CN103483461A - Ziziphora clinopodioides polysaccharide extract and preparation method thereof - Google Patents
Ziziphora clinopodioides polysaccharide extract and preparation method thereof Download PDFInfo
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- CN103483461A CN103483461A CN201310381058.0A CN201310381058A CN103483461A CN 103483461 A CN103483461 A CN 103483461A CN 201310381058 A CN201310381058 A CN 201310381058A CN 103483461 A CN103483461 A CN 103483461A
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Abstract
The invention relates to the technical field of plant polysaccharide, and discloses a Ziziphora clinopodioides polysaccharide extract and a preparation method thereof. The Ziziphora clinopodioides polysaccharide extract is prepared by the following preparation method: 1, mixing Ziziphora clinopodioides with distilled water according to the mass ratio of (1:35) to (1:45), and then carrying out water extraction for 4-5 hours at the temperature of 90-100 DEG C, filtering the mixed solution after water extraction and collecting filtrate, and concentrating the filtrate to be 20-30 folds of mass of the Ziziphora clinopodioides, so as to obtain concentrated solution; 2, mixing the concentrated solution with a sevage reagent according to the volume ratio of (1:1) to (1:1.5). The invention provides a method for extracting the Ziziphora clinopodioides polysaccharide, so that the defect that the Ziziphora clinopodioides polysaccharide and the preparation method thereof are still blank in the field of plant polysaccharide is compensated; a foundation is provided for later analysis of the Ziziphora clinopodioides polysaccharide.
Description
Technical field
the present invention relates to the vegetable polysaccharides technical field, is a kind of lip vanilla polyoses extract and preparation method thereof.
Background technology
the lip vanilla (
ziziphora clinopodioideslam.) 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).Hot, cool, the micro-hardship of lip vanilla nature and flavor, have the effect of cardiac stimulant diuresis, activating QI to eliminate phlegm, diminishing inflammation and resolving masses.Lip vanilla polysaccharide is vegetable polysaccharides, at present, the vegetable polysaccharides extracting method has sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction etc., by with sour formulation, alkaline extraction, enzymolysis process and ultrasonic extraction, lip vanilla polysaccharide being extracted, there is following defect in discovery: sour formulation can cause the fracture of glycosidic link in lip vanilla polysaccharide under acidic conditions, and acid can cause corrosion to container, therefore when extracting lip vanilla polysaccharide, need in specific installation, carry out, so just indirectly improve production cost; Alkaline extraction extracts lip vanilla polysaccharide soln denseer alkali flavor, and it is yellow that solution colour is, and can affect like this local flavor and the color and luster of finished product; The enzymolysis process cost is higher; Ultrasonic extraction extracts more abundant when extracting lip vanilla polysaccharide, but ultrasonic useful effect zone is an annular, if the diameter of extractor is too large, central authorities will form ultrasonic clear area, ultrasonic cell is easily broken, make to extract that impurity is more, viscosity is excessive, be difficult for filtering, so this extraction method should not be carried 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 can effectively 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, poor product quality and the problem that should not carry out scale operation.
one of technical scheme of the present invention realizes 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, in temperature, be that 90 ℃ to 100 ℃ Water Unders are carried 4 hours to 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times to 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, at rotating speed, be that under 130r/min to 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes to 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to in the feed liquid layer by volume 1:4 to 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min to 4000r/min condition, to carry out centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
two of technical scheme of the present invention realizes 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, in temperature, be that 90 ℃ to 100 ℃ Water Unders are carried 4 hours to 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times to 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, at rotating speed, be that under 130r/min to 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes to 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to in the feed liquid layer by volume 1:4 to 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min to 4000r/min condition, to carry out centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
below the further optimization and/or improvements to the foregoing invention technical scheme:
in the above-mentioned the first step, first the 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 are mixed.
in above-mentioned second step, sevage reagent is trichloromethane and the propyl carbinol mixing solutions that 3:1 to 5:1 mixes by volume.
in above-mentioned the 3rd step, the alcohol precipitation solvent is the aqueous ethanolic solution that dehydrated alcohol or mass concentration are 95%.
in above-mentioned the 4th step, by lip vanilla polysaccharide soln, in temperature, be to be dried to constant weight under 60 ℃ of conditions to obtain lip vanilla polyoses extract.
the present invention has higher yield than current vegetable polysaccharides extracting method commonly used, and simultaneously, the present invention extracts lip vanilla polysaccharide and do not need specific installation, and the production technique cost is low, and safety is applicable to industrialized production; And the lip vanilla polysaccharide extracted according to embodiment of the present invention method color and luster under dissolved state is clarified inclusion-free, is brown color, excellent flavor while being solid-state.
Embodiment
the present invention is not subject to the restriction of following embodiment, can 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, in temperature, be that 90 ℃ to 100 ℃ Water Unders are carried 4 hours to 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times to 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, at rotating speed, be that under 130r/min to 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes to 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to in the feed liquid layer by volume 1:4 to 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min to 4000r/min condition, to carry out centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain 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 mix in mass ratio, in temperature, be that 90 ℃ or 100 ℃ of Water Unders are carried 4 hours or 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times or 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 or 1:1.5 mix by volume, at rotating speed, be that under 130r/min or 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes or 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to 1:4 or 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation by volume in the feed liquid layer, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min or 4000r/min condition, to carry out centrifugal 4 minutes or 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
embodiment 3, with the difference of above-described embodiment, are, first the lip vanilla powder are broken to and can cross the Powdered of 40 mesh sieve to 80 mesh sieve, then carry out water extraction after pulverous lip vanilla and distilled water are mixed.
embodiment 4, as above-described embodiment preferably, in second step, sevage reagent is trichloromethane and the propyl carbinol mixing solutions that 3:1 to 5:1 mixes by volume.
embodiment 5, as above-described embodiment preferably, in the 3rd step, the alcohol precipitation solvent is the aqueous ethanolic solution that dehydrated alcohol or mass concentration are 95%.
embodiment 6, as above-described embodiment preferably, in the 4th step, by lip vanilla polysaccharide soln, in temperature, be to be dried to constant weight under 60 ℃ of conditions to obtain lip vanilla polyoses extract.
the present invention is water extraction and alcohol precipitation method, sour formulation, alkaline extraction, enzymolysis process and the ultrasonic extraction than current extraction vegetable polysaccharides, commonly used, the yield average out to 2.98% of the lip vanilla polysaccharide extracted according to embodiment of the present invention method, and the yield mean value of the lip vanilla polysaccharide that adopts existing vegetable polysaccharides extracting method commonly used to be extracted is 1.95%; Simultaneously, water extraction and alcohol precipitation method of the present invention is extracted in while extracting lip vanilla polysaccharide and does not need specific installation, and the production technique cost is low, and safety is applicable to industrialized production; And the lip vanilla polysaccharide extracted according to embodiment of the present invention method color and luster under dissolved state is clarified inclusion-free, is brown color, excellent flavor while being solid-state.
Claims (10)
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, in temperature, be that 90 ℃ to 100 ℃ Water Unders are carried 4 hours to 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times to 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, at rotating speed, be that under 130r/min to 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes to 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to in the feed liquid layer by volume 1:4 to 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min to 4000r/min condition, to carry out centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain 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, first the 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 are 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 3:1 to 5:1 mixes by volume.
4. according to claim 1 or 2 or 3 described lip vanilla polyoses extracts, its feature is in the 3rd step, and the alcohol precipitation solvent is the aqueous ethanolic solution that dehydrated alcohol or mass concentration are 95%.
5. according to claim 1 or 2 or 3 or 4 described lip vanilla polyoses extracts, it is characterized in that in the 4th step, is to be dried to constant weight under 60 ℃ of conditions to obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln in temperature.
6. 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, in temperature, be that 90 ℃ to 100 ℃ Water Unders are carried 4 hours to 5 hours, mixing solutions after water extraction is filtered and collect filtrate, and it is that 20 times to 30 times of lip vanilla quality obtain concentrated solution that filtrate is concentrated into to quality; Second step, after by concentrated solution and sevage reagent, 1:1 to 1:1.5 mixes by volume, at rotating speed, be that under 130r/min to 140r/min condition, the deproteinated processing is carried out in vibration in 25 minutes to 40 minutes, after vibration finishes, mixing solutions is carried out to stratification, standing to after bed interface is clear, stay lower floor's feed liquid layer after discarding upper strata sevage layer; The 3rd step, to in the feed liquid layer by volume 1:4 to 1:5 add the alcohol precipitation solvent to carry out alcohol precipitation, alcohol is sink in solution and generates and obtain the alcohol precipitation mixing solutions without brown floss again, by the alcohol precipitation mixing solutions, at rotating speed, be under 3500r/min to 4000r/min condition, to carry out centrifugal 4 minutes to 6 minutes, the layering of centrifugal rear alcohol precipitation mixing solutions obtains lip vanilla polysaccharide layer and alcohol precipitation solvent layer, then carries out separated and collected lip vanilla polysaccharide layer and obtains lip vanilla polysaccharide soln; The 4th step, obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln being dried to constant weight.
7. the preparation method of lip vanilla polyoses extract according to claim 6, it is characterized in that in the first step, first the 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 are mixed.
8. according to the preparation method of the described lip vanilla of claim 6 or 7 polyoses extract, it is characterized in that in second step, sevage reagent is trichloromethane and the propyl carbinol mixing solutions that 3:1 to 5:1 mixes by volume.
9. according to the preparation method of claim 6 or 7 or 8 described lip vanilla polyoses extracts, it is characterized in that in the 3rd step, the alcohol precipitation solvent is the aqueous ethanolic solution that dehydrated alcohol or mass concentration are 95%.
10. according to the preparation method of claim 6 or 7 or 8 or 9 described lip vanilla polyoses extracts, it is characterized in that in the 4th step, is to be dried to constant weight under 60 ℃ of conditions to obtain lip vanilla polyoses extract by lip vanilla polysaccharide soln in temperature.
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Cited By (5)
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| 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 |
| 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 |
| 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 |
| CN107556398A (en) * | 2017-09-19 | 2018-01-09 | 李仲昆 | A kind of wall fern polyoses extract and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN107556398A (en) * | 2017-09-19 | 2018-01-09 | 李仲昆 | A kind of wall fern polyoses extract and preparation method thereof |
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| 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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