CN103483461B - Lip vanilla polyoses extract and preparation method thereof - Google Patents
Lip vanilla polyoses extract and preparation method thereof Download PDFInfo
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- CN103483461B CN103483461B CN201310381058.0A CN201310381058A CN103483461B CN 103483461 B CN103483461 B CN 103483461B CN 201310381058 A CN201310381058 A CN 201310381058A CN 103483461 B CN103483461 B CN 103483461B
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Abstract
<b> the present invention relates to vegetable polysaccharides technical field, it is a kind of lip vanilla polyoses extract and preparation method thereof, this lip vanilla polyoses extract obtains by following preparation method: the first step, after by lip vanilla and distilled water, 1:35</b><bGreatT .GreaT.GT to 1:45</b><bGreatT .GreaT.GT mixes in mass ratio, being 90</b><bGreatT.G reaT.GT DEG C in temperature, to carry 4</b><bGreatT.Gr eaT.GT to a 100</b><bGreatT. GreaT.GT DEG C Water Under little of 5</b><bGreatT.Gr eaT.GT hour, mixing solutions after water extraction is carried out filtering and collecting filtrate, filtrate being concentrated into quality is that the 20</b><bGreatT.G reaT.GT of lip vanilla quality doubly doubly obtains concentrated solution to 30</b><bGreatT.G reaT.GT, second step, by concentrated solution and sevage</b><bGrea tT.GreaT.GT reagent by volume 1:1</b><bGreatT. GreaT.GT to 1:1.5</b><bGreat T.GreaT.GT mix.The invention provides a kind of method extracted the polysaccharide of lip vanilla, compensate for lip vanilla polysaccharide and preparation method thereof still belongs to blank defect in vegetable polysaccharides field, for the later stage, the analysis of lip vanilla polysaccharide provides foundation.</b>
Description
Technical field
the present invention relates to vegetable polysaccharides technical field, is a kind of lip vanilla polyoses extract and preparation method thereof.
Background technology
lip vanilla (
ziziphoraclinopodioideslam.) be the dry aerial parts of Labiatae Folium Billbergiae platymiscium lip vanilla, call fragrant Folium Billbergiae, Herba Ziziphorae clinopodioidis, Herba Dracocephali etc., Uygur's name is called Su Ze---record in " Uygur medicine will " (first volume).Pungent, cool, the micro-hardship of lip vanilla nature and flavor, has effect of cardiac stimulant diuresis, activating QI to eliminate phlegm, diminishing inflammation and resolving masses.Lip vanilla polysaccharide is vegetable polysaccharides, at present, vegetable polysaccharides extracting method has sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction etc., by extracting lip vanilla polysaccharide with sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction, there is following defect in discovery: sour formulation can cause the fracture of glycosidic link in lip vanilla polysaccharide in acid condition, and acid can cause corrosion to container, therefore when extracting lip vanilla polysaccharide, need to carry out in specific installation, so just indirectly improve production cost; Alkaline extraction extracts lip vanilla polysaccharide soln denseer alkali taste, and solution colour, in yellow, can affect local flavor and the color and luster of finished product like this; Enzymolysis process cost is higher; Ultrasonic extraction extracts more abundant when extracting lip vanilla polysaccharide, but ultrasonic useful effect region is an annular, if the diameter of extractor is too large, central authorities will form ultrasonic clear area, ultrasonic cell is easily broken, make that extraction impurity is more, viscosity is excessive, not easily filter, therefore this extraction method should not carry out scale operation.
Summary of the invention
the invention provides a kind of lip vanilla polyoses extract and preparation method thereof, overcome the deficiency of above-mentioned prior art, it effectively can solve sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction when carrying out the extraction of lip vanilla polysaccharide, has that production cost is high, a poor product quality and should not carry out the problem of scale operation.
one of technical scheme of the present invention is realized by following measures: a kind of lip vanilla polyoses extract, obtain as follows: the first step, after by lip vanilla and distilled water, 1:35 to 1:45 mixes in mass ratio, be that 90 DEG C to 100 DEG C Water Unders are carried in temperature 4 little of 5 hours, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times of lip vanilla quality obtain concentrated solution to 30 times; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, under rotating speed is 130r/min to 140r/min condition, vibration carried out deproteinated process to 40 minutes in 25 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 to 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out under rotating speed is 3500r/min to 4000r/min condition centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
two of technical scheme of the present invention is realized by following measures: a kind of preparation method of lip vanilla polyoses extract, carry out in the steps below: the first step, after by lip vanilla and distilled water, 1:35 to 1:45 mixes in mass ratio, be that 90 DEG C to 100 DEG C Water Unders are carried in temperature 4 little of 5 hours, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times of lip vanilla quality obtain concentrated solution to 30 times; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, under rotating speed is 130r/min to 140r/min condition, vibration carried out deproteinated process to 40 minutes in 25 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 to 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out under rotating speed is 3500r/min to 4000r/min condition centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
here is the further optimization and/or improvements to foregoing invention technical scheme:
in the above-mentioned the first step, first lip vanilla powder is broken to and can crosses the Powdered of 40 mesh sieve to 80 mesh sieve, then carry out water extraction after pulverous lip vanilla and distilled water being mixed.
in above-mentioned second step, sevage reagent is trichloromethane and the propyl carbinol mixing solutions that mixes of 3:1 to 5:1 by volume.
in above-mentioned 3rd step, alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95%.
in above-mentioned 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
the present invention has higher yield compared to vegetable polysaccharides extracting method conventional at present, and meanwhile, the present invention extracts lip vanilla polysaccharide and do not need specific installation, and production technique cost is low, safety, is applicable to industrialized production; And the lip vanilla polysaccharide extracted according to embodiment of the present invention method under dissolved state color and luster clarification inclusion-free, for being brown color time solid-state, excellent flavor.
Embodiment
the present invention by the restriction of following embodiment, can not determine concrete embodiment according to technical scheme of the present invention and practical situation.
below in conjunction with embodiment, the invention will be further described:
embodiment 1, this lip vanilla polyoses extract obtains by following preparation method: the first step, after by lip vanilla and distilled water, 1:35 to 1:45 mixes in mass ratio, be that 90 DEG C to 100 DEG C Water Unders are carried in temperature 4 little of 5 hours, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times of lip vanilla quality obtain concentrated solution to 30 times; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, under rotating speed is 130r/min to 140r/min condition, vibration carried out deproteinated process to 40 minutes in 25 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 to 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out under rotating speed is 3500r/min to 4000r/min condition centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
embodiment 2, this lip vanilla polyoses extract obtains by following preparation method: the first step, after by lip vanilla and distilled water, 1:35 or 1:45 mixes in mass ratio, be that 90 DEG C or 100 DEG C of Water Unders carry 4 hours or 5 hours in temperature, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times or 30 times of lip vanilla quality obtain concentrated solution; Second step, after by concentrated solution and sevage reagent, 1:1 or 1:1.5 mixes by volume, under rotating speed is 130r/min or 140r/min condition, vibration carries out deproteinated process in 25 minutes or 40 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 or 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out centrifugal 4 minutes or 6 minutes under rotating speed is 3500r/min or 4000r/min condition, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
embodiment 3, is with the difference of above-described embodiment, is first broken to by lip vanilla powder and can crosses the Powdered of 40 mesh sieve to 80 mesh sieve, then carry out water extraction after pulverous lip vanilla and distilled water being mixed.
embodiment 4, preferred as above-described embodiment, in second step, sevage reagent is trichloromethane and the propyl carbinol mixing solutions that mixes of 3:1 to 5:1 by volume.
embodiment 5, preferred as above-described embodiment, in the 3rd step, alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95%.
embodiment 6, preferred as above-described embodiment, in the 4th step, is dried to constant weight and namely obtains lip vanilla polyoses extract under temperature is 60 DEG C of conditions by lip vanilla polysaccharide soln.
the present invention is water extraction and alcohol precipitation method, compared to extracting vegetable polysaccharides conventional sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction at present, according to the yield average out to 2.98% of the lip vanilla polysaccharide that embodiment of the present invention method is extracted, and the yield mean value of the lip vanilla polysaccharide adopting existing conventional vegetable polysaccharides extracting method to carry out extracting is 1.95%; Meanwhile, water extraction and alcohol precipitation method of the present invention is extracted in when extracting lip vanilla polysaccharide and does not need specific installation, and production technique cost is low, safety, is applicable to industrialized production; And the lip vanilla polysaccharide extracted according to embodiment of the present invention method under dissolved state color and luster clarification inclusion-free, for being brown color time solid-state, excellent flavor.
Claims (17)
1. a lip vanilla polyoses extract, it is characterized in that obtaining as follows: the first step, after by lip vanilla and distilled water, 1:35 to 1:45 mixes in mass ratio, be that 90 DEG C to 100 DEG C Water Unders are carried in temperature 4 little of 5 hours, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times of lip vanilla quality obtain concentrated solution to 30 times; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, under rotating speed is 130r/min to 140r/min condition, vibration carried out deproteinated process to 40 minutes in 25 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 to 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out under rotating speed is 3500r/min to 4000r/min condition centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
2. lip vanilla polyoses extract according to claim 1, is characterized in that in the first step, is first broken to by lip vanilla powder and can crosses the Powdered of 40 mesh sieve to 80 mesh sieve, then carry out water extraction after pulverous lip vanilla and distilled water being mixed.
3. lip vanilla polyoses extract according to claim 1 and 2, is characterized in that in second step, and sevage reagent is trichloromethane and the propyl carbinol mixing solutions that mixes of 3:1 to 5:1 by volume.
4. lip vanilla polyoses extract according to claim 1 and 2, in the third step, alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95% to its feature.
5. lip vanilla polyoses extract according to claim 3, in the third step, alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95% to its feature.
6. lip vanilla polyoses extract according to claim 1 and 2, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
7. lip vanilla polyoses extract according to claim 3, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
8. lip vanilla polyoses extract according to claim 4, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
9. the preparation method of a lip vanilla polyoses extract, it is characterized in that carrying out in the steps below: the first step, after by lip vanilla and distilled water, 1:35 to 1:45 mixes in mass ratio, be that 90 DEG C to 100 DEG C Water Unders are carried in temperature 4 little of 5 hours, carried out filtering and collecting filtrate by mixing solutions after water extraction, filtrate being concentrated into quality is that 20 times of lip vanilla quality obtain concentrated solution to 30 times; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, under rotating speed is 130r/min to 140r/min condition, vibration carried out deproteinated process to 40 minutes in 25 minutes, after vibration terminates, mixing solutions is carried out stratification, leave standstill to after bed interface is clear, after discarding upper strata sevage layer, leave lower floor's feed liquid layer; 3rd step, in feed liquid layer, 1:4 to 1:5 adds alcohol precipitation solvent and carries out alcohol precipitation by volume, alcohol is sink in solution to generate without brown floss again and namely obtains alcohol precipitation mixing solutions, alcohol precipitation mixing solutions is carried out under rotating speed is 3500r/min to 4000r/min condition centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layers and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layers and obtains lip vanilla polysaccharide soln; 4th step, namely obtains lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
10. the preparation method of lip vanilla polyoses extract according to claim 9, it is characterized in that in the first step, first lip vanilla powder is broken to and can crosses the Powdered of 40 mesh sieve to 80 mesh sieve, then carry out water extraction after pulverous lip vanilla and distilled water being mixed.
The preparation method of 11. lip vanilla polyoses extracts according to claim 9 or 10, is characterized in that in second step, and sevage reagent is trichloromethane and the propyl carbinol mixing solutions that mixes of 3:1 to 5:1 by volume.
The preparation method of 12. lip vanilla polyoses extracts according to claim 9 or 10, it is characterized in that in the 3rd step, alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95%.
The preparation method of 13. lip vanilla polyoses extracts according to claim 11, is characterized in that in the 3rd step, and alcohol precipitation solvent is dehydrated alcohol or mass concentration is the aqueous ethanolic solution of 95%.
The preparation method of 14. lip vanilla polyoses extracts according to claim 9 or 10, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
The preparation method of 15. lip vanilla polyoses extracts according to claim 11, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
The preparation method of 16. lip vanilla polyoses extracts according to claim 12, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
The preparation method of 17. lip vanilla polyoses extracts according to claim 13, is characterized in that in the 4th step, lip vanilla polysaccharide soln is dried under temperature is 60 DEG C of conditions constant weight and namely obtains lip vanilla polyoses extract.
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| CN107556398A (en) * | 2017-09-19 | 2018-01-09 | 李仲昆 | A kind of wall fern polyoses extract and preparation method thereof |
| CN107501431A (en) * | 2017-09-19 | 2017-12-22 | 李仲昆 | A kind of water-soluble giant knotweed polyoses extract and preparation method thereof and purposes |
| CN107383232A (en) * | 2017-09-20 | 2017-11-24 | 李仲昆 | A kind of ching-chieh polyoses extract and preparation method thereof and purposes |
| CN107501433A (en) * | 2017-09-20 | 2017-12-22 | 李仲昆 | A kind of polygonum flaccidum polyoses extract and preparation method thereof and purposes |
| CN107501432A (en) * | 2017-09-20 | 2017-12-22 | 李仲昆 | A kind of gold thread grass polysaccharide extract and preparation method thereof and purposes |
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| CN101235097A (en) * | 2008-02-29 | 2008-08-06 | 武汉大学 | Method for extracting polysaccharide from angelica and application thereof |
| JP2011116850A (en) * | 2009-12-02 | 2011-06-16 | T Hasegawa Co Ltd | Method for producing vanilla extract |
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