CN101926921A - Liriope muscari total saponin and preparation method thereof - Google Patents
Liriope muscari total saponin and preparation method thereof Download PDFInfo
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- CN101926921A CN101926921A CN2009101424880A CN200910142488A CN101926921A CN 101926921 A CN101926921 A CN 101926921A CN 2009101424880 A CN2009101424880 A CN 2009101424880A CN 200910142488 A CN200910142488 A CN 200910142488A CN 101926921 A CN101926921 A CN 101926921A
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Abstract
The invention provides liriope muscari total saponin and a preparation method thereof. The preparation method of the liriope muscari total saponin comprises the following steps of: extracting by taking liriope muscari roots as raw materials and using ethanol with concentration more than or equal to 51 percent by weight; extracting an extracting solution by using normal butanol to obtain a coarse total saponin; dissolving the coarse total saponin by adding water, and optimizing and filtering to discard undissolved substances; firstly eluting a coarse total saponin solution by using water till an eluent is colourless and then eluting by using an aqueous ethanol solution through a nonpolar macroporous resin column; and collecting the eluent till the eluent is colourless so as to obtain the liriope muscari total saponin. The invention also provides the liriope muscari total saponin obtained by the method. The liriope muscari total saponin extracted and finely prepared by the method has specific antitumor effect.
Description
Technical field
The invention provides a kind of Liriope muscari total saponin and preparation method thereof, especially the Liriope muscari total saponin that contains the steroidal saponin constituents, and the preparation method of purification of this total saponins, this method is extracted the refining Liriope muscari total saponin that obtains and is had antitumor action.
Background technology
Liriope muscari Baily (Liriope musacarli (Decne.) Bailey) belongs to Liliaceae Radix Liriopes platymiscium, its tuber always always as Radix Ophiopogonis medical material succedaneum use; " Chinese Pharmacopoeia (one one) " records liriope muscari Baily as one of crude drug source of Radix Liriopes.
Liriope muscari Baily saponin C is a kind of monomeric compound that extracts from liriope muscari Baily, there are some researches show, and it has the good anti-S180 solid tumor and the activity of ehrlich carcinoma.
The extracting method of liriope muscari Baily saponin C is that the liriope muscari Baily medicinal material coarse powder is used methanol extraction earlier, more successively through ether, n-butanol extraction, and the monomeric compound that n-butyl alcohol extract obtains behind sephadex LH-20 and silica gel column chromatography.
Those skilled in the art find, liriope muscari Baily saponin C to go out rate low, the preparation cost height, the market that is applied to field of medicaments directly causes patient's treatment cost significantly to increase, therefore reducing application cost is the certainty that medicine comes into the market to circulate.But the most feasible active path that reduces cost is exactly the monomer of not purifying, and changing it into extraction effective site is known and general in the industry technological means.Effective site mainly refers to total saponins and goes out the rate height with respect to monomer saponin, and preparation cost is low, is fit to clinical use, and can effectively reduces the treatment cost, and patient's compliance is also fine.But the effective site of medical usage is not the mixing of simple effective ingredient etc., but mixture that must get rid of the weed and keep the flower of the leek through special process means at specific purpose (therapeutic effect), after refining, this is to need a large amount of work and consummate skill to be competent at.
At present, the tumor of medical discovery and research is a normal cell that growing in the human body or sophisticated, under the long term of some undesirable element, and the cell mass of certain one, the hyperplasia of appearance or break up unusually and the neoplasm that generates forms lump in the part.But it is different with cell with normal tissue, not according to Normocellular metabolism rule growth, and become unfettered and control, caused cell to present unusual form, function and metabolism, so that can destroy the structure of normal histoorgan and influence its function.Malignant cell can also be soaked into towards periphery and spread, even diffusion transfer continues hypertrophy at double to other organ-tissues, causes human body or life are threatened greatly.Though human body often has lump to form in the process of growth, lump differs, and to establish a capital be tumor.Therefore, the character of lump be must differentiate, correct diagnosis, correct treatment just can be accomplished.Tumor has the branch of solid tumor and non-solid tumor clinically, solid tumor and tangible tumor can by clinical examination such as x line take the photograph that sheet, CT scan, B ultrasonic or palpation are laid one's hand on and to tangible lump claim solid tumor.And X line, CT scan, B ultrasonic and palpation can't be seen or lay one's hand on and to tumor such as the leukemia in the hematopathy just belong to non-solid tumor.
The classification of cancer: leukemia (leukemia), osteocarcinoma, lymphatic cancer (comprising lymphocytoma), intestinal cancer, hepatocarcinoma, gastric cancer, pelvic cancer (comprising uterus carcinoma, cervical cancer), pulmonary carcinoma (comprising the mediastinum cancer), the brain cancer, neural cancer, breast carcinoma, esophageal carcinoma, renal carcinoma.
This shows, can not be positioned the cancer/tumor of any accurate position of human body simply clinically with the experimental result of S180, moreover monomer can not prove effectively that to the tumor strain of certain tumor effective site is effective equally, the present invention will be with this argument of full and accurate digital proof, and therapeutic treatment cancer/tumor is to cure at the growth site or the organ of human body in strict accordance with tumor, therefore, about liriope muscari Baily saponin C and about the document of liriope muscari Baily the effect of leading the way is only played in the clinical research of treatment of cancer in the prior art, and be difficult to think that it is as clinical foundation or play the effect of instruction.
Therefore, this area urgent need invention is a kind of can isolate total saponins and the preparation method of purification thereof that comprises liriope muscari Baily saponin C monomer (but not necessarily main effective ingredient), purpose is to obtain having total saponins in the liriope muscari Baily certain composition, that therapeutic effect is clear and definite, make the total saponins that obtains to be directly used in the clear and definite various preparations of therapeutic purposes of field of medicaments, the medical usage of clear and definite this plant extract of standard reduces the side effect of the product that contains Liriope muscari total saponin and reduces its medical usage risk.
Summary of the invention
The present invention develops a kind of Liriope muscari total saponin and extraction thereof and purified method through a large amount of experiment, and this method is simple, efficient, and the separating degree height makes that the activity of total saponins is more effective, accurate and with strong points, the monomer purity height.
The object of the invention is to provide the preparation method of total saponins in a kind of liriope muscari Baily, its liriope muscari Baily extract that obtains in the existing conventional technology (Liriope muscari total saponin crude extract), further process is refining, thereby has purified active component, makes its useful active effect clearer and more definite.
The object of the invention is to provide total saponins in a kind of liriope muscari Baily, this total saponins has the activity of antitumor, anticancer aspect, this effect has been corrected deviation and the mistaken ideas that the liriope muscari Baily saponin of generally acknowledging in the prior art has the medical science curative effect aspect of treatment solid tumor, overturned existing part theory, the further research and the Liriope muscari total saponin of liriope muscari Baily had valuable directive significance to tumor treatment.
The present invention also aims to provide above-mentioned Liriope muscari total saponin antitumor, as: the therapeutical effect of malignant tumor aspects such as pulmonary carcinoma, hepatocarcinoma and cervical cancer.
The invention provides the preparation method of total saponins in a kind of liriope muscari Baily, this method comprises: with liriope muscari Baily root (tuber or fibrous root) is raw material, with ethanol extraction, the extracting solution n-butanol extraction gets thick total saponins (also claiming the Liriope muscari total saponin crude extract); Getting thick total saponins is dissolved in water, make this thick total saponins solution pass through the non-polar macroporous resin post (as the ab-8 type, macroporous resin column such as d-101 type), with water elution, colourless to eluent, discard this water elution liquid, purpose is to remove carbohydrate content, and again with alcoholic acid aqueous solution eluting, it is colourless to eluent to collect eluent, preferably reclaim solvent again, obtain total saponins.This total saponins is the Liriope muscari total saponin after refining, also is total saponins in the above-mentioned liriope muscari Baily of the present invention.
Above-mentioned eluting is very important with the concentration of alcoholic solution, and the ethanol of the preferred 50-95%wt of the present invention carries out eluting.
Need to prove: in this article, the present invention is for the specification technique term, disambiguation, and the extract that the conventional extracting method of liriope muscari Baily is obtained is referred to as the Liriope muscari total saponin crude extract.
It is ethanol that said extracted obtains the extraction solvent that thick total saponins adopts, and this ethanol is the ethanol of the concentration 〉=51%wt for Diluted Alcohol on the pharmacy meaning, generally refers to the ethanol of 51%～95%wt.The above-mentioned Diluted Alcohol of the present invention refers to the alcoholic solution of alcoholic acid mass concentration≤50.5%.To defining of Diluted Alcohol referring to Chinese Pharmacopoeia appendix " test solution ", 95% ethanol 529ml adds the upper limit that 1000 milliliters of concentration of ethanol that obtain of water are the concentration of Diluted Alcohol, and through measuring and calculating, concentration of alcohol 20 is exactly a Diluted Alcohol when spending, that is, the Cmax of Diluted Alcohol is 49.5-50.5%wt.
Described liriope muscari Baily root is with ethanol extraction, the extracting solution n-butanol extraction, and the amount of this n-butyl alcohol is 0.5～5 times of liriope muscari Baily root weight, more preferably with being equal in weight of liriope muscari Baily root.
Be dissolved in water thick total saponins above-mentioned also comprising before upper prop, refilter, discard insoluble matter, filtrate, upper prop, with the step of alcoholic acid aqueous solution eluting, collect the eluent that eluent is generally at least 4 times of column volumes of collection during eluting, for example collect the eluent of 4～40 times of column volumes, in a preferred embodiment of the invention, the eluent that can collect 8～15 times of column volumes can reach purpose of the present invention and effect.Above-mentioned column volume refers to the volume of the filler filling of non-polar macroporous resin post.
The method that also has at present technology to disclose extraction Liriope muscari total saponin crude extract adopts Diluted Alcohol to extract, and adopts the method for n-butyl alcohol or resin absorption to carry out preliminary remove impurity again.The inventor extracts the crude extract that obtains according to the conventional method repetition not high through detecting proof purity, containing a large amount of carbohydrate content etc. does not have or rare active composition tumor cell, and present the strain of the active target tumor of certain inhibition at tumor locus indeterminate, lack clinical defectives such as actual directive significance.
The objective of the invention is at an existing basic enterprising one-step refining liriope muscari Baily research, removed basically impurity such as carbohydrate content, to the tumor strain of clearly classifying is arranged strong active Liriope muscari total saponin is arranged.
Liriope muscari total saponin crude extract of the present invention preferably makes by following method: with the liriope muscari Baily root is raw material, ethanol extraction with the concentration 〉=51%wt of at least 4 times of amounts of relative liriope muscari Baily raw material weight, extracting solution is concentrated into thick paste, the reuse aqueous dispersion, and then use n-butanol extraction, and get the n-butanol layer extract, reclaim solvent, obtain being described thick total saponins, be also referred to as the Liriope muscari total saponin crude extract.
" thick paste " of the present invention is known in this field, its relative density approximately should 1.35 or more than.
Above-mentioned is in the process of ethanol extraction of raw material with the liriope muscari Baily root, concentration of ethanol is 51～95%wt, alcoholic acid amount generally is preferably 10-20 times of liriope muscari Baily root raw material weight, more preferably 12～18 times, for example use the ethanol extraction of the above concentration of 51%wt (preferably approximately 85%) of 15 times of amounts; The method of extracting can any feasible method, for example be dipping, backflow etc. can, in order to obtain total saponins better, the present invention preferably adopts the method for backflow.
After above-mentioned ethanol extract reclaims solvent, add in the process of aqueous dispersion, amount of water is 0.1～10 times of liriope muscari Baily root raw material weight, preferred 0.5～5 times, in a preferred embodiment of the invention, add the aqueous dispersion of equimultiple (equimultiple of liriope muscari Baily root weight), reuse n-butanol extraction, the amount of n-butyl alcohol are above-mentioned 0.5～5 times of adding the water yield in the aqueous dispersion, the more preferably about equivalent of the water of n-butyl alcohol of Jia Ruing and adding, extract reclaims solvent, gets thick total saponins; This crude extract is the Liriope muscari total saponin crude extract, also claims thick total saponins.
Raw material of the present invention can be liriope muscari Baily or its middle product Liriope muscari total saponin crude extract, and the latter can obtain by the commercially available method of buying or putting down in writing by " Natural Medicine Chemistry " (the 4th edition, the People's Health Publisher).
Through repeatedly, accurate test experiments, stream part that contains total saponins in the liriope muscari Baily that said method is collected, be in the Liriope muscari total saponin, the liriope muscari Baily saponin A content that belongs to monomeric compound is the 3-25%wt of the amount of resulting this Liriope muscari total saponin, preferred 5～20%.
The present invention also provides total saponins in a kind of liriope muscari Baily, it is total saponins in the liriope muscari Baily that adopts above-mentioned preparation method and obtain, wherein, liriope muscari Baily saponin A content 3-25%wt, preferred 5～20%, the weight of the Liriope muscari total saponin that obtains with said method is 100% to calculate as benchmark.
In the Liriope muscari total saponin of the present invention, sign property composition is the liriope muscari Baily saponin A, and it is a monomeric compound, contains in the refining and edulcoration step of Liriope muscari total saponin stream part in collection, and the retention time of this monomeric chromatographic peak is 10～55 minutes.Through further checking, also contain the composition that liriope muscari Baily saponin B, liriope muscari Baily saponin C etc. belong to saponins equally in the liriope muscari Baily of the present invention in the total saponins, liriope muscari Baily saponin B is 12～60 minutes in the retention time that collection contains in the step of stream part of total saponins in the Radix Liriopes.Liriope muscari Baily saponin A: β-sitosterol β-D-glucopyranoside (being called for short Lm-1), liriope muscari Baily saponin B:ruscogenin 1-O-β-D-glucopyranosyl (1 → 2)-β-D-fucopyranoside (be called for short Lm-2) and liriope muscari Baily saponin C:ruscogenin 1-O-[β-D-glucopyranosyl (1 → 2)] structure that waits of [β-D-xylopyranosyl (1 → 3)]-β-D-fucopyranoside (being called for short Lm-3) and analysis be specifically referring to YuB Y, Hirai Y, Shoji J, et al.Comparative studies on the constituents of ophiopogonis tuber and its congeners.VI.Studies on the constituents of the subterranean part of Liriope spicata var.prolifera and L.muscari. (1) .Chem Pharm Bull.1990; 38 (7): 1931-1935.
For proof said extracted thing belongs to total saponins, the present invention adopts the method (TCL) of thin layer chromatography and the method (HPLC) of high performance liquid chromatography to detect (the about 203nm of ultraviolet detection wavelength), the general C18 chromatographic column that adopts, eluting is the mixed solution of methanol (10-60%wt)-water (90-40%wt) or acetonitrile (5-50%)-water (95-50%wt) mutually, more preferably methanol-water gradient elution, through DAD (UV-detector, detect wavelength 190-300nm) and the detection of qtof (two-stage mass spectrum) detector, determine that extract of the present invention belongs to the total saponins class.
In sum, as can be seen, adopt the preparation method of total saponins in traditional liriope muscari Baily, generally preparing product is the mixture of saponin and saccharide and a small amount of other micromolecular compounds, and impurity is more.
The product that the present invention prepares is purified Liriope muscari total saponin, remove impurity such as saccharide and micromolecule and low polar compound as far as possible, obtain the higher total saponin extracts of purity, comprise at the tumor at positions such as liver, lung, gastrointestinal, cervix uteri and nearly all active component of cancer tool therapeutic effect.
The present invention also provides in the above-mentioned liriope muscari Baily total saponins in the effect of anti-tumor aspect, especially the purposes of Liriope muscari total saponin in the medicine of preparation treatment cancer.Tumor of the present invention comprises benign tumor and malignant tumor, and the latter especially comprises hepatocarcinoma, pulmonary carcinoma, gastric cancer, cervical cancer.
1, the exquisite total saponins of Radix Liriopes is to the effect of H22 (hepatocarcinoma) transplanting mice
Laboratory animal: KM mice; Tumor is former: H22 (hepatocarcinoma);
The dosage design: with 200mg/kg is high dose group dosage, and 100mg/kg is a low dose group dosage.
Method and result:
60 KM mices are divided 6 groups---blank group, cyclophosphamide-a control group, acetone extract high dose group, acetone extract low dose group.Conventional inoculation H22.With the 24h administration of inoculation back, give 7 days continuously every day 1 time, in last administration 24h, put to death mice, take out the tumor piece, weigh, do the t check between group, and calculate tumour inhibiting rate.Test repeats 1 time.The results are shown in subordinate list
2, the exquisite total saponins of Radix Liriopes is to the effect of U-14 cervical cancer transplanting mice
Sample: the exquisite total saponins of Radix Liriopes; Tumor is former: U14; Animal: Kunming mouse, the II level, the department of the Chinese Academy of Sciences of Department Of Medicine, Peking University's laboratory animal section provides, credit number SCXK (capital) 2006-0008
3, the exquisite total saponins of Radix Liriopes is to the effect of Lewis lung cancer transplanting mice
Sample: the exquisite total saponins of Radix Liriopes
Tumor is former: Lewis lung cancer
Animal: C57, the II level, the department of the Chinese Academy of Sciences of Department Of Medicine, Peking University's laboratory animal section provides, credit number SCXK (capital) 2006-0008
4, the exquisite total saponins of Radix Liriopes is to the effect of S-180 sarcoma transplanting mice
Sample: the exquisite total saponins of Radix Liriopes; Tumor is former: S180;
Mice, Kunming mouse, female, body weight 18～22g.
Above-mentioned through the pharmacological effect experimental verification, by setting up the animal model of mouse transplanting tumor, result verification, the monomeric anti-pulmonary carcinoma of total saponins in the liriope muscari Baily that the present invention makes, the effect of hepatocarcinoma and cervical cancer and document record are not quite similar, what existing document was put down in writing is the effect that liriope muscari Baily saponin c has anti-ehrlich ascites carcinoma and S-180 sarcoma, the present invention is through experiment repeatedly, verified that advancing purified Liriope muscari total saponin through the present invention has lewis pulmonary carcinoma, the effect of H-22 hepatocarcinoma and U-14 cervical cancer, but the effect of anti-S-180 sarcoma is not obvious, corrected the deviation that existing theory may exist for studying and use Liriope muscari total saponin, accurate believable foundation is provided.
Confirm that through acute toxicity testing and long term toxicity test the Liriope muscari total saponin safety range is wide; Acute toxicity testing shows, the LD at total saponins position
50Can reach 1600mg/kg, the therapeutic index height, clinical practice also has safety in the treatment tumor or as the oncotherapy adjuvant drug when having effective active.
Description of drawings
Fig. 1: the chromatogram of the Liriope muscari total saponin that preparation method of the present invention obtains, wherein abscissa be the time (minute), vertical coordinate is a trap.
The specific embodiment
Describe the present invention in detail below in conjunction with accompanying drawing, but do not limit practical range of the present invention.
Embodiment 1:
Get the liriope muscari Baily medical material, add about 15 times of amount 85% alcohol reflux; Extracting solution reclaims solvent to the thick paste shape, adds to wait crude drug amount (weight) aqueous dispersion, and with n-butanol extraction 2 times, combining extraction liquid, the recovery solvent gets thick total saponins.With thick total saponins add again the crude drug amount etc. the water dissolution of times of weight, last ab-8 type macroporous resin column is earlier with water elution, be negative to eluent molish reaction, with the ethanol elution of the 95%wt of 8 times of column volumes, eluent reclaims solvent again, Liriope muscari total saponin.
Detect through the method (HPLC) that adopts efficient liquid phase chromatographic analysis, chromatographic column is C18, eluting is the mixed solution of methanol-water or acetonitrile-water mutually, the solution of methanol-water gradient elution more preferably, detect through DAD and qtof detector, the collection of illustrative plates that obtains is referring to Fig. 1, and collection of illustrative plates determines that the extract that present embodiment obtains belongs to the total saponins class, is the Liriope muscari total saponin after making with extra care.
In this total saponins, except the liriope muscari Baily saponin A, outside liriope muscari Baily saponin B and the liriope muscari Baily saponin C, also contain liriope muscari Baily saponin D (Lm-4): ruscogenin 1-β-D-fucopyranoside and liriope muscari Baily saponin E (Lm-5): pennogenin 3-O-[4 '-O-rhamnopyranosyl (1 → 3)-β-D-xylopyranosyl (1 → 4)]-β-D-fucopyranoside, specifically referring to Yu B Y, Hirai Y, Shoji J, etal.Comparative studies on the constituents of ophiopogonis tuber and its congeners.VI.Studies on the constituents of the subterranean part of Liriope spicatavar.prolifera and L.muscari. (1) .Chem Pharm Bull.1990; 38 (7): 1931-1935.
Embodiment 2:
Get the liriope muscari Baily medical material, add about 8 times of amount 75% alcohol dipping and extract 2 times; Extracting solution reclaims solvent to the thick paste shape, adds 0.5 times of crude drug amount (weight) aqueous dispersion, and with n-butanol extraction 2～5 times, combining extraction liquid reclaims solvent and gets the thick total saponins of Radix Liriopes.Thick total saponins is added the water dissolution of 0.5 times of weight of crude drug amount again, and last d-101 type macroporous resin column is earlier with water elution, be negative to eluent molish reaction, with the ethanol elution of the 80%wt of 10 times of column volumes, eluent reclaims solvent again, Liriope muscari total saponin.
Detect through the method (HPLC) that adopts efficient liquid phase chromatographic analysis, chromatographic column is C18, eluting is the solution of methanol-water gradient elution mutually, DAD and qtof detector detect, the collection of illustrative plates that obtains determines that the extract that present embodiment obtains belongs to the total saponins class, is the Liriope muscari total saponin after making with extra care.
Embodiment 3:
Get the liriope muscari Baily medical material, add about 4 times of amount 80% ethanol heating extraction; Extracting solution reclaims solvent to the thick paste shape, adds 1.5 times of crude drug amounts (weight) aqueous dispersion, and with n-butanol extraction 4 times, combining extraction liquid reclaims solvent and gets the thick total saponins of Radix Liriopes.Thick total saponins is added the water dissolution of 1.5 times of weight of crude drug amount again, and last d-101 type macroporous resin column is earlier with water elution, be negative to eluent molish reaction, with the ethanol elution of the 50%wt of 15 times of column volumes, eluent reclaims solvent again, Liriope muscari total saponin.
Embodiment 4:
Get the liriope muscari Baily medical material, add about 20 times of amount 90% ethanol heating extraction; Extracting solution reclaims solvent to the thick paste shape, adds 1.5 times of crude drug amounts (weight) aqueous dispersion, and with n-butanol extraction 4 times, combining extraction liquid reclaims solvent and gets the thick total saponins of Radix Liriopes.Thick total saponins is added the water dissolution of 1.5 times of weight of crude drug amount again, and last d-101 type macroporous resin column is earlier with water elution, be negative to eluent molish reaction, with the ethanol elution of the 90%wt of 4 times of column volumes, eluent reclaims solvent again, Liriope muscari total saponin.
Embodiment 5:
Get the liriope muscari Baily medical material, add about 15 times of amount 85% alcohol reflux; Extracting solution reclaims solvent to the thick paste shape, adds to wait crude drug amount (weight) aqueous dispersion, and with n-butanol extraction 2 times, combining extraction liquid, the recovery solvent gets thick total saponins; With thick total saponins add again the crude drug amount etc. the water dissolution of times of weight, last ab-8 type macroporous resin column is earlier with water elution, be negative to eluent molish reaction, with the ethanol elution of the 75%wt of 8 times of column volumes, eluent reclaims solvent again, Liriope muscari total saponin.
Claims (10)
1. the preparation method of a Liriope muscari total saponin, this method comprises: with the liriope muscari Baily root is raw material, with ethanol extraction, the extracting solution n-butanol extraction, thick total saponins; After getting thick total saponins and being dissolved in water, make it pass through the non-polar macroporous resin post, earlier colourless to eluent with water elution, with the alcoholic solution eluting of 50-95%wt, it is colourless to eluent to collect eluent again, Liriope muscari total saponin.
2. the described preparation method of claim 1, wherein, described thick total saponins makes by following method: with the liriope muscari Baily root is raw material, with the ethanol extraction with respect to the concentration 〉=51%wt of at least 4 times of amounts of the raw material weight of liriope muscari Baily, extracting solution is concentrated into the thick paste of degree of comparing 1.35, the reuse aqueous dispersion, use n-butanol extraction, get the n-butanol layer extract, drying gets described thick total saponins.
3. the described preparation method of claim 1, wherein, in the process of ethanol extraction liriope muscari Baily root, described alcoholic acid amount be described liriope muscari Baily root weight 10-20 doubly.
4. the described preparation method of claim 2 wherein, adds in the aqueous dispersion reuse n-butanol extraction at described extracting solution, and water is 0.1～10 times of liriope muscari Baily root weight, and n-butyl alcohol is 0.5～5 times of weight of water.
5. the described method of claim 1, wherein, described collection eluent to eluent colourless after, the content of liriope muscari Baily saponin A is 3-25%wt in the Liriope muscari total saponin that obtains.
6. Liriope muscari total saponin, it obtains for adopting the described method of claim 1.
7. the described Liriope muscari total saponin of claim 6, in this Liriope muscari total saponin, liriope muscari Baily saponin A content is 3-25%wt, is 100% in the weight of described Liriope muscari total saponin.
8. the described Liriope muscari total saponin of claim 6, wherein, described thick total saponins makes by following method: with the liriope muscari Baily root is raw material, ethanol extraction with the concentration 〉=51%wt of 4 times of amounts being at least liriope muscari Baily weight, extracting solution is concentrated into thick paste, add aqueous dispersion again, use n-butanol extraction, get thick total saponins; Get thick total saponins and be dissolved in water, after filtration discarded insoluble matter, filtrate is by the non-polar macroporous resin post, and was earlier colourless to eluent with water elution, and again with alcoholic acid aqueous solution eluting, it is colourless to eluent to collect eluent, gets Liriope muscari total saponin.
9. the purposes of the described Liriope muscari total saponin of claim 6 in the medicine of preparation treatment tumor.
10. the described purposes of claim 9, wherein, described tumor is benign tumor and/or the malignant tumor that comprises hepatocarcinoma, pulmonary carcinoma, cervical cancer.
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| CN102180932A (en) * | 2011-03-30 | 2011-09-14 | 中国药科大学 | Method for preparing steroid saponin DT-13 |
| CN107522765A (en) * | 2016-06-16 | 2017-12-29 | 天士力制药集团股份有限公司 | A kind of Liriope muscari total saponin and its preparation method and application |
| CN114113445A (en) * | 2021-12-03 | 2022-03-01 | 苏州市药品检验检测研究中心 | Method for rapidly checking adulteration of liriope spicata in heat-clearing and detoxifying oral liquid |
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2009
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| CN102085293A (en) * | 2011-01-14 | 2011-06-08 | 中国食品药品检定研究院 | Liriope muscari extract with anti-tumor action and preparation method thereof |
| CN102180932A (en) * | 2011-03-30 | 2011-09-14 | 中国药科大学 | Method for preparing steroid saponin DT-13 |
| CN102180932B (en) * | 2011-03-30 | 2013-03-13 | 天士力制药集团股份有限公司 | Method for preparing steroid saponin DT-13 |
| CN107522765A (en) * | 2016-06-16 | 2017-12-29 | 天士力制药集团股份有限公司 | A kind of Liriope muscari total saponin and its preparation method and application |
| CN107522765B (en) * | 2016-06-16 | 2021-03-09 | 天士力医药集团股份有限公司 | Liriope muscari baily total saponin and preparation method and application thereof |
| CN114113445A (en) * | 2021-12-03 | 2022-03-01 | 苏州市药品检验检测研究中心 | Method for rapidly checking adulteration of liriope spicata in heat-clearing and detoxifying oral liquid |
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