pass through single factor experiment, the most suitable liquid ratio for extracting wintercherry polysaccharide, ultrasonic temperature, ultrasonic time, ultrasonic power is determined, obtained polysaccharide carries out sevage methods and carries out de- albumen, pass through single factor experiment, the volume ratio of the final most suitable sample liquid sevage reagents that purified polysaccharide is determined, the volume ratio of chloroform n-butanol, the time is shaken, take off albumen number.Hydrogen peroxide method decolourizes, and by single factor experiment, most suitable bleaching temperature, solution ph, bleaching time, hydrogen peroxide addition is finally determined.
Description
Technical field
The present invention relates to it is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method, belong to extraction polysaccharide preparation
Field, and albumen is taken off using sevage methods, hydrogen peroxide decoloring method carries out the purifying of polysaccharide.
Background technology
Wintercherry is plant of Solanaceae, is divided into red acid slurry and yellow acid starches two kinds.Red acid slurry is also known as wintercherry fruit or calyx, franchet groundcherry persistent calyx or fruit, fruit
For spheroidal, berry is orange red when ripe, has the calyx expanded outside such as lantern-shaped is loose is enclosed in outside berry.The traditional Chinese medical science is recognized
For its nature and flavor slight bitter, return lung warp, there is the effect of clearing heat and detoxicating, relieving sore-throat resolving sputum, diuresis.And among the people also spread in China is controlled with wintercherry
Diabetes are treated, there is the effect of preferably hypoglycemic.At present, research and development and application of the China to wintercherry are also in starting rank
Section, it is also less to the overall research of wintercherry, therefore the research tool to red acid slurry is of great significance.
Polysaccharide is the high-molecular compound formed by more than 10 monosaccharide molecules by dehydrating condensation, and polysaccharide is a kind of natural
Macromolecular substances, it is prevalent among animals and plants, is one of four big base substances for forming life, in the balance of physiological function
With important regulatory function is played in stabilization process.Research has shown that polysaccharide has obvious enhancing body immunity and suppression
The effect of tumour processed, hypoglycemic and preventing and treating diabetes effect, reducing blood lipid, anticoagulant, anti thrombotic action, strengthens body's immunity
The generation of the cell factors such as interferon, TNF can also be promoted.
Wintercherry Polyose extraction can use hot water, diluted acid, diluted alkaline also to use ultrasonic extraction method as digestion agent.Leaching
Formulation is to extract the conventional method of wintercherry polysaccharide, but the time is long, efficiency is low, energy consumption is big, in addition under the conditions of diluted acid, diluted alkaline, easily
Make polysaccharide that the fracture of glycosidic bond occur, par-tial polysaccharide occurs hydrolysis and reduces the recovery rate of polysaccharide, therefore the recovery rate of polysaccharide
It is universal not high.Ultrasonic extraction method polysaccharide simple and fast, time saving low consumption, industrialization extraction and production to wintercherry polysaccharide have non-
Often important realistic meaning.
The content of the invention
It is an object of the invention to provide a kind of using ultrasonic wave extraction and the method for purifying wintercherry polysaccharide, extraction side of the invention
Method extracts wintercherry polysaccharide using supercritical ultrasonics technology, and extraction conditions are optimized, and takes off albumen, hydrogen peroxide with sevage methods
Method is decolourized, and preparation-obtained wintercherry polysaccharide properties are stable.
The purpose of the present invention is achieved through the following technical solutions：
It is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method, wintercherry polysaccharide is extracted using supercritical ultrasonics technology, wrap
Include following steps：
Wintercherry is cleaned, be beaten, dry, crush, crosses 60 mesh sieves, obtains wintercherry powder；Ultrasound Jing Guo different condition again
After processing, centrifugation, supernatant is polysaccharide extraction liquid.
The present invention have studied under different liquid ratios, ultrasonic time, ultrasonic temperature, ultrasonic power conditions, more to wintercherry
The influence of sugared recovery rate.According to result of the test, optimal horizontal combination is determined.
Drawn by single factor experiment, obtaining optimum process condition is：50 DEG C of ultrasonic temperature, ultrasonic power 280W,
Sonication times 30min, liquid ratio 25：When 1 (mL/g), the wintercherry polysaccharide extract rate obtained on this condition is maximum.
Sevage methods take off albumen and have studied sample liquid-sevage reagent volume ratios, chloroform and n-butanol volume ratio, during shaking
Between, take off influence of the albumen number to removal of protein rate and polysaccharide retention rate.According to result of the test, optimal horizontal group is determined
Close.
Drawn by single factor experiment, obtaining optimum process condition is：Sample liquid-sevage reagent volumes are than 5:1, chloroform with
N-butanol volume ratio 4:1, time 30min is shaken, takes off albumen number 3 times.
Hydrogen peroxide decoloring method have studied bleaching temperature, and solution ph, bleaching time, hydrogen peroxide addition is to percent of decolourization
With the influence of polysaccharide retention rate.According to result of the test, optimal horizontal combination is determined.
Drawn by single factor experiment, obtaining optimum process condition is：50 DEG C of bleaching temperature, pH value of solution 8, bleaching time
4h, hydrogen peroxide addition 50%.
Brief description of the drawings
Influence of Fig. 1 liquid ratios to wintercherry polysaccharide extract rate；
Influence of Fig. 2 sonication times to wintercherry polysaccharide extract rate；
Influence of Fig. 3 ultrasonic temperatures to wintercherry polysaccharide extract rate；
Influence of Fig. 4 ultrasonic powers to wintercherry polysaccharide extract rate；
The influence of Fig. 5 sample liquid-sevage reagent volume aligned protein removal efficiencies and polysaccharide retention rate；
Fig. 6 chloroforms and influence of the n-butanol volume ratio to removal of protein rate and polysaccharide retention rate；
Fig. 7 shakes influence of the time to removal of protein rate and polysaccharide retention rate；
Fig. 8 takes off influence of the albumen number to removal of protein rate and polysaccharide retention rate；
Influence of Fig. 9 bleaching temperatures to percent of decolourization and polysaccharide retention rate；
Influence of Figure 10 pH value of solution to percent of decolourization and polysaccharide retention rate；
Influence of Figure 11 bleaching times to percent of decolourization and polysaccharide retention rate；
Influence of Figure 12 hydrogen peroxide addition to percent of decolourization and polysaccharide retention rate；
Embodiment
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
First, the preparation of wintercherry powder
It is beaten, dries after wild wintercherry is cleaned, 60 mesh sieves is crossed after being crushed with pulverizer, obtain wintercherry powder, it is standby.
1st, single factor experiment designs
Liquid ratio (20 is investigated respectively:1、25:1、30:1、35:1、40:1), ultrasonic temperature (35,40,45,50,55 DEG C),
Ultrasonic power (160,200,240,280,320W) and ultrasonic time (10,20,30,40,50min) etc. 4 factors it is more to wintercherry
The influence of sugared recovery rate.
2nd, experiment of single factor
1st, influence of the liquid ratio to wintercherry polysaccharide extract rate
As shown in figure 1, work as liquid ratio from 20：1 increases to 25：When 1, the recovery rate of wintercherry polysaccharide can be raised significantly, from 3.8%
Increase to 5.9%；When liquid ratio continues to increase, the recovery rate of polysaccharide reduces on the contrary, therefore selects 25：1 as wintercherry polysaccharide
Optimal liquid ratio.
2nd, influence of the ultrasonic time to wintercherry polysaccharide extract rate
From figure 2 it can be seen that when ultrasonic time increases to 30min from 10min, polysaccharide extract rate increases from 4.3%
To 5.5%, the recovery rate of wintercherry polysaccharide raises；And when ultrasonic time continues increase, polysaccharide extract rate declines on the contrary, therefore selects
Select optimal ultrasonic times of the 30min as extraction wintercherry polysaccharide.
3rd, influence of the ultrasonic temperature to wintercherry polysaccharide extract rate
From figure 3, it can be seen that when temperature is from when being increased to 50 DEG C for 35 DEG C, the recovery rate of wintercherry polysaccharide increases from 3.8%
To 4.9%,；When temperature continues to raise, the recovery rate of wintercherry polysaccharide can be remarkably decreased, therefore select 50 DEG C to be used as extraction wintercherry more
The optimal ultrasonic temperature of sugar.
4th, influence of the ultrasonic power to wintercherry polysaccharide extract rate
Figure 4, it is seen that when ultrasonic power increases to 280W from 160W, polysaccharide extract rate increases to from 3.7%
5.3%, the increase of wintercherry polysaccharide extract rate；But if ultrasonic power continues to increase, polysaccharide extract rate reduces, therefore selects 280W to make
To extract the optimal ultrasonic power of wintercherry polysaccharide.
According to the result of single factor test, the best of breed of wintercherry Polyose extraction is determined, draws the optimum extraction work of wintercherry polysaccharide
Skill：Liquid ratio 25：1 (mL/g), 50 DEG C of ultrasonic temperature, ultrasonic power 280W, ultrasonic time 30min.In order to verify the experiment
Accuracy, proving test is carried out to polysaccharide extract rate, parallel test 3 times, the average value of recovery rate is 5.2%.
5th, the influence of sample liquid and sevage reagent volume aligned protein removal efficiencies and polysaccharide retention rate
From fig. 5, it can be seen that with sample liquid-sevage reagent volumes than increase, albumen removal efficiency and polysaccharide retention rate
Dramatically increase.When sample liquid-sevage reagent volume ratios reach 5：When 1, albumen removal efficiency is maximum, is 63.42%, while polysaccharide
Retention rate is 87.23%；When ratio continues increase, albumen removal efficiency is begun to decline, although working as sample liquid-sevage reagent volumes
Than for 6：Polysaccharide retention rate is maximum when 1, is 87.98%.But the results of analysis of variance shows, this two groups of data variances do not show
Write, accordingly, it is considered to the influence of albumen effect is taken off to polysaccharide to two indices, the optimal sample liquid-sevage reagents that this experiment is selected
Volume ratio is 5：1.
6th, chloroform-influence of the n-butanol volume ratio to removal of protein rate and polysaccharide retention rate
From fig. 6 it can be seen that with the increase of chloroform-n-butanol volume ratio, albumen removal efficiency is during this period with body
Accumulate the increase of ratio and increase；The polysaccharide retention rate also increase increase trend in direct ratio with volume ratio simultaneously.When chloroform-n-butanol
Volume ratio reaches 4：When 1, albumen removal efficiency is 60.69%, while polysaccharide retention rate is 88.87%；When ratio continues to be increased to
5：When 1, albumen removal efficiency and polysaccharide retention rate have increased slightly, and respectively 61.2% and 89.32%, although working as chloroform-positive fourth
Alcohol volume ratio is 5：Albumen removal efficiency and polysaccharide retention rate are maximum when 1, but compared with chloroform-n-butanol volume ratio 4：When 1, albumen takes off
Except rate and polysaccharide retention rate increase only 0.85% and 0.50%.The results of analysis of variance shows that this two groups of data variances do not show
Write, accordingly, it is considered to the influence of albumen effect is taken off to polysaccharide to two indices, optimal chloroform-n-butanol volume that this experiment is selected
Than for 4：1.
7th, influence of the time to removal of protein rate and polysaccharide retention rate is shaken
It can be seen from figure 7 that with the increase of shaking time, when albumen removal efficiency and polysaccharide retention rate are all with shaking
Between increase and increase.When the shaking time reaching 30min, albumen removal efficiency increases with the increase of shaking time during this period
Greatly, maximum 64.21%；Increase of the polysaccharide retention rate also to shaking the time simultaneously is directly proportional, is 89.78%；When shaking
Between continue to increase, albumen removal efficiency has increased slightly, when shake the time be 50min when polysaccharide retention rate it is maximum, for 90.54%, this
When albumen removal efficiency be 65.21%, but and shake the time compared for 30min, polysaccharide retention rate only increases 0.85%.Side
Poor analysis result shows that this two groups of data variances are not notable, therefore, considers albumen removal efficiency and polysaccharide retention rate at the same time
In the case of, the optimal shaking time that this experiment is selected is 30min.
8th, influence of the albumen number to removal of protein rate and polysaccharide retention rate is taken off
From figure 8, it is seen that with the increase of removing protein number, albumen removal efficiency gradually increases, and polysaccharide retention rate is gradual
Reduce, reason is probably：Polysaccharide solution easily forms a kind of gel after the organic reagents such as chloroform, n-butanol repeatedly processing
Material, also cause the reduction of polysaccharide retention rate there is a small amount of polysaccharide material among these.From the result of variance analysis, remove
Albumen once, it is secondary, notable with albumen removal efficiency otherness at four times three times, albumen removal efficiency is poor during removing protein four times and five times
The opposite sex is not notable；Meanwhile removing protein it is secondary, three times when polysaccharide retention rate otherness it is not notable, then difference between three groups of experiments
Property is notable.Economically consider, can not only save the use of test material, save the time but also can to obtain substantial amounts of purifying more
Sugar.Therefore, in the case of considering albumen removal efficiency and polysaccharide retention rate at the same time, this experiment uses de- albumen number as three times.
9th, influence of the bleaching temperature to percent of decolourization and polysaccharide retention rate
From fig. 9, it can be seen that when bleaching temperature is gradually increased to 50 DEG C from 40 DEG C, the percent of decolourization and polysaccharide of wintercherry polysaccharide
Retention rate increases with the rise of temperature, but not notable by the ascendant trend of polysaccharide retention rate at 45 DEG C to 50 DEG C,
From the point of view of variance analysis, otherness is not notable.When bleaching temperature continues rise by 50 DEG C, percent of decolourization ascendant trend does not show
Write, polysaccharide retention rate declines with the rise of temperature.Therefore, the situation of albumen removal efficiency and polysaccharide retention rate is considered at the same time
Under, the optimal bleaching temperature of this experiment is 50 DEG C.
10th, influence of the pH value of solution to percent of decolourization and polysaccharide retention rate
From fig. 10 it can be seen that with the increase of solution ph, under the percent of decolourization of wintercherry polysaccharide solution occurs after first increasing
The trend of drop, when pH is 8.0, percent of decolourization reaches maximum, is 70.42%；And polysaccharide retention rate and pH increase are inversely proportional
Example, and seen by the result of variance analysis, five groups of pH value are respectively provided with significant difference.This is probably due in alkaline environment on the weak side
Under, hydrogen peroxide decolourizes to be adapted to the most.Continue to increase with pH value, wintercherry polysaccharide can degrade under alkaline environment, make
Polysaccharide retention rate declines.Therefore, in the case of considering percent of decolourization and polysaccharide retention rate at the same time, optimal pH value of solution is selected in this experiment
It is worth for 8.0.
11st, influence of the bleaching time to percent of decolourization and polysaccharide retention rate
It can be seen from figure 11 that when bleaching time is from during 1h increases to 4h, the percent of decolourization increase of wintercherry polysaccharide solution
And otherness is notable, when bleaching time is from during 4h increases to 5h, percent of decolourization is increased over time and gradually increased but poor
The opposite sex is not notable；With the increase of bleaching time, polysaccharide retention rate is gradually reduced, from the result of variance analysis, during decolouring
Between when being 1h and 2h, polysaccharide retention rate otherness is not notable, during bleaching time 2h, 3h, 4h and 5h, polysaccharide retention rate otherness
Significantly；This is probably not dissolved fully initial stage in decolouring because of hydrogen peroxide, with the progress of decolouring, having in wintercherry polysaccharide
Color substance and then by fully degraded；Decolourize more long, the decoloring ability of hydrogen peroxide more tends to the limit.Prolonged hydrogen peroxide takes off
Color can cause the degraded of polysaccharide, and so as to cause polysaccharide retention rate to decline, the operation cycle is extended.Therefore, consider to decolourize at the same time
In the case of rate and polysaccharide retention rate, this experiment is 4h from optimal bleaching time.
12nd, influence of the hydrogen peroxide addition to percent of decolourization and polysaccharide retention rate
It can be recognized from fig. 12 that work as H2O2Addition is from during 20% increases to 50%, the percent of decolourization of Armillariella mellea polysaccharide solution
Increase and otherness is notable, work as H2O2From during 50% increases to 60%, percent of decolourization declines addition.In whole course of reaction
In, polysaccharide retention rate and H in wintercherry polysaccharide solution2O2The increase of addition is inversely proportional, and otherness is notable.In hydrogen peroxide
The fracture of peroxide bridge produces a large amount of free radicals, and the free radical reacts with coloring matter, is oxidized coloring matter, loses original
Some colors.When content of hydrogen peroxide is excessive in solution, unit volume hydrogen peroxide tends to the oxidation of coloring matter
Saturation.If the concentration for now continuing increase hydrogen peroxide may result in the degraded of polysaccharide.Therefore, at the same time consider percent of decolourization and
In the case of polysaccharide retention rate, optimal H is selected in this experiment2O2Addition is 50%.
Claims (5)
1. it is a kind of using ultrasonic wave extraction and purify wintercherry polysaccharide method, it is characterised in that methods described step is as follows：Step
One：Wild wintercherry is cleaned into mashing, drying, pulverizer crushing, wintercherry powder is made；Step 2：By water and wintercherry powder according to
Different liquid ratios (20:1、25:1、30:1、35:1、40:1) mix；Step 3：Solution after above-mentioned processing is used super
Sonication, ultrasonic temperature (35,40,45,50,55 DEG C), ultrasonic power (160,200,240,280,320W) and ultrasonic time
(10,20,30,40,50min), centrifuge afterwards, supernatant is wintercherry polysaccharide extraction liquid.Step 4：Polysaccharide extraction liquid is taken according to sample
Liquid and sevage reagent volumes ratio (2:1、3：1、4:1、5:1、6:1), chloroform-n-butanol volume ratio (2:1、3：1、4:1、5:1、
6:1), shake the time (10,20,30,40,50min), de- albumen number (1,2,3,4,5) carries out de- albumen, step 5：According to
Bleaching temperature (35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C), solution ph (5,6,7,8,9), bleaching time (1,2,3,4,5h),
Hydrogen peroxide addition (20%, 30%, 40%, 50%, 60%) is decolourized.
2. according to the preparation method described in claim 1, it is characterised in that the liquid ratio of the solution described in step 2 is 25：1.
3. according to the preparation method described in claim 1, it is characterised in that the ultrasonic temperature of the solution described in step 3 is 50
DEG C, ultrasonic time 30min, ultrasonic power 280W.
4. according to the preparation method described in claim 1, it is characterised in that sample liquid and sevage reagents described in step 4
Volume ratio is 5:1st, the volume ratio of chloroform-n-butanol is 4:1st, the shaking time be 30min, de- albumen number be 3 times.
5. according to the preparation method described in claim 1, it is characterised in that the bleaching temperature described in step 5 is 50 DEG C, solution
PH value is 8, bleaching time 4h, hydrogen peroxide addition are 50%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110558416A (en) * | 2019-09-24 | 2019-12-13 | 商洛学院 | Throat clearing buccal tablet and preparation method thereof |
| CN110596074A (en) * | 2019-09-19 | 2019-12-20 | 广西科技大学 | Dynamics research method for sucrose hydrolysis reaction process |
-
2017
- 2017-10-16 CN CN201710956930.8A patent/CN107556400A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110596074A (en) * | 2019-09-19 | 2019-12-20 | 广西科技大学 | Dynamics research method for sucrose hydrolysis reaction process |
| CN110596074B (en) * | 2019-09-19 | 2022-04-15 | 广西科技大学 | Dynamics research method for sucrose hydrolysis reaction process |
| CN110558416A (en) * | 2019-09-24 | 2019-12-13 | 商洛学院 | Throat clearing buccal tablet and preparation method thereof |
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