CN110563854A - Method for extracting polygonatum polysaccharide - Google Patents
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- CN110563854A CN110563854A CN201910673565.9A CN201910673565A CN110563854A CN 110563854 A CN110563854 A CN 110563854A CN 201910673565 A CN201910673565 A CN 201910673565A CN 110563854 A CN110563854 A CN 110563854A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
the invention discloses a process for extracting polygonatum polysaccharide under the assistance of ultrasonic waves, which comprises the following steps: step 1: screening, cleaning and slicing polygonatum longstem, and grinding into powder; step 2: adding the long-stem fine yellow powder into a round-bottom flask, adding petroleum ether, heating and refluxing for extraction for 0.5-1 h, filtering, refluxing and extracting filter residues for 1-2 h at 70 ℃ by using 95% ethanol, and air-drying to obtain a sample. And step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 30-70 min at room temperature by using an ultrasonic extractor, standing and layering after ultrasonic treatment, extracting supernatant, mixing lower-layer precipitates with 3 times of 70% ethanol, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution; and 4, step 4: extracting the concentrated solution with chloroform-n-butanol for 2-3 times, separating liquid, adding active carbon into the upper layer liquid for decolorization, and performing suction filtration; and 5: filtering the filtrate, centrifuging to obtain filter cake, and washing with 95% ethanol, anhydrous ethanol, and diethyl ether respectively once to obtain refined rhizoma Polygonati polysaccharide product.
Description
Technical Field
The invention belongs to the technical field of extraction of polygonatum polysaccharide, and particularly relates to a method for extracting polygonatum polysaccharide.
background
Rhizoma Polygonati is dried rhizome of Polygonatum kingianum, Polygonatum kingianum or Polygonatum cyrtonema of Polygonatum of Liliaceae, is a traditional Chinese medicine in China, and belongs to Chinese herbal medicine with homology of medicine and food. The product is sweet and neutral in nature, and has effects of invigorating spleen, replenishing qi, invigorating spleen, moistening lung, invigorating kidney, and strengthening bone. Mainly contains many components such as rhizoma Polygonati polysaccharide, saponin, nicotinic acid, quinones, amino acids and microelements, and has various pharmacological actions such as delaying aging, enhancing immunity, regulating blood lipid, lowering blood sugar, and resisting tumor. The polysaccharide is a main active ingredient, and has remarkable human body immunological activity, anti-tumor effect, anti-aging, antibacterial, anti-atherosclerosis, blood sugar and blood lipid regulating effects. According to the characteristics of solubility and the like, the extraction and separation methods for extracting polygonatum polysaccharide at present comprise hot water extraction, alcohol separation, microwave-assisted extraction and the like. However, the above extraction and separation method has low extraction efficiency and low yield.
disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting polygonatum polysaccharide.
In order to achieve the purpose, the invention is realized by the following technical scheme:
A process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is lower than 3%;
step 2: adding the long-stem fine yellow powder into a round-bottom flask, adding petroleum ether, heating and refluxing for extraction for 0.5-1 h, filtering with gauze to obtain filter residue, refluxing and extracting the filter residue for 1-2 h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
and step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 30-70 min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 120-240W, centrifuging by using a centrifuge after the ultrasonic oscillation extraction is completed, the rotating speed is 4000r/min, the time is 20-30 min, standing and layering, extracting supernatant, mixing lower-layer precipitates with 70% ethanol with the volume of 3 times, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution with chloroform-n-butanol for 2-3 times, separating liquid, adding active carbon into the upper layer liquid for decoloring, and performing suction filtration on the decolored concentrated solution;
And 5: filtering the filtrate, centrifuging to obtain filter cake, sequentially washing the filter cake with 95% ethanol, anhydrous ethanol and diethyl ether, and vacuum drying to obtain refined rhizoma Polygonati polysaccharide product.
Further, the feed-liquid ratio of the petroleum ether added in the step 2 is 1: 20-40.
Further, the volume ratio of the chloroform-n-butanol for extraction in the step 4 to the concentrated solution is 1-3: 1.
Detailed Description
in order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one skilled in the art from the embodiments given herein are intended to be within the scope of the invention.
example 1
A process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
Step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is 2.1%;
Step 2: adding the fine long-stem radix scutellariae powder into a round-bottom flask, adding petroleum ether with the material-liquid ratio of 1:20, heating and refluxing for 0.5h, filtering with gauze to obtain filter residue, refluxing and extracting the filter residue for 1.5h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
And step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 50min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 120W, centrifuging by using a centrifugal machine after the ultrasonic oscillation extraction is completed, the rotating speed is 4000r/min, the time is 20min, standing and layering, extracting supernatant, mixing lower-layer precipitate with 70% ethanol with 3 times of volume, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution once with 2 times of the volume of the chloroform-n-butanol, separating the solution, extracting once with 1 time of the volume of the chloroform-n-butanol, separating the solution, combining the upper layer liquid obtained by two extraction and separation, adding activated carbon particles for decoloring, and performing suction filtration on the decolored concentrated solution;
And 5: filtering the filtrate by centrifugation to obtain a filter cake, washing the filter cake with 95% ethanol, absolute ethanol and diethyl ether in a feed-liquid ratio of 1:0.3 respectively, and vacuum drying at 80 deg.C to obtain refined rhizoma Polygonati polysaccharide product.
Example 2
A process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is 1.8%;
Step 2: adding the long-stem radix polygonati powder into a round-bottom flask, adding petroleum ether with the material-liquid ratio of 1:25, heating and refluxing for 1h, filtering with gauze to obtain filter residue, refluxing and extracting the filter residue for 1h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
and step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 50min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 150W, centrifuging by using a centrifugal machine after the ultrasonic oscillation extraction is completed, the rotating speed is 4000r/min, the time is 25min, standing and layering, extracting supernatant, mixing lower-layer precipitate with 70% ethanol with 3 times of volume, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution once with 3 times of chloroform-n-butanol, separating, extracting once with 1 time of chloroform-n-butanol, separating, mixing the upper layer liquid obtained by two extraction and separation, adding activated carbon particles for decolorization, and performing suction filtration on the decolorized concentrated solution;
And 5: filtering the filtrate by centrifugation to obtain a filter cake, washing the filter cake with 95% ethanol, absolute ethanol and diethyl ether in a feed-liquid ratio of 1:0.6 respectively once, and vacuum drying to obtain refined rhizoma Polygonati polysaccharide product.
example 3
a process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is 1.8%;
step 2: adding the long-stem radix polygonati powder into a round-bottom flask, adding petroleum ether, heating and refluxing for extraction for 1h, filtering by using gauze to obtain filter residue, refluxing and extracting the filter residue for 2h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
and step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 60min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 180W, centrifuging by using a centrifugal machine after completion, wherein the rotating speed is 4000r/min and the time is 30min, standing for layering, extracting supernatant, mixing lower-layer precipitate with 70% ethanol with 3 times of volume, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution with 1.5 times of chloroform-n-butanol, separating, extracting with 1.5 times of chloroform-n-butanol, separating, mixing the upper layer liquid, adding activated carbon particles, decolorizing, and vacuum filtering the decolorized concentrated solution;
And 5: filtering the filtrate by centrifugation to obtain a filter cake, washing the filter cake with 95% ethanol, absolute ethanol and diethyl ether in a feed-liquid ratio of 1:1 respectively, and vacuum drying to obtain refined rhizoma Polygonati polysaccharide product.
example 4
A process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is 2.6%;
step 2: adding the fine long-stem radix scutellariae powder into a round-bottom flask, adding petroleum ether, heating and refluxing for extraction for 0.8h, filtering with gauze to obtain filter residue, refluxing and extracting the filter residue for 1.5h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
and step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 65min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 240W, centrifuging by using a centrifuge after completion, wherein the rotating speed is 4000r/min and the time is 30min, standing for layering, extracting supernatant, mixing lower-layer precipitate with 70% ethanol with the volume of 3 times, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution once with 2 times of the volume of the chloroform-n-butanol, separating the solution, extracting once with 2 times of the volume of the chloroform-n-butanol, separating the solution, combining the upper layer liquid obtained by two extraction and separation, adding activated carbon particles for decolorization, and performing suction filtration on the decolorized concentrated solution;
and 5: filtering the filtrate by centrifugation to obtain a filter cake, washing the filter cake with 95% ethanol, absolute ethanol and diethyl ether in a feed-liquid ratio of 1:0.5 respectively once, and vacuum drying to obtain refined rhizoma Polygonati polysaccharide product.
Although the present invention has been described with reference to the specific embodiments, it should be understood that the scope of the present invention is not limited thereto, and those skilled in the art will appreciate that various modifications and variations can be made without inventive changes by those skilled in the art based on the technical solutions of the present invention.
Claims (3)
1. a process for extracting polygonatum polysaccharide with the assistance of ultrasonic waves comprises the following steps:
Step 1: screening, cleaning, slicing and grinding polygonatum longstem powder into powder to obtain polygonatum longstem powder, wherein the water content of the polygonatum longstem powder is lower than 3%;
Step 2: adding the long-stem fine yellow powder into a round-bottom flask, adding petroleum ether, heating and refluxing for extraction for 0.5-1 h, filtering with gauze to obtain filter residue, refluxing and extracting the filter residue for 1-2 h at 70 ℃ by using 95% ethanol with the volume being 20 times that of the filter residue, and air-drying to obtain a sample.
and step 3: weighing a sample, adding distilled water, performing ultrasonic oscillation extraction for 30-70 min at room temperature by using an ultrasonic extractor, wherein the ultrasonic power is 120-240W, centrifuging by using a centrifuge after the ultrasonic oscillation extraction is completed, the rotating speed is 4000r/min, the time is 20-30 min, standing and layering, extracting supernatant, mixing lower-layer precipitates with 70% ethanol with the volume of 3 times, filtering, mixing filtrate and supernatant, and performing reduced pressure distillation and concentration to prepare concentrated solution;
And 4, step 4: extracting the concentrated solution with chloroform-n-butanol for 2-3 times, separating liquid, adding active carbon into the upper layer liquid for decoloring, and performing suction filtration on the decolored concentrated solution;
And 5: filtering the filtrate, centrifuging to obtain filter cake, sequentially washing the filter cake with 95% ethanol, anhydrous ethanol and diethyl ether, and vacuum drying to obtain refined rhizoma Polygonati polysaccharide product.
2. The ultrasonic-assisted extraction process of polygonatum polysaccharides according to claim 1, wherein the ratio of the petroleum ether added in the step 2 to the liquid is 1: 20-40.
3. The ultrasonic-assisted extraction process of polygonatum polysaccharides according to claim 1, wherein the volume ratio of the chloroform-n-butanol used for extraction to the concentrated solution in the step 4 is 1-3: 1.
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Cited By (3)
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| CN113817079A (en) * | 2021-11-11 | 2021-12-21 | 云南恩润生物科技发展有限公司 | Extraction method of polygonatum polysaccharide |
| CN113956374A (en) * | 2021-11-15 | 2022-01-21 | 云南恩润生物科技发展有限公司 | Extraction process of polygonatum sibiricum extract |
| CN115043955A (en) * | 2022-06-29 | 2022-09-13 | 西南林业大学 | Polygonatum polysaccharide extract and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113817079A (en) * | 2021-11-11 | 2021-12-21 | 云南恩润生物科技发展有限公司 | Extraction method of polygonatum polysaccharide |
| CN113956374A (en) * | 2021-11-15 | 2022-01-21 | 云南恩润生物科技发展有限公司 | Extraction process of polygonatum sibiricum extract |
| CN115043955A (en) * | 2022-06-29 | 2022-09-13 | 西南林业大学 | Polygonatum polysaccharide extract and preparation method thereof |
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