CN101904968B - Preparation method of Chinese paris rhizome yam type saponin and anti-tumor medicinal preparation thereof - Google Patents
Preparation method of Chinese paris rhizome yam type saponin and anti-tumor medicinal preparation thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of Chinese paris rhizome yam type saponin and an anti-tumor medicinal preparation thereof. The preparation method of the Chinese paris rhizome yam type saponin comprises the following steps of: extracting the Chinese paris rhizome yam type saponin from Chinese paris rhizome by using an ethanol extraction method; and combining a resin filling material and a silica gel chromatographic column to effectively remove the impurities of sugar, protein, amino acid and the like in the Chinese paris rhizome, wherein t he extraction rate reaches up to 82 to 88 percent, the content of active ingredients is high, the process is simple, and the quality is controllable, so the preparation method is suitable for industrial production. Besides, the extract namely the Chinese paris rhizome yam type saponin has definite ingredients and obvious anti-tumor action, and can be directly prepared into the anti-tumor medicinal preparation or prepared into the anti-tumor medicinal preparation by matching the Chinese paris rhizome yam type saponin with common accessories, and the preparation contains 40 to 60 percent of the Chinese paris rhizome yam type saponin and 60 to 40 percent of the common medicinal accessories.
Description
Technical field
The present invention relates to belong to the preparation and the applied technical field of Chinese herbal medicine active component, particularly relate to a kind of preparation method and anti-tumor medicinal preparation thereof of Chinese paris rhizome yam type saponin.
Background technology
Rhizoma Paridis (Rhizoma paridis) claims Rhizoma Paridis again, is a kind of Liliaceae paris plant, is stated from Shennong's Herbal with the name head of Rhizoma Paridis, the history of existing more than one thousand years in the application of Chinese medicine, and in anticancer Chinese medicine preparation, often use.Rhizoma Paridis total saponins is the main effective ingredient of the multiple pharmacological action of Rhizoma Paridis, has the effect of the calm and antitumor of anti-inflammation, pain relieving.Content with the Rhizoma Dioscoreae saponins in its main active steroidal saponin is the highest.The Rhizoma Dioscoreae saponins is that sapogenin is a diosgenin, is that in glucose, rhamnose, the arabinose one or more combine with the straight or branched form with joining glycosyl.
The preparation of active component and anti-tumor activity thereof have been subjected to the extensive concern of numerous researcheres in the Rhizoma Paridis in recent years: the effective ingredient saponin is to animal transplanting tumor 8 in the Rhizoma Paridis
180, S
37, EAC, ARS, L
759Deng the obvious suppression effect is arranged; Rhizoma Paridis total saponins is to H
22The animal transplanting tumor growth has influence, and Rhizoma Paridis total saponins 350mg/kg ig and 10,5mg/kg ig all can obviously suppress the growth of tumor cell; Monomer saponin I and IV have cytotoxicity etc. to mouse lymph leukemia (L1210) in the Rhizoma Paridis.But do not see the preparation technology of Chinese paris rhizome yam type saponin and the research of anti-tumor biological aspect up to now as yet and be seen in report.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of method simple and be suitable for the preparation method of the Chinese paris rhizome yam type saponin of suitability for industrialized production.
Another object of the present invention is to provide more than one to state the anti-tumor medicinal preparation that Chinese paris rhizome yam type saponin is made as active component.
In order to achieve the above object, the preparation method of Chinese paris rhizome yam type saponin provided by the invention comprises the following step that carries out in order:
1) Rhizoma Paridis is crushed to graininess, the alcoholic solution that adds 60%-90% then, Rhizoma Paridis is 1g: 3-20ml, heating and refluxing extraction 1-3 time with the adding ratio of 60%-90% alcoholic solution, each 1-3 hour, merge extractive liquid, also was concentrated into every milliliter of concentrated solution and is equivalent to the 1g crude drug;
2) alcoholic solution with above-mentioned concentrated solution water or 1%-40% dilutes 1-20 doubly, then above-mentioned diluent is adsorbed by saponin absorbent-type macroporous adsorptive resins, the alcoholic solution eluting of water or 1%-40% afterwards, use the alcoholic solution eluting of 40%-60%, 70%-90% more successively, collect with the eluent behind the 70%-90% alcoholic solution eluting and to be concentrated into relative density be 1.2 Chinese paris rhizome yam type saponin crude product solution;
3) be incorporated as its weight 1-3 silica gel and mix homogeneously doubly in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel;
4) the above-mentioned sample silica gel of mixing is packed into in its weight 20-50 silicagel column doubly, use then by in ethyl acetate, the dichloromethane any one, any one and water in methanol and the ethanol and the mixed solvent made carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin composition, concentrating under reduced pressure, drying, pulverizing promptly get Powdered Chinese paris rhizome yam type saponin.
Described saponin absorbent-type macroporous adsorbent resin is D101 type, SP type or AB-8 type.
The weight ratio of described Rhizoma Paridis and saponin absorbent-type macroporous adsorbent resin is 3: 1-10: 1, and the post footpath of saponin absorbent-type macroporous adsorptive resins is 1 with the ratio of post height: 4-1: 8.
The volume ratio of any one in any one in the mixed solvent of described step 4) in ethyl acetate, the dichloromethane, methanol and the ethanol and water is 72～76: 18～20: 4.
Described Powdered Chinese paris rhizome yam type saponin can be prepared into solid orally ingestible or liquid oral medicine commonly used clinically.
The anti-tumor medicinal preparation of making as active component with above-mentioned Chinese paris rhizome yam type saponin provided by the invention is made up of the Chinese paris rhizome yam type saponin of 40%-60% and the common medicinal supplementary material of 60%-40%.Pharmaceutic adjuvant is conventional drug excipient, as diluent, solvent, disintegrating agent, correctives and antiseptic etc.
Described anti-tumor medicinal preparation is solid orally ingestible or a liquid oral medicine commonly used clinically, such as tablet, capsule, pill, granule, drop pill or oral liquid.
The preparation method of Chinese paris rhizome yam type saponin provided by the invention and anti-tumor medicinal preparation thereof have following beneficial effect:
1, this preparation method is to utilize the method for alcohol extraction to extract Chinese paris rhizome yam type saponin from Rhizoma Paridis, and the impurity such as sugar, protein and aminoacid in the Rhizoma Paridis are effectively removed in the combination that utilizes resin extender and silica gel chromatographic column, extraction ratio is up to 82%-88%, so content of effective height, and technology is simple, quality controllable, therefore be suitable for suitability for industrialized production.
2, extract Chinese paris rhizome yam type saponin definite ingredients, antitumor action is obvious, and can directly make or cooperate with adjuvant commonly used and make anti-tumor medicinal preparation.
Description of drawings
The ascites tumor mice survival rate curve chart of Fig. 1 for drawing in the present invention's experiment.
The specific embodiment
Below in conjunction with embodiment in detail the present invention is described in detail, embodiment only is used for explanation, but can not limit the scope of the invention.
Embodiment 1:
The 1kg Rhizoma Paridis is crushed to graininess, adds 4 liter 75% alcoholic solution then, heating and refluxing extraction 3 times, each 3 hours, merge extractive liquid, also was concentrated into 1L; With 10 times of above-mentioned concentrated solution dilute with waters, then above-mentioned diluent to be adsorbed by D101 type macroporous adsorptive resins, the weight ratio of Rhizoma Paridis and macroporous adsorbent resin is 5: 1, the post footpath of macroporous adsorbent resin resin column is 1: 8 with the ratio of post height; Carry out eluting with 10 liter 30% alcoholic solution, 8 liter 50% alcoholic solution and 12 liter 80% alcoholic solution successively then, collect that to carry out the eluent behind the eluting and be concentrated into relative density with 80% alcoholic solution be 1.2 Chinese paris rhizome yam type saponin crude product solution; Add 2 times of silica gel and mix homogeneously that amount is heavy in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel; The above-mentioned sample silica gel of mixing is packed in the silicagel column for 30 times of its weight, use dichloromethane, the volume ratio of first alcohol and water is that 74: 18: 4 mixed solvent carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin, concentrating under reduced pressure, dry, pulverize, promptly get the pale brown toner powder of 15g Chinese paris rhizome yam type saponin, the whole Rhizoma Dioscoreae saponins in the Rhizoma Paridis have been comprised through the above-mentioned Chinese paris rhizome yam type saponin of measuring, wherein Formosanin is not less than 26%, Gracillin is not less than 14%, Polyphyllin D is not less than 38%, and Dioscin content is not less than 2%, and the total amount of above-mentioned these compositions is not less than 80%
Embodiment 2:
The 1kg Rhizoma Paridis is crushed to graininess, adds 4 liter 80% alcoholic solution then, heating and refluxing extraction 3 times, each 2 hours, merge extractive liquid, also was concentrated into 1L; Above-mentioned concentrated solution with 8 times of 20% alcoholic solution dilutions, is adsorbed above-mentioned diluent then by SP825 type macroporous adsorptive resins, the weight ratio of Rhizoma Paridis and macroporous adsorbent resin is 4: 1; The post footpath of macroporous adsorbent resin resin column is 1: 7 with the ratio of post height, carry out eluting with 10 liter 25% alcoholic solution, 7 liter 55% alcoholic solution and 12 liter 75% alcoholic solution successively afterwards, collect that to carry out the eluent behind the eluting and be concentrated into relative density with 75% alcoholic solution be 1.2 Chinese paris rhizome yam type saponin crude product solution; Add 3 times of silica gel and mix homogeneously that amount is heavy in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel; The above-mentioned sample silica gel of mixing is packed in the silicagel column for 40 times of its weight, use ethyl acetate, the volume ratio of first alcohol and water is that the lower floor's solvent in 76: 20: 4 the mixed solvent carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin, concentrating under reduced pressure, dry, pulverize, promptly get the pale brown toner powder of 15g Chinese paris rhizome yam type saponin, the whole Rhizoma Dioscoreae saponins in the Rhizoma Paridis have been comprised through the above-mentioned Chinese paris rhizome yam type saponin of measuring, wherein Formosanin is not less than 26%, Gracillin is not less than 14%, Polyphyllin D is not less than 38%, Dioscin content is not less than 2%, and the total amount of above-mentioned these compositions is not less than 80%.
Embodiment 3:
The 1kg Rhizoma Paridis is crushed to graininess, adds 3 liter 85% alcoholic solution then, heating and refluxing extraction 3 times, each 3 hours, merge extractive liquid, also was concentrated into 1L; Above-mentioned concentrated solution with 7 times of 25% alcoholic solution dilutions, is adsorbed above-mentioned diluent then by AB-8 type macroporous adsorptive resins, the weight ratio of Rhizoma Paridis and macroporous adsorbent resin is 3: 1; The post footpath of macroporous adsorbent resin resin column is 1: 6 with the ratio of post height, carry out eluting with 10 liter 30% alcoholic solution, 8 liter 50% alcoholic solution and 12 liter 80% alcoholic solution successively afterwards, collect that to carry out the eluent behind the eluting and be concentrated into relative density with 80% alcoholic solution be 1.2 Chinese paris rhizome yam type saponin crude product solution; Add 3 times of silica gel and mix homogeneously that amount is heavy in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel; The above-mentioned sample silica gel of mixing is packed in the silicagel column for 30 times of its weight, use dichloromethane, the volume ratio of second alcohol and water is that the lower floor's solvent in 74: 18: 4 the mixed solvent carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin, concentrating under reduced pressure, dry, pulverize, promptly get the pale brown toner powder of 15g Chinese paris rhizome yam type saponin, the whole Rhizoma Dioscoreae saponins in the Rhizoma Paridis have been comprised through the above-mentioned Chinese paris rhizome yam type saponin of measuring, wherein Formosanin is not less than 26%, Gracillin is not less than 14%, PolyphyllinD is not less than 38%, Dioscin content is not less than 2%, and the total amount of above-mentioned these compositions is not less than 80%.
Embodiment 4:
The 1kg Rhizoma Paridis is crushed to graininess, adds 6 liter 70% alcoholic solution then, heating and refluxing extraction 2 times, each 2 hours, merge extractive liquid, also was concentrated into 1L; Above-mentioned concentrated solution with 8 times of 30% alcoholic solution dilutions, is adsorbed above-mentioned diluent then by D101 type macroporous adsorptive resins, the weight ratio of Rhizoma Paridis and macroporous adsorbent resin is 6: 1; The post footpath of macroporous adsorbent resin resin column is 1: 8 with the ratio of post height, carry out eluting with 10 liter 35% alcoholic solution, 6 liter 50% alcoholic solution and 12 liter 85% alcoholic solution successively afterwards, collect that to carry out the eluent behind the eluting and be concentrated into relative density with 85% alcoholic solution be 1.2 Chinese paris rhizome yam type saponin crude product solution; Add 2 times of silica gel and mix homogeneously that amount is heavy in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel; The above-mentioned sample silica gel of mixing is packed in the silicagel column for 40 times of its weight, use ethyl acetate, the volume ratio of second alcohol and water is that the lower floor's solvent in 74: 20: 4 the mixed solvent carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin, concentrating under reduced pressure, dry, pulverize, promptly get the pale brown toner powder of 15g Chinese paris rhizome yam type saponin, the whole Rhizoma Dioscoreae saponins in the Rhizoma Paridis have been comprised through the above-mentioned Chinese paris rhizome yam type saponin of measuring, Formosanin is not less than 26%, Gracillin is not less than 14%, Polyphyllin D is not less than 38%, Dioscin content is not less than 2%, and the total amount of above-mentioned these compositions is not less than 80%.
Embodiment 5:
The 1kg Rhizoma Paridis is crushed to graininess, adds 4 liter 90% alcoholic solution then, heating and refluxing extraction 3 times, each 3 hours, merge extractive liquid, also was concentrated into 1L; Above-mentioned concentrated solution with 9 times of 10% alcoholic solution dilutions, is adsorbed above-mentioned diluent then by SP825 type macroporous adsorptive resins, the weight ratio of Rhizoma Paridis and macroporous adsorbent resin is 7: 1; The post footpath of macroporous adsorbent resin resin column is 1: 9 with the ratio of post height, carry out eluting with 10 liter 40% alcoholic solution, 5 liter 60% alcoholic solution and 12 liter 85% alcoholic solution successively afterwards, collect that to carry out the eluent behind the eluting and be concentrated into relative density with 85% alcoholic solution be 1.2 Chinese paris rhizome yam type saponin crude product solution; Add 3 times of silica gel and mix homogeneously that amount is heavy in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel; The above-mentioned sample silica gel of mixing is packed in the silicagel column for 30 times of its weight, use dichloromethane, the volume ratio of first alcohol and water is that the lower floor's solvent in 76: 20: 4 the mixed solvent carries out eluting, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin, concentrating under reduced pressure, dry, pulverize, promptly get the pale brown toner powder of 15g Chinese paris rhizome yam type saponin, the whole Rhizoma Dioscoreae saponins in the Rhizoma Paridis have been comprised through the above-mentioned Chinese paris rhizome yam type saponin of measuring, wherein Formosanin is not less than 26%, Gracillin is not less than 14%, Polyphyllin D is not less than 38%, Dioscin content is not less than 2%, and the total amount of above-mentioned these compositions is not less than 80%.
Embodiment 6:
With 16g Chinese paris rhizome yam type saponin and the 24g microcrystalline Cellulose mix homogeneously of making in the foregoing description, add polyvinylpolypyrrolidone 1.2g then, make soft material with ethanol water, cross 20 mesh sieve system granules, 60 ℃ were descended granulate dry 1 hour, add the 1g magnesium stearate afterwards, mixing, tabletting can make 100 tablets of Chinese paris rhizome yam type saponin antitumor tablets.
Embodiment 7:
With 20g Chinese paris rhizome yam type saponin and 10g lactose and the 10g dextrin mix homogeneously of making in the foregoing description, add 3% polyvinylpolypyrrolidone 1.5g then, make granule with 3% polyvidone ethanol water, drying is 1 hour under 60 ℃, granulate adds the 1g Pulvis Talci, mixing afterwards, filled capsules can make 150 Chinese paris rhizome yam type saponin anti-tumor capsules.
Embodiment 8:
With 15g Chinese paris rhizome yam type saponin and 10g Polyethylene Glycol-6000 mix homogeneously of making in the foregoing description, heating makes its fusion, moves to drop pill then and drips in the jar, in the liquid paraffin with medicine liquid droplet to 6～8 ℃, oil removing can make 300 Chinese paris rhizome yam type saponin antitumor drop pill.
The Chinese paris rhizome yam type saponin that utilizes preparation method provided by the invention to make has the effect of treatment malignant solid tumor, and its pharmacological action can be verified by following pharmacodynamic experiment.
One, Chinese paris rhizome yam type saponin is to the inhibitory action of tumor cell in-vitro multiplication
(1) experiment material
Cell strain
Mice lung adenocarcinoma cell line LA795, human lung adenocarcinoma cell line A549, human colon cancer cell strain CaCo-2, human hepatoma cell strain BEL7402, human hepatoma cell strain HepG2, human cervical carcinoma cell Hela, people's epidermal carcinoma A431, people's acute myeloid leukaemia cell HL-60, people's renal adenocarcinoma cell strain A498 is all provided by the China Concord Medical Science University Institute of Basic Medical Sciences.
Reagent
The Rhizoma Paridis saponin standard substance all obtain (purity＞95%) by the present patent application people extraction separation.The cisplatin powder ampoule agent for injection is produced by Qilu Pharmaceutical Co., Ltd., and molecular weight is 300.
Instrument
Cell culture incubator, microplate reader
(2) experimental technique
The exponential phase cell is mixed with certain density cell suspension after with trypsinization, and (wherein, the LA795 cell is 3 * 10
4Individual/mL, the A549 cell is 2 * 10
4Individual/mL, the CaCo-2 cell is 5 * 10
4Individual/mL, the BEL7402 cell is 2 * 10
3Individual/mL, the HepG2 cell is 1 * 10
5Individual/mL, the Hela cell is 5 * 10
4Individual/mL, the A431 cell is 1 * 10
5Individual/mL, the HL-60 cell is 2 * 10
5Individual/mL, the A498 cell is 1 * 10
4Individual/as mL), to be inoculated in 96 hole ELISA Plate, every hole 200 μ L.Change the culture fluid that does not contain serum behind the 24h and make cell synchronization growth, every hole 200 μ L.(the 3rd day) adds the fresh medium contain variable concentrations saponin (dimethyl sulfoxide as solvent, final concentration＜0.1%) and dimethyl sulphoxide control behind the 24h, and every hole 200 μ L are subjected to reagent to establish 4 dosage groups, establish 8 parallel holes for every group, and establish the blank well zeroing.After cultivating 24h under these conditions, add the freshly prepared 0.5mg/mL MTT of 100 μ L serum-free mediums at every Kong Zhongzai, continue to cultivate 4h, add 100 μ L dimethyl sulfoxide with dissolving MTT first Za granule at every Kong Zhongzai then, behind microoscillator vibration mixing, measure optical density value (OD) on microplate reader, repeated experiments 3 times is averaged.Handling tumor cell with solvent control is matched group, calculates suppression ratio, inhibitory rate of cell growth (%)=[(1-sample sets OD value/matched group OD value) * 100%] by the OD value.
(3) experimental result (seeing Table 1)
The Chinese paris rhizome yam type saponin of table 1 variable concentrations is to the influence of various growth of tumour cell suppression ratio
As can be seen from the above table, Rhizoma Paridis total saponins is followed successively by LA795＞A549＞Hela＞CaCo-2＞HL-60＞A498＞A431＞HepG2＞BEL7402 to the inhibition power of each tumor cell line.The result shows that Chinese paris rhizome yam type saponin has the obvious suppression effect in external growth to tumor cell.
Two, Chinese paris rhizome yam type saponin is to the influence of mice LA795 adenocarcinoma of lung transplanted tumor suppression ratio
Adenocarcinoma of lung LA795 tumor tissue is inoculated in 50 nude mouse right side axillary fossas under aseptic condition subcutaneous.With vernier caliper measurement Nude Mice diameter, treat that tumor growth is to 100-300mm
3The time, above-mentioned mice is divided into 5 groups at random, 10 every group: (1) Chinese paris rhizome yam type saponin high dose group: 100mg/kgbw (bw represents body weight) irritates stomach; (2) dosage group in the Chinese paris rhizome yam type saponin, 60mg/kgbw irritates stomach; (3) Chinese paris rhizome yam type saponin low dose group, 30mg/kgbw irritates stomach; (4) cyclophosphamide group, the 20mg/kgbw lumbar injection; (5) normal saline group is irritated stomach.Every 0.2ml uses the method for measuring the tumor footpath to dynamic observe tested thing Graft Versus Tumor.The measurement number of times of diameter of tumor is 2 times weekly, divides the another name Mus heavy before the administration and before each the measurement.The computing formula of gross tumor volume (TV) is: TV=1/2 * a * b
2(a, b represent length and width respectively).Calculate relative tumour volume (RTV) according to measurement result, computing formula is RTV=V
t/ V
0(V
0Measure gained gross tumor volume, V when promptly dividing the cage administration
tGross tumor volume when measuring each time after the administration).The evaluation index of anti-tumor activity is relative tumor proliferation rate T/C (%), and computing formula is as follows: T/C (%)=T
RTV÷ C
RTV* 100% (T wherein
RTV: treatment group RTV; C
RTV: negative control group RTV), Chinese paris rhizome yam type saponin the results are shown in Table 2 to the experimental treatment influence of human lung adenocarcinoma Nude Mice LA795.
Table 2 Chinese paris rhizome yam type saponin is to the experimental treatment influence of human lung adenocarcinoma Nude Mice LA795
Compare * p＜0.05 with the normal saline matched group.
Three, Chinese paris rhizome yam type saponin is to the influence of ascites tumor mice survival rate
Get S180 ascites tumor cell suspension under aseptic condition, with normal saline dilution, counting, being deployed into cell concentration is 1 * 10
7The cell suspension of/mL, with the intraperitoneal of above-mentioned cell suspension inoculation in 30 healthy mices, every 0.2mL, inoculum density are 2 * 10 under condition of ice bath
6/ mL.Inoculate after 3 days above-mentioned 30 mices are divided into 3 groups at random, 10 every group, the beginning administration, every day 1 time: model group gavages normal saline, every 0.2ml; The cisplatin group is pressed the 2mg/kgbw lumbar injection; Rhizoma Paridis dioscin group, oral administration, dosage 30mg/kgbw, the state and the death condition of observing mice, the residue number of elements of counting mice.Utilize statistical method to analyze (see figure 1) above-mentioned experimental data, the result shows that Chinese paris rhizome yam type saponin can obviously improve the survival rate of ascites tumor mice.
Claims (6)
1. the preparation method of a Chinese paris rhizome yam type saponin, it is characterized in that: the preparation method of described Chinese paris rhizome yam type saponin comprises the following step that carries out in order:
1) Rhizoma Paridis is crushed to graininess, the alcoholic solution that adds 60%-90% then, Rhizoma Paridis is 1g: 3-20ml, heating and refluxing extraction 1-3 time with the adding ratio of 60%-90% alcoholic solution, each 1-3 hour, merge extractive liquid, also was concentrated into every milliliter of concentrated solution and is equivalent to the 1g crude drug;
2) alcoholic solution with above-mentioned concentrated solution water or 1%-40% dilutes 1-20 doubly, then above-mentioned diluent is adsorbed by saponin absorbent-type macroporous adsorptive resins, the alcoholic solution eluting of water or 1%-40% afterwards, use the alcoholic solution eluting of 40%-60%, 70%-90% more successively, collect with the eluent behind the 70%-90% alcoholic solution eluting and to be concentrated into relative density be 1.2 Chinese paris rhizome yam type saponin crude product solution;
3) be incorporated as its weight 1-3 silica gel and mix homogeneously doubly in above-mentioned Rhizoma Dioscoreae saponins crude product solution, drying under reduced pressure must be mixed sample silica gel;
4) the above-mentioned sample silica gel of mixing is packed into in its weight 20-50 silicagel column doubly, use then by in ethyl acetate, the dichloromethane any one, any one and water in methanol and the ethanol and the mixed solvent made carries out eluting, the volume ratio of any one in any one in the mixed solvent in ethyl acetate, the dichloromethane, methanol and the ethanol and water is 72～76: 18～20: 4, detect eluent is online with the silica gel G plate, collection contains the eluent of Chinese paris rhizome yam type saponin composition, concentrating under reduced pressure, drying, pulverizing promptly get Powdered Chinese paris rhizome yam type saponin.
2. the preparation method of Chinese paris rhizome yam type saponin according to claim 1, it is characterized in that: described saponin absorbent-type macroporous adsorbent resin is D101 type, SP type or AB-8 type.
3. the preparation method of Chinese paris rhizome yam type saponin according to claim 1, it is characterized in that: the weight ratio of described Rhizoma Paridis and saponin absorbent-type macroporous adsorbent resin is 3: 1-10: 1, and the post footpath of saponin absorbent-type macroporous adsorptive resins is 1 with the ratio of post height: 4-1: 8.
4. the preparation method of Chinese paris rhizome yam type saponin according to claim 1 is characterized in that: described Powdered Chinese paris rhizome yam type saponin can be prepared into solid orally ingestible or liquid oral medicine commonly used clinically.
5. anti-tumor medicinal preparation of making as active component with the described Chinese paris rhizome yam type saponin of claim 1, it is characterized in that: described anti-tumor medicinal preparation is made up of the Chinese paris rhizome yam type saponin of 40%-60% and the common medicinal supplementary material of 60%-40%.
6. anti-tumor medicinal preparation according to claim 5 is characterized in that: described anti-tumor medicinal preparation is solid orally ingestible or liquid oral medicine commonly used clinically.
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| CN105726553A (en) * | 2016-01-28 | 2016-07-06 | 中国科学院昆明植物研究所 | Paris forrestii (Takht) H. Li. anti-cancer active component as well as pharmaceutical composition and application thereof |
| CN107854590B (en) * | 2016-09-22 | 2021-11-26 | 西南大学 | Sweet potato saponin extract and application thereof |
| CN108434245A (en) * | 2018-06-20 | 2018-08-24 | 广东工业大学 | A kind of plant button son eggplant extract and its preparation method and application |
| CN110787107B (en) * | 2019-11-19 | 2021-09-17 | 云南贝泰妮生物科技集团股份有限公司 | Preparation method and application of paris polyphylla shell extract |
| CN111454321A (en) * | 2020-04-30 | 2020-07-28 | 云南贝泰妮生物科技集团股份有限公司 | Method for separating and preparing high-purity saponin compound from paris polyphylla stems and leaves |
| CN114668773B (en) * | 2022-04-08 | 2023-10-03 | 山东中医药大学 | Application of paris polyphylla extract in resisting Crimedes congo hemorrhagic fever virus |
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| CN100500196C (en) * | 2006-06-30 | 2009-06-17 | 浙江大学 | Method for preparing paris polyphylla total saponin |
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