CN102178720A - Method for simultaneously preparing total saponin and polysaccharide from fiveleaf gynostemma herb - Google Patents
Method for simultaneously preparing total saponin and polysaccharide from fiveleaf gynostemma herb Download PDFInfo
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Abstract
The invention relates to a method for preparing total saponin and polysaccharide from fiveleaf gynostemma herb. The method comprises the following steps: crushing the fiveleaf gynostemma herb medicinal material; adding water and extracting with microwave assistance; adsorbing the saponin by macroporous resin to separate the polysaccharide; decoloring with H2O2, and precipitating with alcohol to prepare the polysaccharide; and extracting n-butyl alcohol, precipitating acetone, and recrystallizing ethanol to prepare the total saponin. The method has the advantages of short period, safety and reliability and low cost, and is simple in operation.
Description
Technical field:
The invention belongs to the Chinese medicine extraction field, be specifically related to a kind of method that from Herb Gynostemmae Pentaphylli, prepares total saponins and polysaccharide simultaneously.
Background technology:
Herb Gynostemmae Pentaphylli is a cucurbitaceae genus gynostemma, has another name called Herba Gynostemmatis, Pentapanax, gynostemma pentaphyllum makino, Radix Rhodiolae etc.Has blood pressure lowering, blood fat reducing, blood sugar lowering; Arteriosclerosis, inhibition thrombosis, the treatment cardiovascular disease; Calm the nerves and nourish one's nature, slow down aging improves mental activity, improves cerebral function; The activating human body normal cell, is separated fatigue at fat, the strengthening the spleen and stomach of losing weight, and calmness is arranged, hypnosis, antipsycholic action, treatment migraine; Anti-cancer and cancer-preventing suppresses to kill cancerous cell; Strengthen the activity of blood of human body medium-sized lymphocyte, strengthen the immunologic function of human body; Eliminate the toxic and side effects of hormone medicine; Effects such as antiinflammatory, anti-intestinal, gastric ulcer and abscess, the Herb Gynostemmae Pentaphylli product is used for medicine, food, beverage and cosmetics in a large number.
It is gypenoside, Herb Gynostemmae Pentaphylli glucoside (polysaccharide), water-soluble amino acid, flavonoid, multivitamin, trace element, mineral etc. that Herb Gynostemmae Pentaphylli mainly contains effective constituent.Modern pharmacological research finds that Herb Gynostemmae Pentaphylli has many-sided pharmacological action, morely thinks that it mainly gives the credit to the gypenoside composition, thereby general production after Herb Gynostemmae Pentaphylli is extracted saponin, and it contains composition residue such as saccharide and is just discarded, and has caused the waste of resource.Gypenoside is used for blood pressure lowering, and blood fat reducing treats constipation and the raising immunity of nourishing one's nature of calming the nerves, and physical strength reinforcing makes weakly, and fatigue symptom alleviates or eliminates, and slow down aging improves mental activity, improves cerebral function; Safeguard the health of cardiovascular and cerebrovascular vessel, arteriosclerosis suppresses the formation of thrombosis; Calmness is arranged, and hypnosis, antitonic are controlled poliosis, the treatment migraine, eliminates uncomfortable in chest, the elimination hormone medicine toxic and side effects.Kingdom's grace etc. are the research of Gynostemma pentaphyllum Makino polysaccharide just both at home and abroad, summarized gynostemma pentaphylla polysaccharide antitumor, to the protection of hepatic injury, improve the pharmacological action aspect the immunocompetence, hypoglycemic etc. seven.
At present, the method for extraction gypenoside mainly contains: chromatography, circumfluence method, ultrasonic extraction.Though these methods have yield preferably, complicated operation requires high to instrument.Chinese patent (application number is CN03157680.X) " a kind of extracting method of Herb Gynostemmae Pentaphylli polysaccharides ", the method of this patent disclosure is that Herb Gynostemmae Pentaphylli is in the 4.5-8.0 water at pH value, temperature is 40 ℃-70 ℃ and extracts for several times with cellulase (or mixed enzyme of cellulase) enzymatic reaction down, merge extractive liquid, concentrates, goes precipitation, clear liquor adds more than the alcohol precipitation 24h, tells polysaccharide precipitation, dehydration, vacuum drying and promptly gets Herb Gynostemmae Pentaphylli polysaccharides.This invention recovery rate is higher, but raw material availability is low.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of method for preparing simultaneously total saponin(e and polysaccharide from gynostemma pentaphylla.This method can be with short production cycle, the product yield height, and production cost is low.
Extractive technique scheme of the present invention is as follows:
A kind of method for preparing simultaneously total saponin(e and polysaccharide from gynostemma pentaphylla is characterized in that, comprises the steps:
(1) extracts: with the Herb Gynostemmae Pentaphylli pulverizing medicinal materials, add 5-8 times of V/W water microwave-assisted and extract 1-3 time, filter merge extractive liquid;
(2) macroporous resin separates total saponins and polysaccharide: said extracted liquid by macroporous resin, is collected lower column liquid, water elution, water lotion and lower column liquid are merged, obtain polysaccharide rough segmentation liquid, the alcoholic solution eluting, and collect the alcohol eluen that is rich in saponin, obtain saponin rough segmentation liquid;
(3) purifying of polysaccharide: with above-mentioned polysaccharide rough segmentation liquid H
2O
250-65 ℃ of insulation decolouring, the absolute ethyl alcohol precipitation leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide;
(4) purifying of total saponin(e: the saponin(e rough segmentation liquid that step (2) is obtained concentrates nothing alcohol, adds extracting n-butyl alcohol, and butanol extraction liquid concentrates, add acetone precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 2-4 time, leach crystallizing and drying and namely get gypenosides.
Microwave power in the step (1) is 200～900W, and extracting temperature is 60～85 ℃.
A kind of among the optional AB-8 of macroporous resin in the step (2), HPD300, D141, X-8, the X-5, alcoholic solution concentration is 30-70%.
H in the step (3)
2O
2Concentration is 30%, insulation decolouring 30-80min, and alcohol precipitation concentration is 80-95%.
In sum, good effect of the present invention is: at first adopt microwave-assisted that total saponins in the Herb Gynostemmae Pentaphylli and polysaccharide are extracted, extracting solution carries out concentration and separation through the macroporous adsorbent resin method, has the advantage that step is simple, yield is high, cost is low, and the present invention prepares two class materials simultaneously from Herb Gynostemmae Pentaphylli, the raw material availability height provides cost savings.
The specific embodiment:
The present invention is described further below in conjunction with specific embodiment, but do not limit the present invention in any way.
Embodiment one:
Gynostemma pentaphyllum is pulverized, got 1kg, add 5 times of V/W water Microwave-assisted Extractions and get 3 times, microwave power is 900W, and extracting temperature is 85 ℃, filters to merge extract, by the AB-8 macroporous resin column, collect lower column liquid, wash with water earlier to the sugar-free reaction, use again 40%, 55%, 70% ethanolic solution wash-out, water lotion and lower column liquid are merged, and collect the alcohol eluen that is rich in saponin(e, and obtain polysaccharide rough segmentation liquid and saponin(e rough segmentation liquid, add 30%H in the polysaccharide rough segmentation liquid
2O
250 ℃ of insulation decolouring 30min, adding absolute ethyl alcohol to concentration is 95% precipitation, leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide 8.9g, and content is 67.6%; Saponin(e rough segmentation liquid is concentrated into nothing alcohol, add the equal-volume extracting n-butyl alcohol, butanol extraction liquid is concentrated into 1/5 of original volume, add acetone to no longer producing precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 4 times, leach crystallizing and drying and namely get gypenosides 33g, content is 78.6%.
Embodiment two:
Gynostemma pentaphyllum is pulverized, got 1kg, add 8 times of V/W water Microwave-assisted Extractions and get 1 time, microwave power is 200W, and extracting temperature is 60 ℃, filters to merge extract, by the HPD300 macroporous resin column, collect lower column liquid, wash with water earlier to the sugar-free reaction, use again 30%, 45%, 65% ethanolic solution wash-out, water lotion and lower column liquid are merged, and collect the alcohol eluen that is rich in saponin(e, and obtain polysaccharide rough segmentation liquid and saponin(e rough segmentation liquid, add 30%H in the polysaccharide rough segmentation liquid
2O
265 ℃ of insulation decolouring 60min, adding absolute ethyl alcohol to concentration is 80% precipitation, leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide 9.5g, and content is 72.1%; Saponin(e rough segmentation liquid is concentrated into nothing alcohol, add the equal-volume extracting n-butyl alcohol, butanol extraction liquid is concentrated into 1/10 of original volume, add acetone to no longer producing precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 2 times, leach crystallizing and drying and namely get gypenosides 30.3g, content is 75.5%.
Embodiment four:
Gynostemma pentaphyllum is pulverized, got 1kg, add 6 times of V/W water Microwave-assisted Extractions and get 2 times, microwave power is 700W, and extracting temperature is 65 ℃, filters to merge extract, by the D141 macroporous resin column, collect lower column liquid, wash with water earlier to the sugar-free reaction, use again 30%, 50%, 70% ethanolic solution wash-out, water lotion and lower column liquid are merged, and collect the alcohol eluen that is rich in saponin(e, and obtain polysaccharide rough segmentation liquid and saponin(e rough segmentation liquid, add 30%H in the polysaccharide rough segmentation liquid
2O
250 ℃ of insulation decolouring 50min, adding absolute ethyl alcohol to concentration is 95% precipitation, leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide 7.3g, and content is 69.5%; Saponin(e rough segmentation liquid is concentrated into nothing alcohol, add the equal-volume extracting n-butyl alcohol, butanol extraction liquid is concentrated into 1/5 of original volume, add acetone to no longer producing precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 4 times, leach crystallizing and drying and namely get gypenosides 29.1g, content is 80.8%.
Embodiment five:
Gynostemma pentaphyllum is pulverized, got 1kg, add 6 times of V/W water Microwave-assisted Extractions and get 1 time, microwave power is 600W, and extracting temperature is 75 ℃, filters to merge extract, by the X-8 macroporous resin column, collect lower column liquid, wash with water earlier to the sugar-free reaction, use again 40%, 55%, 70% ethanolic solution wash-out, water lotion and lower column liquid are merged, and collect the alcohol eluen that is rich in saponin(e, and obtain polysaccharide rough segmentation liquid and saponin(e rough segmentation liquid, add 30%H in the polysaccharide rough segmentation liquid
2O
255 ℃ of insulation decolouring 80min, adding absolute ethyl alcohol to concentration is 85% precipitation, leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide 9.5g, and content is 71.3%; Saponin(e rough segmentation liquid is concentrated into nothing alcohol, add the equal-volume extracting n-butyl alcohol, butanol extraction liquid is concentrated into 1/7 of original volume, add acetone to no longer producing precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 2 times, leach crystallizing and drying and namely get gypenosides 28.gg, content is 78.2%.
Embodiment six:
Gynostemma pentaphyllum is pulverized, got 1kg, add 8 times of V/W water Microwave-assisted Extractions and get 2 times, microwave power is 800W, and extracting temperature is 65 ℃, filters to merge extract, by the X-5 macroporous resin column, collect lower column liquid, wash with water earlier to the sugar-free reaction, use again 30%, 50%, 65% ethanolic solution wash-out, water lotion and lower column liquid are merged, and collect the alcohol eluen that is rich in saponin(e, and obtain polysaccharide rough segmentation liquid and saponin(e rough segmentation liquid, add 30%H in the polysaccharide rough segmentation liquid
2O
255 ℃ of insulation decolouring 40min, adding absolute ethyl alcohol to concentration is 85% precipitation, leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide 8.4g, and content is 70.8%; Saponin(e rough segmentation liquid is concentrated into nothing alcohol, add the equal-volume extracting n-butyl alcohol, butanol extraction liquid is concentrated into 1/5 of original volume, add acetone to no longer producing precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 2 times, leach crystallizing and drying and namely get gypenosides 31.2g, content is 77.7%.
Claims (4)
1. a method for preparing simultaneously total saponin(e and polysaccharide from gynostemma pentaphylla is characterized in that comprising the steps:
(1) extracts: with the Herb Gynostemmae Pentaphylli pulverizing medicinal materials, add 5-8 times of V/W water microwave-assisted and extract 1-3 time, filter merge extractive liquid;
(2) macroporous resin separates total saponins and polysaccharide: said extracted liquid by macroporous resin, is collected lower column liquid, water elution, water lotion and lower column liquid are merged, obtain polysaccharide rough segmentation liquid, the alcoholic solution eluting, and collect the alcohol eluen that is rich in saponin, obtain saponin rough segmentation liquid;
(3) purifying of polysaccharide: with above-mentioned polysaccharide rough segmentation liquid H
2O
250-65 ℃ of insulation decolouring, the absolute ethyl alcohol precipitation leaches precipitation, and vacuum drying namely gets gynostemma pentaphylla polysaccharide;
(4) purifying of total saponin(e: the saponin(e rough segmentation liquid that step (2) is obtained concentrates nothing alcohol, adds extracting n-butyl alcohol, and butanol extraction liquid concentrates, add acetone precipitation, leach precipitation with absolute ethyl alcohol backflow dissolving, let cool crystallization, repeat 2-4 time, leach crystallizing and drying and namely get gypenosides.
2. a kind of method for preparing total saponins and polysaccharide from Herb Gynostemmae Pentaphylli simultaneously as claimed in claim 1 is characterized in that the microwave power in the described step (1) is 200～900W, and extracting temperature is 60～85 ℃.
3. a kind of method for preparing total saponins and polysaccharide from Herb Gynostemmae Pentaphylli simultaneously as claimed in claim 1 is characterized in that a kind of among the optional AB-8 of macroporous resin, HPD300, D141, X-8, X-5 in the described step (2), and alcoholic solution concentration is 30-70%.
4. a kind of method for preparing simultaneously total saponin(e and polysaccharide from gynostemma pentaphylla as claimed in claim 1 is characterized in that H in the described step (3)
2O
2Concentration is 30%, insulation decolouring 30-80min, and alcohol precipitation concentration is 80-95%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102600228A (en) * | 2012-04-10 | 2012-07-25 | 湖南麓山天然植物制药有限公司 | Method for preparing gypenoside in gypenoside grains |
| CN103040917A (en) * | 2012-12-26 | 2013-04-17 | 浙江农林大学 | Method for preparing total saponins and polysaccharides from Apios americana flowers simultaneously, and application of total saponins and polysaccharides |
| CN103393742A (en) * | 2013-08-19 | 2013-11-20 | 广西中医药大学 | Gynostemma pentaphyllum (thunb) makino effective fraction and application thereof |
| CN104072626A (en) * | 2013-03-26 | 2014-10-01 | 正大天晴药业集团股份有限公司 | Preparation method for clematichinenoside |
| CN106420855A (en) * | 2016-09-28 | 2017-02-22 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN107050095A (en) * | 2017-06-21 | 2017-08-18 | 遵义医学院 | A kind of preparation method of gypenoside side chain oligosaccharides |
| CN108392503A (en) * | 2018-05-29 | 2018-08-14 | 重庆医药高等专科学校 | A kind of method of total saposins in extraction Sabia parviflora Wall.ex Roxb |
| CN113813298A (en) * | 2021-10-22 | 2021-12-21 | 湖南华诚生物资源股份有限公司 | Method for separating various natural active ingredients from gynostemma pentaphylla |
| CN113929723A (en) * | 2021-10-10 | 2022-01-14 | 深圳市真味生物科技有限公司 | Preparation method and application of sweet gynostemma pentaphylla sweetener |
-
2011
- 2011-01-24 CN CN2011100291291A patent/CN102178720A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102600228A (en) * | 2012-04-10 | 2012-07-25 | 湖南麓山天然植物制药有限公司 | Method for preparing gypenoside in gypenoside grains |
| CN103040917A (en) * | 2012-12-26 | 2013-04-17 | 浙江农林大学 | Method for preparing total saponins and polysaccharides from Apios americana flowers simultaneously, and application of total saponins and polysaccharides |
| CN104072626A (en) * | 2013-03-26 | 2014-10-01 | 正大天晴药业集团股份有限公司 | Preparation method for clematichinenoside |
| CN103393742A (en) * | 2013-08-19 | 2013-11-20 | 广西中医药大学 | Gynostemma pentaphyllum (thunb) makino effective fraction and application thereof |
| CN106420855A (en) * | 2016-09-28 | 2017-02-22 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN106420855B (en) * | 2016-09-28 | 2020-10-09 | 内蒙古宏魁生物药业有限公司 | Method for leaching saponin and polysaccharide |
| CN107050095A (en) * | 2017-06-21 | 2017-08-18 | 遵义医学院 | A kind of preparation method of gypenoside side chain oligosaccharides |
| CN107050095B (en) * | 2017-06-21 | 2020-11-24 | 遵义医科大学 | Preparation method of gypenoside side chain oligosaccharide |
| CN108392503A (en) * | 2018-05-29 | 2018-08-14 | 重庆医药高等专科学校 | A kind of method of total saposins in extraction Sabia parviflora Wall.ex Roxb |
| CN113929723A (en) * | 2021-10-10 | 2022-01-14 | 深圳市真味生物科技有限公司 | Preparation method and application of sweet gynostemma pentaphylla sweetener |
| CN113813298A (en) * | 2021-10-22 | 2021-12-21 | 湖南华诚生物资源股份有限公司 | Method for separating various natural active ingredients from gynostemma pentaphylla |
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Application publication date: 20110914 |