CN101235056A - Method for preparing plants total glycosides - Google Patents
Method for preparing plants total glycosides Download PDFInfo
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- CN101235056A CN101235056A CNA2007100731577A CN200710073157A CN101235056A CN 101235056 A CN101235056 A CN 101235056A CN A2007100731577 A CNA2007100731577 A CN A2007100731577A CN 200710073157 A CN200710073157 A CN 200710073157A CN 101235056 A CN101235056 A CN 101235056A
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Abstract
The invention relates to a preparation method of plant total glycoside which uses macroporous resin adsorption method. The invention is characterized by comprising: A adding alcohol solvent with plant materials, heating and mixing, collecting filter liquor; B combining filter liquor, depressurizing and concentrating to obtain alcohol extract; C adding water of 10 powered into the extract, mixing and standing, taking supernatant and filtering; D using macroporous adsorption column to treat the filter liquor, using water and alcohol water solution to elute, collecting eluent, depressurizing, concentrating, atomizing and drying to obtain plant total glycoside. The preparation method of plant total glycoside has the advantages that (1), the whole process utilizes alcohol and water most and avoids other harmful solvents to improve the safety of plant total glycoside, (2), the invention eliminates defat step of organic solvent to shorten the process and production time, (3), the invention reduces cost, (4) the invention is suitable for industrial production.
Description
[technical field]
The present invention relates to the preparation method of plant total glycoside, the preparation method of particularly a kind of high efficiency, low cost and free of contamination plant total glycoside.
[background technology]
Glycosides in plant or the Chinese medicine refers to the compound that is formed by connecting by sugar or sugared derivative and another nonsugar end group carbon atom by sugar.Glycosides compound is widely distributed at occurring in nature, is the important active substance of a class.
The extraction of plant total glycoside or the method for purifying generally have following several: 1, solvent extration; 2, macroreticular resin absorbing method; 3, solvent precipitation; 4, magnesium oxide adsorbing method; 5, the cholesterol precipitator method; 6, lead salt precipitation; 7, chromatography.
Relate in the method for the extraction of plant total glycoside or purifying at above seven kinds of enumerating:
Extraction process is used for the laboratory more, when carrying out solvent treatment, emulsion often occurs, and need could layering separate through stable for a long time.This method length consuming time is prone to emulsion layer, has a strong impact on the effect of extracting of total glycosides, and this method should not be to the processing of a large amount of samples.
Aspect separation and purifying plant total glycoside, no matter in the laboratory, still aborning, macroreticular resin absorbing method is the most frequently used a kind of method.Grease in plant, lipotropic component or low polarity component combine with macroporous resin, resin surface will be coated with one deck oil layer, moreover the solvent elution of macroporous resin is water or hydrophilic solvent, therefore when resin combines with grease, will reduce the macroporous resin absorption carrying capacity greatly, have a strong impact on separating effect.When using the macroporous resin purification plant total glycoside, handle sample and must carry out the pre-treatment grease removal for this reason, specific practice is: in alcohol extract, approximately 5 times of amounts by extract add entry, make it suspendible,, remove the lipophilic component purpose to reach then with sherwood oil or chloroform extraction.The aqueous solution after the grease removal just can be added in the resin column and separate at this moment.
Because of before carrying out plastic resin treatment, must remove lipophilic composition with low polar organic solvent (as ether, benzene, chloroform etc.) after, can carry out the resin chromatography purifying; Like this, to bringing a lot of problems in big the production: 1) organic solvent residual; 2) sherwood oil is an inflammable liquid, can bring serious safety problem; 3) cause production cost to rise; 4) prolong the production time etc.
[summary of the invention]
The present invention remedies the preparation method that the above-mentioned deficiency of prior art proposes a kind of plant total glycoside, improves the purity of total glycosides greatly, reduces production costs greatly and not pollution.
On the whole, most of glycoside composition tool wetting ability, water-soluble, methyl alcohol, ethanol isopolarity organic solvent.Macroporous resin is to belong to organic polymer material, and its grain pattern is the porous convex and concave feature; Contain a large amount of polar groups in the glycoside molecular structure in hydrophily is situated between, glycosides and resin-bonded are adsorbed, and use pure water solvent system wash-out then, and eluting solvent is concentrated, thereby obtain highly purified total glycosides.In a large amount of practical production experience practices, for reducing cost, raise the efficiency, we invent proposition and handle with water replacement organic solvent in the total glycosides of purifying.
Technical scheme of the present invention is as follows: the preparation method of plant total glycoside, adopt macroreticular resin absorbing method, and may further comprise the steps:
A, get plant material and add alcoholic solvent, heated and stirred is filtered, and collects filtrate;
B, merging filtrate, concentrating under reduced pressure obtains extraction using alcohol medicinal extract;
C, add to extract in the medicinal extract, stir, leave standstill with the water more than 10 times; Get supernatant liquor and filtration;
Macroporous absorption post on D, the filtrate, water and aqueous ethanolic solution wash-out are collected elutriant, and concentrating under reduced pressure, and spraying drying get plant total glycoside.
Wherein, alcoholic solvent can be methyl alcohol, ethanol or propyl alcohol etc. in the steps A.Because of the plant total glycoside that extracts mostly is medicinal, the security of drug manufacture is crucial in pharmacy, should avoid using toxic reagent to cause toxicity in process of production as far as possible, and this is the major issue of pharmaceutical technology; So solvent is preferably: ethanol.In steps A, the alcohol concn scope is 70%-99%; The temperature range of heating is 50-80 ℃; The number of times that heated and stirred is extracted is 1-4 time.
Steps A comprises step by step following again:
A1, the described plant material weight 2-8 of adding ethanol heating was doubly stirred 1.5-8 hour, filtered, and collected filtrate;
A2, filter residue add described filter residue weight 1-6 ethanol heating doubly again, stir 1-6 hour, filter, and collect filtrate.
Being evaporated to proportion among the step B is 1.1-1.4.
The amount of the water that step C adds is 15-40 a times of medicinal extract weight, is preferably 20 times.Stir after adding heavy dose of water, the glycoside material is gone out by water-soluble, and low polar water-insoluble fraction (comprising the solid fat constituents) forms precipitation, and the liquid lipid composition forms oil layer; Leave standstill for some time, get supernatant liquid filtering, remove precipitation and oil layer, must contain the aqueous solution of plant total glycoside.
Each operation among the step D all detects with the TLC method, is eluted in the water-insoluble fraction not contain till the glycoside composition.May further comprise the steps:
D1, described macroporous absorption post, with water elution, water is eluted to fraction and no longer contains till the sugared composition;
D2, with the described macroporous absorption post of 50% aqueous ethanolic solution wash-out, to described fraction, no longer contain till the glycoside composition.
Gained plant total glycoside purity is greater than 95% thus.
The high efficiency, low cost preparation method of plant total glycoside is based on the basis of macroreticular resin absorbing method and carries out improved effective ways.Glycosides is a class high polarity, and the hydrophilic element of the first species adds in the extract medicinal extract with the water of big doubly amount, and the glycoside material is gone out by water-soluble, and low polar water-insoluble fraction just forms precipitation or oil layer, thereby reaches aqueous solution part and the isolating purpose of non-water capacity part.This method utilizes the similar principle that mixes of material to propose, and puts into practice successful method.
The present invention is the improvement to macroreticular resin absorbing method, and its beneficial effect is:
1) whole process adopts the second alcohol and water as far as possible, and avoids using other hazardous solvents as far as possible, and the plant total glycoside that makes is safer;
2) reduce organic solvent grease removal step, thereby shorten processing step, reduce the production time;
3) reduce cost greatly;
4) the optimum industrialization is produced.
[description of drawings]
Fig. 1 plant total glycoside preparation flow synoptic diagram
[embodiment]
The present invention will be described below in conjunction with embodiment.
Embodiment 1:
Get digitalis purpurea (Digitalis purpurea L.) crude drug leaf powder, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the purple foxglove of 95% content.
Embodiment 2:
Get Root of Chinese Pulsatilla root powder (Amenone chinensis Bunge), add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 6 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 4.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the Root of Chinese Pulsatilla of 95% content.
Embodiment 3:
Get Chinese yam root (Dioscorea tokoro) powder, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 6 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 4.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the Chinese yam of 95% content.
Embodiment 4:
Get polygala root (Dioscorea tokoro) crude drug powder, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 4 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 3.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain the Radix Polygalae total glucosides of purity greater than 95% content.
Embodiment 5:
Get purplestem privet leaf (Ligustrum purpurascens) and pulverize cured leaf, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the purplestem privet leaf of 95% content.
Embodiment 6:
Get Root-bark of Softleaf Ash (Franxinus malacophylla) and pulverize cured leaf, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the Root-bark of Softleaf Ash of 95% content.
Embodiment 7:
Get preface stalk glossy privet (Ligustrum pedunculare) and pulverize cured leaf, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain the preface stalk glossy privet total glycosides of purity greater than 95% content.
Embodiment 8:
Get Leaf of Chinese Holly (Ilex kudincha) and pulverize cured leaf, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain the ilexlutifolia thumb total glycosides of purity greater than 95% content.
Embodiment 9:
Get Cortex Ilicis Rotundae (Ilex latifolia) and pulverize cured leaf, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate, merged filtrate twice, and concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain purity greater than the total glycosides of the Cortex Ilicis Rotundae of 95% content.
Embodiment 10:
Get Rhizoma Picrorhizae (Picrorhiza scrophulariiflora) root dry powder, add 5 times of amount 95% ethanol, filter, collect filtrate in 60 ℃ of stirring heating 2 hours.Filter residue with 3 times of amount 95% extraction using alcohols, heated 1.5 hours again, filtered, and collected filtrate.Merge filtrate twice, concentrating under reduced pressure is concentrated into proportion 1.2, obtains extraction using alcohol medicinal extract.Water with 20 times of amounts adds in the extraction medicinal extract, stirs, and leaves standstill; Get supernatant liquor and filtration, go up the macroporous absorption post then; Carry out each operation, all detect, be eluted in the water-insoluble fraction and do not contain till the glycoside composition with the TLC method.The macroporous absorption post of load sample, with water elution, water is eluted to fraction and no longer contains till the sugared composition.When not containing sugar component in the fraction, use 50% aqueous ethanolic solution wash-out instead, be eluted to stay in part and no longer contain till the glycoside composition.Merge 50% ethanol water elution liquid, concentrating under reduced pressure, and spraying drying so can obtain the Rhizoma Picrorhizae total glucosides of purity greater than 95% content.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought can not limit the present invention to explanation of the present invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, in implication suitable and any change in the scope, all should think to be included in the scope of claims with claims of the present invention.
Claims (10)
1. the preparation method of a plant total glycoside adopts macroreticular resin absorbing method, it is characterized in that may further comprise the steps:
A, get plant material and add the alcoholic solvent heated and stirred, filter, collect filtrate;
B, merging filtrate, concentrating under reduced pressure obtains extraction using alcohol medicinal extract;
C, add to extract in the medicinal extract, stir, leave standstill with water more than 10 times; Get supernatant liquor and filtration;
Macroporous absorption post on D, the filtrate, water and aqueous ethanolic solution wash-out are collected elutriant, and concentrating under reduced pressure, and spraying drying get plant total glycoside.
2. according to the preparation method of the described plant total glycoside of claim 1, it is characterized in that:
Alcoholic solvent in the described steps A is meant: methyl alcohol, ethanol or propyl alcohol.
3. according to the preparation method of the described plant total glycoside of claim 2, it is characterized in that:
Alcoholic solvent in the described steps A is an ethanol;
Described alcohol concn scope is 70%-99%; The temperature range of described heating is 50-80 ℃; The number of times that described heated and stirred is extracted is 1-4 time.
4. according to the preparation method of the described plant total glycoside of claim 3, it is characterized in that:
Described steps A comprises step by step following:
A1, the described plant material weight 2-8 of adding ethanol heating was doubly stirred 1.5-8 hour, filtered, and collected filtrate;
A2, filter residue add described filter residue weight 1-6 ethanol heating doubly again, stir 1-6 hour, filter, and collect filtrate.
5. according to the preparation method of the described plant total glycoside of claim 1, it is characterized in that:
Being evaporated to proportion among the described step B is 1.1-1.4.
6. according to the preparation method of the described plant total glycoside of claim 1, it is characterized in that:
The amount of the water that described step C adds is 15-40 a times of medicinal extract weight.
7. according to the preparation method of the described plant total glycoside of claim 6, it is characterized in that:
The amount of the water that adds among the described step C is 20 times of medicinal extract weight.
8. according to the preparation method of the described plant total glycoside of claim 1, it is characterized in that:
Be eluted in the water-insoluble fraction among the described step D and do not contain till the glycoside composition.
9. the preparation method of described plant total glycoside according to Claim 8 is characterized in that:
Described step D comprises step by step following again:
D1, described macroporous absorption post, with water elution, water is eluted to fraction and no longer contains till the sugared composition;
D2, with the described macroporous absorption post of 50% aqueous ethanolic solution wash-out, to described fraction, no longer contain till the glycoside composition
10. according to the preparation method of the described ilexlutifolia thumb total glycosides of claim 1-9, it is characterized in that:
Gained plant total glycoside purity is greater than 95%.
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| CNA2007100731577A CN101235056A (en) | 2007-01-30 | 2007-01-30 | Method for preparing plants total glycosides |
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| CNA2007100731577A CN101235056A (en) | 2007-01-30 | 2007-01-30 | Method for preparing plants total glycosides |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127121A (en) * | 2010-12-29 | 2011-07-20 | 华宝食用香精香料（上海）有限公司 | Method for extracting glucoside compound from tobacco leaves |
| CN111285908A (en) * | 2020-02-25 | 2020-06-16 | 白银香生物科技有限公司 | Preparation method of active ingredient acteoside in traditional Chinese medicine |
-
2007
- 2007-01-30 CN CNA2007100731577A patent/CN101235056A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127121A (en) * | 2010-12-29 | 2011-07-20 | 华宝食用香精香料（上海）有限公司 | Method for extracting glucoside compound from tobacco leaves |
| CN111285908A (en) * | 2020-02-25 | 2020-06-16 | 白银香生物科技有限公司 | Preparation method of active ingredient acteoside in traditional Chinese medicine |
| CN111285908B (en) * | 2020-02-25 | 2020-12-15 | 白银香生物科技有限公司 | Preparation method of active ingredient acteoside in traditional Chinese medicine |
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