CN101804092A - Method for preparing Chinse clinopodium herb total saponins - Google Patents
Method for preparing Chinse clinopodium herb total saponins Download PDFInfo
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- CN101804092A CN101804092A CN201010156096A CN201010156096A CN101804092A CN 101804092 A CN101804092 A CN 101804092A CN 201010156096 A CN201010156096 A CN 201010156096A CN 201010156096 A CN201010156096 A CN 201010156096A CN 101804092 A CN101804092 A CN 101804092A
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- total saponins
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Abstract
The invention relates to a method for preparing Chinse clinopodium herb total saponins. The technology steps are as follows: carrying out ultrasonic extraction on methanol or ethanol solution, extracting for 2-3 times with normal butanol, recovering normal butanol, adding acetone for precipitation, normal butanol refluxing and dissolving, adding activated carbon and aluminum oxide to remove impurity, adding acetone and precipitating for 2-3 times and the like. The Chinse clinopodium herb total saponins prepared by the method of the invention have low energy consumption, less waste liquor, short period and high product content; and the obtained product can be directly used as raw materials of medicine and health care products.
Description
Technical field:
The invention belongs to the bioseparation technology field, particularly a kind of method that adopts precipitation method to prepare Herba Clinopodii total saponins.
Background technology:
The Chinese medicine Herba Clinopodii is the dry aerial parts of the labiate Herba Clinopodii Polycephali and the Clinopodium Polycephalum Herba Clinopodii (Herba Clinopodii Polycephali), is the medical herbs of the use among the people of excavating out from Anhui Province at first.Contain saponins, flavonoid, amino acids, polysaccharide, phenolic substance and volatilization wet goods chemical compound, be mainly used in treatment metrorrhagia, hysteromyoma hemorrhage, hematuria, epistaxis, gingival hemorrhage, plane is hindered hemorrhages such as hemorrhage.Herba Clinopodii is to screen from folk remedy the seventies, after clinical verification by one of a few single medicinal material of state-promulgated pharmacopoeia typing, its determined curative effect, safe, be acknowledged as the first-selected oral gynecologic hemostatic of tcm clinical practice.The saponins material is a Herba Clinopodii medical material hemostatic functional components.
The Herba Clinopodii saponin belongs to the triterpenes saponin, is soluble in hot water, rare alcohol, is insoluble in acetone, ether, chloroform equal solvent.Record saponin about 2% in " supersound extraction-spectrophotometry Herba Clinopodii total saponins content " document that the beautiful rosy clouds of Zan are delivered.
The patent medicine Herba Clinopodii Tabellae, " pharmacopeia " clear and definite its extracting method and effect and differentiate and confirm that total saponins is a functional components.Method for making is got Herba Clinopodii 4500g, cutting, decoct with water secondary, each 1.5 hours, collecting decoction, filter, it is 1.15 (80 ℃) that filtrate is concentrated into relative density, adds the ethanol of 1.7 times of amounts, fully stir, left standstill 24 hours, get supernatant, concentrating under reduced pressure becomes the thick paste shape, is dried to dry extract, adds right amount of auxiliary materials, make granule, compacting in flakes: function with cure mainly: cooling blood for hemostasis.Be used for dysfunctional uterine hemorrhage, menorrhagia, postpartum hemorrhage, hysteromyoma hemorrhage, hematuria is had blood in stool, and spits blood spitting of blood, epistaxis, simple purpura, idiopathic thrombocytopenic purpura etc.; Assay, chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-water (80: 20) is mobile phase; The detection wavelength is 250nm.Number of theoretical plate calculates by Herba Buddlejae Lindleyanae saponin I V b peak should be not less than 3000.It is an amount of that Herba Buddlejae Lindleyanae saponin I V b reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 15 μ g, promptly.20 of this product are got in the preparation of need testing solution, remove coating, and accurate the title decides, porphyrize is got about 0.3g, and accurate the title decides, put in the tool plug conical flask, add methanol 20ml, close plug, supersound process (power 220W, frequency 50kHz) 15 minutes filters. and filtering residue adds methanol 20ml again, supersound process 15 minutes filters merging filtrate, evaporate to dryness, residue add water 30ml makes dissolving, moves in the separatory funnel, extract 4 times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, with the saturated ammonia solution 30ml of n-butyl alcohol washing, the saturated water washing of reuse n-butyl alcohol 2 times, each 30ml, divide and to get n-butyl alcohol liquid, be recycled to dried, the residue dissolve with methanol, be transferred in the 100ml measuring bottle, add methanol to scale, shake up, filter, get subsequent filtrate, promptly.Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Mostly existing the extraction with to separate Herba Clinopodii saponin products obtained therefrom content lower, method are water or alcohol reflux, extraction, purification by macroporous resin.As " the purification with macroreticular resin Herba Clinopodii total saponins technical study " that Zhang Yi etc. delivers, the document adopts purification by macroporous resin Herba Clinopodii saponin, and has contrasted the elute effect of eluant, and content has 7.7% of original solid content to bring up to 11.8%.Patent 200510027812.4 " extracting method of Chinese medicine Herba Clinopodii total saponins ", disclosed method also are to adopt water extraction and purification by macroporous resin.
And patent 200510038206.4 " preparation method of Chinese medicine Herba Clinopodii total saponins ", this method products obtained therefrom total saponins is greater than 50%, the Herba Buddlejae Lindleyanae saponin is greater than 5%, multiple working procedure such as disclosed technology is that water is carried, precipitate with ethanol, resin purification, silica gel magnesium oxide chromatography and n-butanol extraction, trivial operations.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of Herba Clinopodii saponin, and this method can improve the product content height, shortens the production cycle.
Why this method adopts supersound extraction, because supersound extraction speed is fast, energy consumption is low." supersound extraction-spectrophotometry Herba Clinopodii total saponins content " that the beautiful rosy clouds of Zan are delivered also compared supersound extraction and reflux, extract, effect, and experimental result confirms that supersound extraction is better than reflux, extract.
The object of the present invention is achieved like this:
A kind of preparation method of Herba Clinopodii total saponins is characterized in that comprising following step:
Get Herba Clinopodii pulverizing medicinal materials and its 5-7 and doubly measure alcoholic solution to add frequency be in the 40-80KHz ultrasonic extraction jar supersound extraction 1-2 hour, extract merge extractive liquid, 2-3 time;
Extracting solution is evaporated to density 1.1-1.2 adds n-butanol extraction 2-3 time, collect butanol extraction liquid and reclaim n-butyl alcohol, concentrated solution adds acetone, leaves standstill precipitating;
The precipitating thing is leached, and the adding n-butyl alcohol refluxes and dissolves, dissolving back adding activated carbon and aluminium oxide decolouring fully, and filtration, solution adds acetone again, and precipitating repeats 2-3 time, is drying to obtain product.
Alcoholic solution is methanol or alcoholic acid aqueous solution in the step 1), determining alcohol 50-70%.Preferred 60% methanol solution.
Step 2) in the n-butyl alcohol consumption be concentrated solution 3-5 doubly.
Active carbon is an injection class medicinal carbon in the step 3), and consumption 1-2%, aluminium oxide are 100-200 order neutral alumina, and consumption is 5-8%, and the acetone addition is the 1/10-1/5 of liquid.
In sum, the present invention exists following advantage: 50-70% alcohol supersound extraction can reduce the stripping of other compositions, the extraction efficiency height, and energy consumption is low; N-butanol extraction is to remove water-solubility impurity, and the adding of acetone has reduced nonpolarity element again and separated out in the precipitating process; The precipitating solvent selects n-butyl alcohol and acetone to help the recovery and the recycling of reagent.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Get 5kg Herba Clinopodii medical material, pulverize and drop into the supersound extraction jar, add the 35L50% methanol solution, with frequency 40KHz supersound extraction 2 hours, extract two 2 times, merge extractive liquid, filters, be evaporated to density 1.2, emit liquid 400ml and change over to and add the 1200ml n-butyl alcohol in the extractor and fully extract, extract the merging butanol extraction liquid 3 times, add 100ml acetone after reclaiming n-butyl alcohol, the placement precipitating that stirs fully leaches precipitate, the acetone recycling after the precipitating.Precipitate adds the decolouring of 9g injection active carbon and 27g aluminium oxide after dissolving with the backflow of 900ml n-butyl alcohol again, filters, add 90ml acetone in the filtrate, fully stir static precipitating, dissolving decolouring precipitating 3 times, the vacuum drying precipitate gets product 150g total saponin content 80%.
Embodiment 2:
Get 5kg Herba Clinopodii medical material, pulverize and drop into the supersound extraction jar, add the 35L70% methanol solution, with frequency 80KHz supersound extraction 1 hour, extract two 2 times, merge extractive liquid, filters, be evaporated to density 1.1, emit liquid 370ml and change over to and add the 1500ml n-butyl alcohol in the extractor and fully extract, extract the merging butanol extraction liquid 2 times, add 120ml acetone after reclaiming n-butyl alcohol, the placement precipitating that stirs fully leaches precipitate, the acetone recycling after the precipitating.Precipitate adds the decolouring of 20g injection active carbon and 50g aluminium oxide after dissolving with the backflow of 1000ml n-butyl alcohol again, filters, add 200ml acetone in the filtrate, fully stir static precipitating, dissolving decolouring precipitating 2 times, the vacuum drying precipitate gets product 130g total saponin content 82%.
Embodiment 3:
Get 5kg Herba Clinopodii medical material, pulverize and drop into the supersound extraction jar, add the 25L60% alcoholic solution, with frequency 60KHz supersound extraction 1.5 hours, extract two 3 times, merge extractive liquid, filters, be evaporated to density 1.12, emit liquid 380ml and change over to and add the 1200ml n-butyl alcohol in the extractor and fully extract, extract the merging butanol extraction liquid 3 times, add 150ml acetone after reclaiming n-butyl alcohol, the placement precipitating that stirs fully leaches precipitate, the acetone recycling after the precipitating.Precipitate adds the decolouring of 7g injection active carbon and 28g aluminium oxide after dissolving with the backflow of 1000ml n-butyl alcohol again, filters, add 100ml acetone in the filtrate, fully stir static precipitating, dissolving decolouring precipitating 3 times, the vacuum drying precipitate gets product 145g total saponin content 81%.
Embodiment 4:
Get 10kg Herba Clinopodii medical material, pulverize and drop into the supersound extraction jar, add the 60L60% methanol solution, with frequency 80KHz supersound extraction 1 hour, extract two 3 times, merge extractive liquid, filters, be evaporated to density 1.15, emit liquid 600ml and change over to and add the 1800ml n-butyl alcohol in the extractor and fully extract, extract the merging butanol extraction liquid 3 times, add 300ml acetone after reclaiming n-butyl alcohol, the placement precipitating that stirs fully leaches precipitate, the acetone recycling after the precipitating.Precipitate adds the decolouring of 20g injection active carbon and 100g aluminium oxide after dissolving with the backflow of 2000ml n-butyl alcohol again, filters, add 300ml acetone in the filtrate, fully stir static precipitating, dissolving decolouring precipitating 3 times, the vacuum drying precipitate gets product 308g total saponin content 81%.
Embodiment 5:
Get 10kg Herba Clinopodii medical material, pulverize and drop into the supersound extraction jar, add the 50L60% methanol solution, with frequency 80KHz supersound extraction 1 hour, extract two 3 times, merge extractive liquid, filters, be evaporated to density 1.15, emit liquid 580ml and change over to and add the 2000ml n-butyl alcohol in the extractor and fully extract, extract the merging butanol extraction liquid 3 times, add 350ml acetone after reclaiming n-butyl alcohol, the placement precipitating that stirs fully leaches precipitate, the acetone recycling after the precipitating.Precipitate adds the decolouring of 20g injection active carbon and 100g aluminium oxide after dissolving with the backflow of 2000ml n-butyl alcohol again, filters, add 200ml acetone in the filtrate, fully stir static precipitating, dissolving decolouring precipitating 3 times, the vacuum drying precipitate gets product 290g total saponin content 82%.
Claims (4)
1. the preparation method of a Herba Clinopodii total saponins is characterized in that comprising following step:
1) gets Herba Clinopodii pulverizing medicinal materials and its 5-7 and doubly measure alcoholic solution to add frequency be in the 40-80KHz ultrasonic extraction jar supersound extraction 1-2 hour, extract merge extractive liquid, 2-3 time;
2) extracting solution is evaporated to density 1.1-1.2 and adds n-butanol extraction 2-3 time, collect butanol extraction liquid and reclaim n-butyl alcohol, concentrated solution adds acetone, leaves standstill precipitating;
3) the precipitating thing is leached, the adding n-butyl alcohol refluxes and dissolves, dissolving back adding activated carbon and aluminium oxide decolouring fully, and filtration, solution adds acetone again, and precipitating repeats 2-3 time, is drying to obtain product.
2. according to the preparation method of the described Herba Clinopodii total saponins of claim 1, it is characterized in that alcoholic solution is methanol or alcoholic acid aqueous solution in the step 1), determining alcohol 50-70%.
3. according to the preparation method of the described Herba Clinopodii total saponins of claim 1, it is characterized in that step 2) in the n-butyl alcohol consumption be concentrated solution 3-5 doubly.
4. according to the preparation method of the described Herba Clinopodii total saponins of claim 1, it is characterized in that active carbon is an injection class medicinal carbon in the step 3), consumption 1-2%, aluminium oxide are 100-200 order neutral alumina, consumption is 5-8%, and the acetone addition is the 1/10-1/5 of liquid.
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| CN201010156096A CN101804092A (en) | 2010-04-27 | 2010-04-27 | Method for preparing Chinse clinopodium herb total saponins |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106491454A (en) * | 2016-12-15 | 2017-03-15 | 柳州两面针股份有限公司 | Chinese medicinal toothpaste |
| CN108126006A (en) * | 2016-12-01 | 2018-06-08 | 林凡友 | The preparation process of clinopodium polycephalum oral preparation |
| CN110787212A (en) * | 2019-12-12 | 2020-02-14 | 柳州两面针股份有限公司 | Method for decoloring clinopodium polycephalum extract |
| CN112641824A (en) * | 2020-12-30 | 2021-04-13 | 柳州两面针股份有限公司 | Chinese medicine clinopodium polycephalum flow extraction method |
-
2010
- 2010-04-27 CN CN201010156096A patent/CN101804092A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126006A (en) * | 2016-12-01 | 2018-06-08 | 林凡友 | The preparation process of clinopodium polycephalum oral preparation |
| CN106491454A (en) * | 2016-12-15 | 2017-03-15 | 柳州两面针股份有限公司 | Chinese medicinal toothpaste |
| CN110787212A (en) * | 2019-12-12 | 2020-02-14 | 柳州两面针股份有限公司 | Method for decoloring clinopodium polycephalum extract |
| CN112641824A (en) * | 2020-12-30 | 2021-04-13 | 柳州两面针股份有限公司 | Chinese medicine clinopodium polycephalum flow extraction method |
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Application publication date: 20100818 |