CN105982937A - Preparation method and medicinal application of Atractylodes lancea antitumor extract and composition thereof - Google Patents
Preparation method and medicinal application of Atractylodes lancea antitumor extract and composition thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of medicines, and concretely relates to a preparation method of a Uygur medicine Atractylodes lancea antitumor extract and a composition thereof, and an application of the extract in the preparation of medicines for preventing and treating breast cancer, lung cancer, stomach cancer, colorectal carcinoma, pancreas cancer, cervical carcinoma, brain glioma, liver cancer and other malignant tumors. The preparation method of the Atractylodes lancea antitumor extract comprises the following steps: eluting with a petroleum ether and ethyl acetate mixed solvent (with the volume ratio of petroleum ether to ethyl acetate of 100:0), eluting with a petroleum ether and ethyl acetate mixed solvent (with the volume ratio of petroleum ether to ethyl acetate of 100-1:100:4), and drying an eluate obtained after elution with the petroleum ether and acetone mixed solvent (with the volume ratio of petroleum ether to acetone of 100:1-100:4); or eluting with a petroleum ether and ethyl acetate mixed solvent (with the volume ratio of petroleum ether to ethyl acetate of 100:6), eluting with a petroleum ether and acetone mixed solvent (with the volume ratio of petroleum ether to acetone of 100:8), and drying an eluate obtained after elution with the petroleum ether and ethyl acetate mixed solvent (with the volume ratio of petroleum ether to ethyl acetate of 100:8) in order to obtain the extract.
Description
Technical field
The invention belongs to pharmaceutical technology field, be specifically related to the preparation of a kind of Uigurs medicine Rhizoma Atractylodis antineoplastic extract and combinations thereof thing
Method and its preparation prevent and treat hepatocarcinoma, pulmonary carcinoma, gastric cancer, colon cancer, cancer of pancreas, breast carcinoma, cervical cancer, cerebral glioma
Deng the application in malignant tumor medicine.
Background technology
This product is feverfew Rhizoma Atractylodis, Classification system Atractylodes Lancea (Thunb.) DC..Perennial herb
Plant.Root stock is flat sleeping or oblique ascension, thick long or generally in knob-like, the raw the most isometric or the most isometric adventitious roots such as most.Distribution
Heilungkiang, Liaoning, Jilin, the Inner Mongol, Hebei, Shanxi, Gansu, Shaanxi, Henan, Jiangsu, Zhejiang, Jiangxi, Anhui,
The ground such as Sichuan, Hunan, Hubei.Korea and the Far East Area of the Soviet Union also have distribution Rhizoma Atractylodis to be grown in sparse toothed oak birch woods, shrub forest belt more
In patana, shrubbery and woodland thick grass, see accompanying plant for dilute.Wherein Jiangsu is the major production areas of Atractylodes lancea (Thunb.) DC., is referred to as tunnel
Rhizoma Atractylodis producing region, one to adjusting for the whole nation.For retention of dampness in middle-JIAO, distension and fullness in the abdomen, have loose bowels, edema, tinea pedis flaccidity is preesed, rheumatic arthralgia,
Anemofrigid cold, nyctalopia, eyes dusk is puckery.
But, the most unclear to its antineoplastic effective composition, the present invention passes through systematically screening study, grey in research
It was unexpectedly observed that Rhizoma Atractylodis also have good breast carcinoma, cervical cancer, hepatocarcinoma, pulmonary carcinoma, gastric cancer, knot during art anti-tumor activity
The prevention of the malignant tumor such as intestinal cancer, cancer of pancreas, cerebral glioma and therapeutical effect, can apply prevention and the treatment of cancer.
Summary of the invention
Technical problem solved by the invention is to provide a kind of Rhizoma Atractylodis extract.
Present invention also offers the compositions with Rhizoma Atractylodis extract as main active.
Invention also provides the preparation of Rhizoma Atractylodis extract and combinations thereof thing and the application in preparing antitumor drug.
The present invention is achieved through the following technical solutions:
Uigurs medicine Rhizoma Atractylodis are through methanol supersound extraction, after extracting solution concentrates, with silica gel (SiO2) post separation, the silica gel after loading
Post, with petroleum ether: ethyl acetate mixed solvent (100:0-0:100) gradient elution (petroleum ether: ethyl acetate, concrete ratio
It is shown in Table 1), then again with methanol eluting, each petroleum ether: ethyl acetate ratio mixed solvent eluent, concentrate, after drying,
Anti tumor activity in vitro screening system is utilized to test its anti-tumor activity, it has unexpectedly been found that first with petroleum ether: ethyl acetate mixing is molten
Agent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting, continues with petroleum ether: ethyl acetate mixed solvent (petroleum ether:
Ethyl acetate, 100:1-100:4, volume ratio) eluting, petroleum ether: ethyl acetate 100:1-100:4 eluent is dried,
There is anti-tumor activity significantly.Preferably, first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:4, volume ratio) eluting,
Petroleum ether: ethyl acetate 100:1-100:4 eluent is drying to obtain.The compound of anti-tumor activity, can pass through above method,
It is enriched with, thus is separated with other impurities compositions.This active site from having no that document is reported, its 100:4 eluent
TLC analysis and characterization such as Fig. 1, TLC chromatographic condition: GF254Silica gel plate, development system: petroleum ether: ethyl acetate: acetone
(6:1:1), coloration method: vanillin-concentrated sulphuric acid colour developing.
Or Uigurs medicine Rhizoma Atractylodis are through methanol supersound extraction, first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:0-100:6, volume ratio) eluting, continues with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8,
Volume ratio) eluting, petroleum ether: ethyl acetate 100:8 eluent is dried, has anti-tumor activity significantly.Preferably,
First with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting, continue with petroleum ether:
Ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting, petroleum ether: ethyl acetate 100:8 is washed
De-liquid after drying and get final product.The compound of anti-tumor activity, can pass through above method, be enriched with, thus with other impuritiess
Composition is separated.This active site from having no that document is reported, TLC analysis and characterization such as Fig. 2, TLC of its 100:8 eluent
Chromatographic condition: GF254Silica gel plate, development system: petroleum ether: ethyl acetate: acetone (6:1:1), coloration method: vanillin
-concentrated sulphuric acid develops the color.
Specifically, discovery procedure is as follows:
1, Uigurs medicine Rhizoma Atractylodis are through the preparation of methanol sonicated extract
Taking Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol supersound extraction 15min, after extracting solution concentrates, obtaining extract must extract
Thing SN0135A, loading SN0135A:1.8499g, keep sample SN0135A:0.0975g.
2, petroleum ether: ethyl acetate mixed solvent gradient elution method and result
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol supersound extraction 15min, after extracting solution concentrates, obtain extract SN0135A,
Loading SN0135A:1.8499g, keep sample SN0135A:0.0975g, and methanol dissolves, and mixes sample silica gel 3.0g, blank silica gel 10g,
Glass column internal diameter 2cm, petroleum ether-ethyl acetate system is washed
De-(condition is shown in Table 1), column volume 25ml, each gradient elution 200ml, obtain, each concentration extracts the eluting of eluent
Thing, recycling design, to obtain final product, petroleum ether: ethyl acetate gradient extract, yield is shown in Table 1, and TLC analysis result is shown in Fig. 3,
Fig. 4, TLC chromatographic condition: GF254Silica gel plate, development system: petroleum ether: ethyl acetate: acetone (6:1:1), colour developing side
Method: vanillin-concentrated sulphuric acid colour developing.
Table 1
| Gradient (stone: second) | Elution volume (ml) | Numbering |
| 100:00 | 200 | SN0135A01 |
| 100:01 | 200 | SN0135A02 |
| 100:02 | 200 | SN0135A03 |
| 100:03 | 200 | SN0135A04 |
| 100:04 | 200 | SN0135A05 |
| 100:05 | 200 | SN0135A06 |
| 100:06 | 200 | SN0135A07 |
| 100:08 | 200 | SN0135A08 |
| 100:10 | 200 | SN0135A09 |
| 100:12 | 200 | SN0135A10 |
| 100:14 | 200 | SN0135A11 |
| 100:17 | 200 | SN0135A12 |
| 100:20 | 200 | SN0135A13 |
| 100:25 | 200 | SN0135A14 |
| 100:30 | 200 | SN0135A15 |
| 100:50 | 200 | SN0135A16 |
| 100:100 | 200 | SN0135A17 |
| 0:100 | 200 | SN0135A18 |
| Pure methanol | 200 | SN0135A19 |
3, antitumor activity screening method and result
1) experiment condition
A) cell strain information
Rat glioma C6 is purchased from China typical culture collection center cell bank
B) medicine and reagent
Under sample aseptic condition, it is 100mg/mL that DMSO dissolving is configured to mother liquid concentration, uses RPMI-1640 culture fluid during use
It is diluted to desired concn (DMSO≤1 ‰).
RPMI Medium 1640 culture medium dry powder is purchased from GIBCO company of the U.S..Hyclone is purchased from Beijing unit Heng Shengma biology skill
Art institute.Trypsin 1:250, dimethyl diphenyl tetrazole bromide (MTT).
C) instrument
CO2Incubator (SANYO, Japan)
Vertical laminar flow clean bench (upper marine clean cleaning equipment company limited)
Inverted biological microscope (Chongqing Optical & Electrical Instrument Co., Ltd.)
Low high speed desk centrifuge (Anting Scientific Instrument Factory, Shanghai)
Electronic balance (Ao Haosi Instrument Ltd.)
Microplate reader (Bole life medical product company limited)
Vertical pressure steam sterilizer (Shenan Medical Appliances Factory, Shanghai)
Air dry oven (Shanghai leap medical apparatus and instruments factory)
PH meter (SARTORIUS, Germany)
2) experimental technique and process
Rat glioma C6 is laid on 96 orifice plates, every hole 100ul with the density in 4000/ hole, uses after 12h.Each component is with DMSO
Be dissolved as 100mg/mL store liquid, be stored in-20 DEG C stand-by.12h after bed board, observation of cell converges rate and is about 40%, dosing,
Concentration is 100 μ g/mL, the multiple hole of each component 3.Every plate cell sets up two matched group (culture medium+cells；Contain
0.1%DMSO culture medium+cell), 3 blank well (only culture medium).Addition medicine, after 24 hours, adds 20 μ l tetramethyls
Azo azoles salt chemical name is 3-(4,5-dimethylthiazole)-2,5-diphenyltetrazolium bromide bromide
(3-(4,5-dimethyl-2thiazolyl)-2,5-diphenyl-tetrazolium bromide, MTT), continues cultivation 4
Hour.Abandoning supernatant completely, adds 100 μ l DMSO, and mixing makes MTT be completely dissolved, removes bubble.490nm measures OD
Value.
3) experimental result
Table 2
Found that:
The preferred version of the present invention is as follows: Uigurs medicine Rhizoma Atractylodis, through methanol supersound extraction, after extracting solution concentrates, divide with silicagel column
From, the silicagel column after loading, with petroleum ether: ethyl acetate mixed solvent gradient elution (petroleum ether: ethyl acetate, be shown in by ratio
Table 1), each petroleum ether: ethyl acetate ratio mixed solvent eluent, concentrate, after drying, utilize anti tumor activity in vitro to sieve
System is selected to test its anti-tumor activity, it has unexpectedly been found that first petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:0, volume ratio) eluting, continues with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:4, volume
Than) eluting, petroleum ether: ethyl acetate 100:4 eluent is dried, has anti-tumor activity significantly.That is, antitumor is lived
The compound of property, can pass through above method, be enriched with, thus separate with other impurities compositions.This active site from
Have no that document is reported, its TLC analysis and characterization such as Fig. 1.
Uigurs medicine Rhizoma Atractylodis are through methanol supersound extraction, after extracting solution concentrates, separate with silicagel column, the silicagel column after loading, use stone
Oil ether: ethyl acetate mixed solvent gradient elution (petroleum ether: ethyl acetate, ratio is shown in Table 1), each petroleum ether: acetic acid second
Ester ratio mixed solvent eluent, concentrates, and after drying, utilizes anti tumor activity in vitro screening system to test its anti-tumor activity,
It is surprised to find that first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting, continues
With petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting, petroleum ether: acetic acid second
Ester 100:8 eluent is dried, has anti-tumor activity significantly, i.e. the compound of anti-tumor activity, can pass through more than
Method, is enriched with, thus separates with other impurities compositions.This active site is from having no that document is reported, its TLC analyzes
Characterize such as Fig. 2.
4, the Study on Extraction Method of antitumor effective extract
1) Research on kinds of Extraction solvent
Organic with methanol, ethanol, acetone, chloroform, ethyl acetate, methanol-water mixed solvent, ethanol water mixed solvent etc. respectively
Solvent extraction, and the anti-tumor activity that Test extraction thing is to C6 cell, result is as follows:
Table 3
Result of study shows: extraction organic solvent can be methanol, ethanol, acetone, chloroform, ethyl acetate, methanol-water mix
Bonding solvent, ethanol water mixed solvent.
2) Extraction solvent use quantity research
Respectively with 1,2,5,10,20,30,40,50 times of (weight/volume) organic solvent extraction, and Test extraction
The anti-tumor activity of thing, result is as follows:
Table 4
Extract extraction consumption of organic solvent is 2-50 times (weight/volume) of medical material weight.
3) research of drying means
The methods such as seasoning are steamed, to obtain respectively with boulton process, freeze-drying, forced air drying, centrifugal drying, rotation
Antitumor active site is dried, with water content, TLC, active testing as index, find boulton process, freeze-drying,
Forced air drying, centrifugal drying, rotation are steamed seasoning and are applicable to be dried C6 cell anti-tumor activity extract, wherein, optimum
For boulton process, freeze-drying.
Table 5
| Sample 20g | Boulton process | Freeze-drying | Forced air drying method | Centrifugal drying method | Seasoning is steamed in rotation |
| Water content (%) | 7.9 | 8.9 | 10.7 | 13.5 | 10.0 |
| Suppression ratio (%) | 44.2 | 33.4 | 24.8 | 21.8 | 35.9 |
Therefore, the preparation method of Rhizoma Atractylodis antineoplastic extract is:
Uigurs medicine Rhizoma Atractylodis are through organic solvent supersound extraction, after extracting solution concentrates, separate with silicagel column, the silicagel column after loading,
First with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) 2-50 times of column volume of eluting,
Continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:4, volume ratio) 2-50 times of column volume of eluting.
Petroleum ether: the recovered organic solvent of ethyl acetate 100:4 eluent, is dried, is this extract.Wherein optimum for first using stone
Oil ether: 10 times of column volumes of ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:4, volume ratio) eluting, continues and uses stone
Oil ether: 15 times of column volumes of ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:4, volume ratio) eluting.
Wherein,
1) extract extraction solvent can be methanol, ethanol, acetone, chloroform, ethyl acetate, methanol-water mixed solvent, ethanol
Water mixed solvent, optimal conditions is methanol and 95% ethanol.Extract extraction consumption of organic solvent is the 2-50 of medical material weight
Again (weight/volume).
2) extract drying means can be boulton process, freeze-drying, forced air drying, centrifugal drying, rotation steaming seasoning etc.,
Optimum is boulton process, freeze-drying.
Uigurs medicine Rhizoma Atractylodis are through methanol supersound extraction, after extracting solution concentrates, separate with silicagel column, the silicagel column after loading, use stone
Oil ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) 2-50 times of column volume of eluting eluting,
Continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) 2-50 times of post of eluting eluting
Volume.Petroleum ether: the recovered organic solvent of ethyl acetate 100:8 eluent, is dried, is this extract.Conditions above is
Excellent is first with petroleum ether: 10 times of cylinders of ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting
Long-pending, continue with petroleum ether: 15 times of cylinders of ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting
Long-pending.Wherein,
1) extract extraction solvent can be methanol, ethanol, acetone, chloroform, ethyl acetate, methanol-water mixed solvent, ethanol
Water mixed solvent, optimal conditions is methanol and 95% ethanol.Extract extraction consumption of organic solvent is the 2-50 of medical material weight
Again (weight/volume).
2) extract drying means can be boulton process, freeze-drying, forced air drying, centrifugal drying, rotation steaming seasoning etc.,
Optimum is boulton process, freeze-drying.
5. Rhizoma Atractylodis antitumor effective extract is (first with the petroleum ether of 100:0: ethyl acetate eluting, then with the stone of 100:4
Oil ether: the extract obtained after ethyl acetate eluting) antitumor activity
Utilize various tumor cell, such as breast carcinoma, pulmonary carcinoma, gastric cancer, colon cancer, cancer of pancreas, cervical cancer, cerebral glioma, liver
The Cell lines such as cancer, test the anti-tumor activity of Rhizoma Atractylodis antineoplastic extract, IC respectively50Result is as follows:
Table 6
Therefore, it has been found that Rhizoma Atractylodis antineoplastic extract possesses anti-tumor activity, it is expected to for various tumors such as hepatocarcinoma, pulmonary carcinoma,
The prevention of the malignant tumor such as gastric cancer, intestinal cancer, cerebral glioma and treatment.
6, compositions of Rhizoma Atractylodis antitumor effective extract and preparation method thereof research
1) solid dispersion
Prescription
Preparation method:
Weigh Rhizoma Atractylodis extract and carrier polyvinylpyrrolidone (PVP) in proportion, the mass ratio of 1:2,1:4,1:6 respectively
Putting in beaker, add dehydrated alcohol, magnetic stirrer to Rhizoma Atractylodis extract and carrier are completely dissolved, and proceed to rotation and steam instrument
Middle removing organic solvent, dry, pulverize 80 mesh sieves, obtained Rhizoma Atractylodis extract PVP clathrate.
2) cyclodextrin clathrate
Prescription:
Preparation method:
Beta-schardinger dextrin-and 1～5 times of water are ground well, add Rhizoma Atractylodis extract (slightly water-soluble should be first dissolved in a small amount of organic solvent
In) be fully ground to becoming pastel, cold drying and get final product.
3) dispersible tablet prescription:
Preparation method:
1. the preparation of Rhizoma Atractylodis extract starch dispersions, precision weighs Rhizoma Atractylodis extract extract, adds appropriate lauryl sulphate acid
Sodium, after the ethanol with 70% dissolves the soluble starch mix homogeneously adding equal proportion, is evaporated, powder at a temperature of 70 DEG C
Broken, cross 100 mesh sieves；
2. weigh recipe quantity, Rhizoma Atractylodis extract starch dispersions, polyvinylpolypyrrolidone, pregelatinized Starch, make wetting agent with 70% ethanol,
Stir while adding, make wet granular and cross 14 mesh sieves, after ambient temperatare puts 15min, 60 DEG C of oven for drying 45min,
16 mesh sieve granulate, add Pulvis Talci and differential silica gel, after mix homogeneously, tabletting.
7, the detection method research of Rhizoma Atractylodis antitumor effective extract
It was found that can detect and indicate the feature of Rhizoma Atractylodis antineoplastic extract well by the method for thin layer chromatography, see Fig. 1,
Fig. 2.
Actual conditions is: GF254Silica gel plate, development system: petroleum ether: ethyl acetate: acetone (6:1:1) coloration method: vanillin
-concentrated sulphuric acid develops the color.
Accompanying drawing illustrates:
The TLC chromatogram of Fig. 1 Rhizoma Atractylodis activity extract；
The TLC chromatogram of Fig. 2 Rhizoma Atractylodis activity extract；
The TLC chromatogram of the chemical constituent that Fig. 3 Rhizoma Atractylodis obtain；
The TLC chromatogram of the chemical constituent that Fig. 4 Rhizoma Atractylodis obtain.
Instantiation
Following example represent the practicality of the present invention, and the present invention is not limited.
Embodiment 1:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol supersound extraction 15min, after extracting solution concentrates, separates with silicagel column, loading
After silicagel column (2.0cm internal diameter pillar), first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 10 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:4 eluent, vacuum drying, it is
This extract.
Embodiment 2:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol ultrasonic extraction 15min, after extracting solution concentrates, separates with silicagel column, loading
After silicagel column (2.0cm internal diameter pillar), first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 10 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:4 eluent, lyophilization, is
This extract.
Embodiment 3:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml acetone supersound extraction 15min, after extracting solution concentrates, separates with silicagel column, loading
After silicagel column (2.0cm internal diameter pillar), first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 10 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:4 eluent, forced air drying, is
This extract.
Embodiment 4:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml chloroform supersound extraction 15min, after extracting solution concentrates, separates with silicagel column, loading
After silicagel column (2.0cm internal diameter pillar), first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 10 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:0,
Volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:4 eluent, centrifugal drying, is
This extract.
Embodiment 5:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethyl acetate supersound extraction 15min, after extracting solution concentrates, separates with silicagel column,
Silicagel column (2.0cm internal diameter pillar) after loading, first with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:0, volume ratio) 10 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:0, volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:4 eluent, rotation is evaporated dry,
It is this extract.
Embodiment 6:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol-water mixed solvent (methanol: water=1:1) supersound extraction 15min, extracting solution
After concentration, separate with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, first with petroleum ether: ethyl acetate mixes
10 times of column volumes of solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting, continue with petroleum ether: ethyl acetate mixes
15 times of column volumes of solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting.Petroleum ether: acetone 100:4 eluent
Recovered organic solvent, lyophilization, it is this extract.
Embodiment 7:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol water mixed solvent (ethanol: water=1:1) supersound extraction 15min, extracting solution
After concentration, separate with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, first with petroleum ether: ethyl acetate mixes
10 times of column volumes of solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting, continue with petroleum ether: ethyl acetate mixes
15 times of column volumes of solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting.Petroleum ether: acetone 100:4 eluent
Recovered organic solvent, vacuum drying, it is this extract.
Embodiment 8:
Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol water mixed solvent (ethanol: water=90:10) supersound extraction 15min, extracts
After liquid concentrates, separate with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, first with petroleum ether: ethyl acetate is mixed
10 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting, continue with petroleum ether: ethyl acetate is mixed
15 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:0, volume ratio) eluting.Petroleum ether: acetone 100:4 eluting
The recovered organic solvent of liquid, lyophilization, it is this extract.
Embodiment 9:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol supersound extraction 15min, after extracting solution concentrates, separate with silicagel column, loading
After silicagel column (2.0cm internal diameter pillar), with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:6,
Volume ratio) 20 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate, 100:8, body
Long-pending ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:8 eluent, vacuum drying, it is this and carries
Take thing.
Embodiment 10:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol ultrasonic extraction 15min, after extracting solution concentrates, separate with silicagel column,
Silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:6, volume ratio) 20 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:8, volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:8 eluent, lyophilization,
It is this extract.
Embodiment 11:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml acetone supersound extraction 15min, after extracting solution concentrates, separate with silicagel column,
Silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:6, volume ratio) 20 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:8, volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:8 eluent, forced air drying,
It is this extract.
Embodiment 12:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml chloroform supersound extraction 15min, after extracting solution concentrates, separate with silicagel column,
Silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:6, volume ratio) 20 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: ethyl acetate,
100:8, volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:8 eluent, centrifugal drying,
It is this extract.
Embodiment 13:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethyl acetate supersound extraction 15min, after extracting solution concentrates, divide with silicagel column
From, the silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate mixed solvent (petroleum ether: acetic acid second
Ester, 100:6, volume ratio) 20 times of column volumes of eluting, continue with petroleum ether: ethyl acetate mixed solvent (petroleum ether: acetic acid second
Ester, 100:8, volume ratio) 15 times of column volumes of eluting.Petroleum ether: the recovered organic solvent of acetone 100:8 eluent, rotation is steamed
It is dried, is this extract.
Embodiment 14:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml methanol-water mixed solvent (methanol: water=1:1) supersound extraction 15min, carry
After taking liquid concentration, separate with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate is mixed
20 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting, continue with petroleum ether: ethyl acetate is mixed
15 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting.Petroleum ether: acetone 100:8 eluting
The recovered organic solvent of liquid, lyophilization, it is this extract.
Embodiment 15:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol water mixed solvent (ethanol: water=1:1) supersound extraction 15min, carry
After taking liquid concentration, separate with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate is mixed
20 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting, continue with petroleum ether: ethyl acetate is mixed
15 times of column volumes of bonding solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting.Petroleum ether: acetone 100:8 eluting
The recovered organic solvent of liquid, vacuum drying, it is this extract.
Embodiment 16:
Take Uigurs medicine Rhizoma Atractylodis 20g, through 100ml ethanol water mixed solvent (ethanol: water=90:10) supersound extraction 15min,
After extracting solution concentrates, separating with silicagel column, the silicagel column (2.0cm internal diameter pillar) after loading, with petroleum ether: ethyl acetate
20 times of column volumes of mixed solvent (petroleum ether: ethyl acetate, 100:6, volume ratio) eluting, continue with petroleum ether: ethyl acetate
15 times of column volumes of mixed solvent (petroleum ether: ethyl acetate, 100:8, volume ratio) eluting.Petroleum ether: acetone 100:8 washes
The de-recovered organic solvent of liquid, lyophilization, it is this extract.
Embodiment 17: solid dispersion
Weigh Rhizoma Atractylodis extract and carrier polyvinylpyrrolidone (PVP) in proportion, the mass ratio of 1:2,1:4,1:6 respectively
Putting in beaker, add dehydrated alcohol, magnetic stirrer to Rhizoma Atractylodis extract and carrier are completely dissolved, and proceed to rotation and steam instrument
Middle removing organic solvent, dry, pulverize 80 mesh sieves, obtained Rhizoma Atractylodis extract PVP clathrate.
Embodiment 18: cyclodextrin clathrate
Beta-schardinger dextrin-and 1～5 times of water are ground well, add Rhizoma Atractylodis extract (slightly water-soluble should be first dissolved in a small amount of organic solvent
In) be fully ground to becoming pastel, cold drying and get final product.
Embodiment 19: dispersible tablet
1. weigh dry Rhizoma Atractylodis extract, add appropriate sodium lauryl sulphate, use the ethanol of 70% fully to dissolve, add water
Soluble starch and Rhizoma Atractylodis extract (1:1), be uniformly mixed, dry, pulverize at 70 DEG C, crosses 100 mesh sieves,
Obtain Rhizoma Atractylodis extract dispersion.
2. precision weighs recipe quantity, Rhizoma Atractylodis extract dispersion, polyvinylpolypyrrolidone, amylum pregelatinisatum, makees wetting agent with 70% ethanol,
Stirring while adding, 14 mesh sieves make wet granular, after ambient temperatare puts 15min, and 70 DEG C of oven for drying 45min, 16 mesh
Sieve granulate, adds Pulvis Talci and differential silica gel, after mix homogeneously, tabletting.
Claims (10)
1. a Uigurs medicine Rhizoma Atractylodis extract, it is characterized by, Uigurs medicine Rhizoma Atractylodis are through organic solvent supersound extraction, after extracting solution concentrates, separate with silicagel column, the silicagel column after loading, first with the petroleum ether of volume ratio 100:0: ethyl acetate mixed solvent eluting, continue with the petroleum ether of volume ratio 100:1-100:4: ethyl acetate mixed solvent eluting, petroleum ether: ethyl acetate 100:1-100:4 eluent is drying to obtain；
Or first with the petroleum ether of volume ratio 100:0-100:6: ethyl acetate mixed solvent eluting, continues with the petroleum ether of volume ratio 100:8: acetone mixed solvent eluting, petroleum ether: ethyl acetate 100:8 eluent is drying to obtain.
2. Uigurs medicine Rhizoma Atractylodis extract as claimed in claim 1, it is characterized by, first with the petroleum ether of volume ratio 100:0: ethyl acetate mixed solvent eluting, continue with the petroleum ether of volume ratio 100:4: ethyl acetate mixed solvent eluting, petroleum ether: ethyl acetate 100:4 eluent is dried；
Or first with the petroleum ether of volume ratio 100:6: ethyl acetate mixed solvent gradient elution eluting, continues with the petroleum ether of volume ratio 100:8: ethyl acetate mixed solvent eluting, petroleum ether: ethyl acetate 100:8 eluent is dried.
3. Uigurs medicine Rhizoma Atractylodis extract as claimed in claim 1 or 2, is characterized by, extraction solvent is methanol, ethanol, acetone, chloroform, ethyl acetate, methanol-water mixed solvent or ethanol water mixed solvent.
4. the Uigurs medicine Rhizoma Atractylodis extract as described in claim 1-3 any one, is characterized by, petroleum ether: second
The elution volume of acetoacetic ester mixed solvent is 2-50 times of column volume.
5. the Uigurs medicine Rhizoma Atractylodis extract as described in claim 1-4 any one, is characterized by, first with petroleum ether: 10 times of column volumes of ethyl acetate mixed solvent eluting, then with petroleum ether: 15 times of column volumes of ethyl acetate mixed solvent.
6. a pharmaceutical composition, it is characterised in that comprise the extract described in claim 1-5 any one and pharmaceutically acceptable carrier.
7. a pharmaceutical preparation, it is characterised in that comprise the Rhizoma Atractylodis extract described in claim 1-5 any one or the pharmaceutical composition described in claim 6.
8. the Rhizoma Atractylodis extract described in claim 1-5 any one or the compositions described in claim 6 or the application in preparing antitumor drug of the pharmaceutical preparation described in claim 7.
Applying the most as claimed in claim 9, it is characterized by, described tumor is breast carcinoma, pulmonary carcinoma, gastric cancer, colon cancer, cancer of pancreas, cervical cancer, cerebral glioma or hepatocarcinoma.
10. the Rhizoma Atractylodis extract as described in claim 1-5 any one, it is characterised in that detecting by TLC method, its chromatographic condition is: GF254Silica gel plate, development system: petroleum ether: ethyl acetate: acetone (6:1:1) coloration method: vanillin-concentrated sulphuric acid colour developing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113274420A (en) * | 2021-04-27 | 2021-08-20 | 苏州科技大学 | Method for targeted screening of atractylis lancea breast cancer resistant active ingredients |
| CN114452280A (en) * | 2021-11-11 | 2022-05-10 | 杭州师范大学 | Application of atractylone in preparation of Sirt3 gene activator |
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2015
- 2015-02-15 CN CN201510079852.9A patent/CN105982937A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 赵余庆等: "《食疗与保健食品原料功能因子手册》", 31 March 2013, 中国医药科技出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113274420A (en) * | 2021-04-27 | 2021-08-20 | 苏州科技大学 | Method for targeted screening of atractylis lancea breast cancer resistant active ingredients |
| CN114452280A (en) * | 2021-11-11 | 2022-05-10 | 杭州师范大学 | Application of atractylone in preparation of Sirt3 gene activator |
| CN114452280B (en) * | 2021-11-11 | 2023-11-03 | 杭州师范大学 | Application of atractylone in preparation of glioma treatment drug |
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Application publication date: 20161005 |