CN109354630A - The extracting method of Siberian solomonseal rhizome polysaccharide - Google Patents
The extracting method of Siberian solomonseal rhizome polysaccharide Download PDFInfo
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- CN109354630A CN109354630A CN201811523377.XA CN201811523377A CN109354630A CN 109354630 A CN109354630 A CN 109354630A CN 201811523377 A CN201811523377 A CN 201811523377A CN 109354630 A CN109354630 A CN 109354630A
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- polysaccharide
- solomonseal rhizome
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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 present invention provides a kind of extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps: (1) extracts polysaccharide crude extract: after rhizoma polygonati is dried in vacuo, crushing, it is mixed with water, 30-40min is extracted at 70-80 DEG C, then ultrasonic extraction, be centrifuged, the supernatant rotary evaporation that centrifugation is obtained, then it adds in ethanol solution and stirs, stand, filtering, gained pellet frozen is dry, obtain polysaccharide crude extract；(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, repeat extraction 3 times, merge 3 water phases being obtained by extraction, then the mass concentration that ethanol solution is added to ethyl alcohol into water phase is 80%, 12-24h is stood, obtained solid is washed in filtering, drying is dried, Siberian solomonseal rhizome polysaccharide is made.The recovery rate of extracting method provided by the invention, polysaccharide is high, can reach 15% or so.
Description
Technical field
The invention belongs to technical field of polysaccharide extraction, and in particular to a kind of extracting method of Siberian solomonseal rhizome polysaccharide.
Background technique
Rhizoma polygonati is Liliaceae HUANGJING ZANYU CAPSULE polygonatum kingianurn, rhizoma polygonati or the dry rhizome of polygonatum cyrtonema, is during China is traditional
Medicine belongs to integration of drinking and medicinal herbs Chinese herbal medicine.This product is sweet in flavor mild-natured, has the effect of tonifying middle-Jiao and Qi, invigorating the spleen moistening lung, kidney-nourishing strong bone.It is main
To have containing Multiple components such as Siberian solomonseal rhizome polysaccharide, saponin(e, niacin, quinones, amino acid and microelements and delay senescence, enhance and exempt from
The multiple pharmacological effects such as epidemic disease function, Adjust-blood lipid, hypoglycemic, antitumor.Wherein polysaccharide is main active constituent, is had significant
Human immunity activity, antitumor action, anti-aging, antibacterial, antiatherosclerosis, adjust blood pressure and blood lipoid the effects of.According to
The characteristics such as its dissolubility, the extraction separation method currently used for extracting Siberian solomonseal rhizome polysaccharide include that hot water extracts, alcohol analysis separates, microwave is auxiliary
Help extraction, ultrasonic wave extraction etc..But extraction efficiency is not high, yield is low.
Summary of the invention
In view of the drawbacks of the prior art, the present invention provides a kind of extracting method of Siberian solomonseal rhizome polysaccharide, polysaccharide high income.
The extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps:
(1) it extracts polysaccharide crude extract: after rhizoma polygonati is dried in vacuo, crushed 80 meshes, then according to solid-liquid ratio 1g:40mL and water
Mixing, extracts 30-40min, then ultrasonic extraction 30-40min at 70-80 DEG C, is centrifuged, and the supernatant that centrifugation is obtained rotates
60-80min is evaporated, then adds in ethanol solution and stirs, stands 12-24h, filtering is dry by gained pellet frozen, obtains
Polysaccharide crude extract；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, repeats extraction 3 times,
Merge 3 water phases being obtained by extraction, the mass concentration that ethanol solution is then added to ethyl alcohol into water phase is 80%, stands 12-
For 24 hours, it filters, obtained solid is successively washed 2 times with ethanol solution, dehydrated alcohol, acetone, ether respectively, dry drying, be made
Siberian solomonseal rhizome polysaccharide.
Preferably, the vacuum drying condition are as follows: 40-50 DEG C of temperature, time 3-5h.
Preferably, the power of the ultrasonic extraction be 300-400W, frequency 45KHz.
Preferably, the temperature of the rotary evaporation is 50-60 DEG C.
Preferably, the mass concentration of the ethanol solution is 95%.
Preferably, the volume ratio of chloroform and n-butanol is 1:3 in the chloroform-n-butanol mixed liquor.
Preferably, the dry condition of the drying are as follows: 80-95 DEG C of temperature, time 3-5h.
Advantages of the present invention:
The recovery rate of extracting method provided by the invention, polysaccharide is high, can reach 15% or so.
Specific embodiment
Embodiment 1
The extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps:
(1) it extracts polysaccharide crude extract: rhizoma polygonati being dried in vacuo 5h at 40 DEG C, crushed 80 meshes, then according to solid-liquid ratio 1g:
40mL is mixed with water, and 40min is extracted at 70 DEG C, then ultrasonic extraction under conditions of power is 300W, frequency is 45KHz
Then 30min, centrifugation, the supernatant that centrifugation is obtained rotary evaporation 80min at 50 DEG C are added in ethanol solution and are stirred,
12h is stood, filtering is dry by gained pellet frozen, obtains polysaccharide crude extract；Wherein, the mass concentration of the ethanol solution is
95%；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, the chloroform-is just
The volume ratio of chloroform and n-butanol is 1:3 in butanol mixed liquid, repeats extraction 3 times, merges 3 water phases being obtained by extraction, then
The mass concentration that ethanol solution is added to ethyl alcohol into water phase is 80%, stands 12h, and obtained solid is successively used ethyl alcohol molten by filtering
Liquid, dehydrated alcohol, acetone, ether wash 2 times respectively, and dry 5h is dried under conditions of 80 DEG C of temperature, Siberian solomonseal rhizome polysaccharide is made,
In, the mass concentration of the ethanol solution is 95%.
The recovery rate of polysaccharide is 14.5%.
Embodiment 2
The extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps:
(1) it extracts polysaccharide crude extract: rhizoma polygonati being dried in vacuo 3h at 50 DEG C, crushed 80 meshes, then according to solid-liquid ratio 1g:
40mL is mixed with water, and 30min is extracted at 80 DEG C, and then ultrasound mentions under conditions of power is 300-400W, frequency is 45KHz
40min is taken, is centrifuged, then the supernatant that centrifugation is obtained rotary evaporation 60min at 60 DEG C is added in ethanol solution and stirred
It mixes, stands filtering for 24 hours, gained pellet frozen is dry, obtain polysaccharide crude extract；Wherein, the mass concentration of the ethanol solution
It is 95%；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, the chloroform-is just
The volume ratio of chloroform and n-butanol is 1:3 in butanol mixed liquid, repeats extraction 3 times, merges 3 water phases being obtained by extraction, then
The mass concentration that ethanol solution is added to ethyl alcohol into water phase is 80%, is stood for 24 hours, and obtained solid is successively used ethyl alcohol molten by filtering
Liquid, dehydrated alcohol, acetone, ether wash 2 times respectively, and dry 3h is dried under conditions of 95 DEG C of temperature, Siberian solomonseal rhizome polysaccharide is made,
In, the mass concentration of the ethanol solution is 95%.
The recovery rate of polysaccharide is 14.9%.
Embodiment 3
The extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps:
(1) it extracts polysaccharide crude extract: rhizoma polygonati being dried in vacuo 4h at 48 DEG C, crushed 80 meshes, then according to solid-liquid ratio 1g:
40mL is mixed with water, and 35min is extracted at 75 DEG C, and then ultrasound mentions under conditions of power is 300-400W, frequency is 45KHz
35min is taken, is centrifuged, then the supernatant that centrifugation is obtained rotary evaporation 70min at 55 DEG C is added in ethanol solution and stirred
It mixes, stands 18h, filtering is dry by gained pellet frozen, obtains polysaccharide crude extract；Wherein, the mass concentration of the ethanol solution
It is 95%；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, the chloroform-is just
The volume ratio of chloroform and n-butanol is 1:3 in butanol mixed liquid, repeats extraction 3 times, merges 3 water phases being obtained by extraction, then
The mass concentration that ethanol solution is added to ethyl alcohol into water phase is 80%, stands 18h, and obtained solid is successively used ethyl alcohol molten by filtering
Liquid, dehydrated alcohol, acetone, ether wash 2 times respectively, and dry 4h is dried under conditions of 85 DEG C of temperature, Siberian solomonseal rhizome polysaccharide is made,
In, the mass concentration of the ethanol solution is 95%.
The recovery rate of polysaccharide is 15.2%.
Embodiment 4
The extracting method of Siberian solomonseal rhizome polysaccharide, comprising the following steps:
(1) it extracts polysaccharide crude extract: rhizoma polygonati being dried in vacuo 5h at 45 DEG C, crushed 80 meshes, then according to solid-liquid ratio 1g:
40mL is mixed with water, and 40min is extracted at 75 DEG C, and then ultrasound mentions under conditions of power is 300-400W, frequency is 45KHz
35min is taken, is centrifuged, then the supernatant that centrifugation is obtained rotary evaporation 75min at 55 DEG C is added in ethanol solution and stirred
It mixes, stands filtering for 24 hours, gained pellet frozen is dry, obtain polysaccharide crude extract；Wherein, the mass concentration of the ethanol solution
It is 95%；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, the chloroform-is just
The volume ratio of chloroform and n-butanol is 1:3 in butanol mixed liquid, repeats extraction 3 times, merges 3 water phases being obtained by extraction, then
The mass concentration that ethanol solution is added to ethyl alcohol into water phase is 80%, is stood for 24 hours, and obtained solid is successively used ethyl alcohol molten by filtering
Liquid, dehydrated alcohol, acetone, ether wash 2 times respectively, and dry 4h is dried under conditions of 90 DEG C of temperature, Siberian solomonseal rhizome polysaccharide is made,
In, the mass concentration of the ethanol solution is 95%.
The recovery rate of polysaccharide is 14.5%.
Claims (7)
1. the extracting method of Siberian solomonseal rhizome polysaccharide, it is characterised in that: the following steps are included:
(1) it extracts polysaccharide crude extract: after rhizoma polygonati is dried in vacuo, crushed 80 meshes, then according to solid-liquid ratio 1g:40mL and water
Mixing, extracts 30-40min, then ultrasonic extraction 30-40min at 70-80 DEG C, is centrifuged, and the supernatant that centrifugation is obtained rotates
60-80min is evaporated, then adds in ethanol solution and stirs, stands 12-24h, filtering is dry by gained pellet frozen, obtains
Polysaccharide crude extract；
(2) it extracts: polysaccharide crude extract being added in chloroform-n-butanol mixed liquor according to material ratio 1g:10mL, repeats extraction 3 times,
Merge 3 water phases being obtained by extraction, the mass concentration that ethanol solution is then added to ethyl alcohol into water phase is 80%, stands 12-
For 24 hours, it filters, obtained solid is successively washed 2 times with ethanol solution, dehydrated alcohol, acetone, ether respectively, dry drying, be made
Siberian solomonseal rhizome polysaccharide.
2. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: the vacuum drying condition are as follows: temperature
Spend 40-50 DEG C, time 3-5h.
3. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: the power of the ultrasonic extraction is 300-
400W, frequency 45KHz.
4. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: the temperature of the rotary evaporation is 50-
60℃。
5. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: the mass concentration of the ethanol solution is
95%。
6. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: in the chloroform-n-butanol mixed liquor
The volume ratio of chloroform and n-butanol is 1:3.
7. the extracting method of Siberian solomonseal rhizome polysaccharide according to claim 1, it is characterised in that: the dry condition of the drying are as follows: temperature
Spend 80-95 DEG C, time 3-5h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563854A (en) * | 2019-07-24 | 2019-12-13 | 湖南天泉生物科技有限公司 | Method for extracting polygonatum polysaccharide |
| CN110655591A (en) * | 2019-10-29 | 2020-01-07 | 广西壮族自治区中国科学院广西植物研究所 | Extraction method of polygonatum polysaccharide |
| CN110863208A (en) * | 2019-12-04 | 2020-03-06 | 哈尔滨工业大学（威海） | Carbon steel pickling corrosion inhibitor based on polygonatum polysaccharide |
| CN112293480A (en) * | 2020-10-23 | 2021-02-02 | 江西广雅食品有限公司 | Preparation method of green nutritional bamboo shoot can |
| CN113004433A (en) * | 2021-03-09 | 2021-06-22 | 成都中医药大学 | Rhizoma polygonati fructan and preparation method and application thereof |
| CN113121715A (en) * | 2021-03-31 | 2021-07-16 | 邵阳学院 | A method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence |
| 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 |
| CN115043955A (en) * | 2022-06-29 | 2022-09-13 | 西南林业大学 | Polygonatum polysaccharide extract and preparation method thereof |
-
2018
- 2018-12-13 CN CN201811523377.XA patent/CN109354630A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563854A (en) * | 2019-07-24 | 2019-12-13 | 湖南天泉生物科技有限公司 | Method for extracting polygonatum polysaccharide |
| CN110655591A (en) * | 2019-10-29 | 2020-01-07 | 广西壮族自治区中国科学院广西植物研究所 | Extraction method of polygonatum polysaccharide |
| CN110863208A (en) * | 2019-12-04 | 2020-03-06 | 哈尔滨工业大学（威海） | Carbon steel pickling corrosion inhibitor based on polygonatum polysaccharide |
| CN110863208B (en) * | 2019-12-04 | 2022-08-09 | 威海创惠环保科技有限公司 | Carbon steel pickling corrosion inhibitor based on polygonatum polysaccharide |
| CN112293480A (en) * | 2020-10-23 | 2021-02-02 | 江西广雅食品有限公司 | Preparation method of green nutritional bamboo shoot can |
| CN112293480B (en) * | 2020-10-23 | 2023-07-25 | 江西广雅食品有限公司 | Preparation method of green nutritional canned bamboo shoots |
| CN113004433A (en) * | 2021-03-09 | 2021-06-22 | 成都中医药大学 | Rhizoma polygonati fructan and preparation method and application thereof |
| CN113121715A (en) * | 2021-03-31 | 2021-07-16 | 邵阳学院 | A method for separating and extracting rhizoma Polygonati polysaccharide with intestinal mucosa immunocompetence |
| 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 |
| 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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Application publication date: 20190219 |