CN105106259A - Method for preparing colon cancer resistance notopterygium extract powder in scale mode - Google Patents
Method for preparing colon cancer resistance notopterygium extract powder in scale mode Download PDFInfo
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- CN105106259A CN105106259A CN201510586059.8A CN201510586059A CN105106259A CN 105106259 A CN105106259 A CN 105106259A CN 201510586059 A CN201510586059 A CN 201510586059A CN 105106259 A CN105106259 A CN 105106259A
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- radix notopterygii
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Abstract
The invention relates to a method for preparing colon cancer resistance notopterygium extract powder in a scale mode, which comprises steps: 1 exaction: notopterygium medical materials are extracted by alcohol and filtered after being smashed, and is decompress and dried to be a paste state, thereby obtaining notopterygium alcohol extract; 2 liquid-liquid distribution enrichment: the notopterygium alcohol extract is smashed, extracted, decompressed and dried to obtain a notopterygium ethyl acetate position; 3 resin column chromatography edulcoration: the notopterygium ethyl acetate position is separated through a resin column after being dissolved, is eluted in a gradient mode, 90% methanol contents are collected, the 90% methanol contents are decompressed and dried to obtain notopterygium extract coarse powder; 4 silica gel column chromatography separation: the notopterygium extract coarse powder is separated and eluted through a silica gel column chromatography after being dissolved, and is detected through a thin-layer chromatography, and fractions which are 0.1-0.8 in radio frequency (Rf) values are collected, id decompressed and dried to obtain yellow powder-shaped notopterygium extract powder. The method for preparing the colon cancer resistance notopterygium extract powder in the scale mode is simple in process, easy to carry out in a scale mode and is steady and controllable in quality.
Description
Technical field
The present invention relates to pharmaceutical chemistry and biomedicine technical field, particularly relate to a kind of large-scale preparation method of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder.
Background technology
Rhizoma Et Radix Notopterygii (
notopterygiumincisumtingexH.TChang) be dry root and the supporting root of Umbelliferae (Umbelliferae) Notopterygium (Notopterygium) plant, be mainly distributed in the ground such as Sichuan, Yunnan, Qinghai and Gansu.Modern study shows that in Rhizoma Et Radix Notopterygii, chemical composition mainly comprises monoterpenes, sesquiterpenoids, Phenylpropanoid Glycosides class, Coumarins, amino acids, organic acid and organic acid ester, and wherein coumarin kind compound is known by people with its significant anti-tumor activity.
At present, Chinese patent (102367256A) report adopts that supercritical carbon dioxide extraction method extracts, crystallization two step obtains Rhizoma Et Radix Notopterygii isoimperatorin extract, but the research that inhibitor against colon carcinoma cells extract powder is prepared in scale from Rhizoma Et Radix Notopterygii has no bibliographical information.
Summary of the invention
Technical problem to be solved by this invention is to provide the large-scale preparation method of the inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder that a kind of technique is simple, easily scale is implemented, repeatability is better, stable and controllable for quality.
For solving the problem, the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder of the present invention, comprises the following steps:
Extract: after the order of Rhizoma Et Radix Notopterygii pulverizing medicinal materials to 60 ~ 120, add volume fraction be 95% alcoholic solution or methanol solution carry out alcohol extraction, obtain filtrate after filtration; This filtrate to paste, obtains Notopterol extract through drying under reduced pressure;
(2) liquid liquid distributes enrichment: the analytical pure aqueous dispersion of its quality 30 ~ 50 times of described Notopterol extract, obtains dispersion liquid; This dispersion liquid extraction into ethyl acetate 3 times of its 30 ~ 50 times of volumes, merges and obtains acetic acid ethyl acetate extract; Described acetic acid ethyl acetate extract obtains Rhizoma Et Radix Notopterygii ethyl acetate extract through drying under reduced pressure;
(3) resin column chromatography remove impurity: the volume fraction adding its quality 2 ~ 5 times in described Rhizoma Et Radix Notopterygii ethyl acetate extract be 5 ~ 20% methanol solution dissolve, then be separated through resin column, and with aqueous solution, volume fraction be successively 90% methanol solution carry out gradient elution by the column volume of 2 ~ 5 times, collect 90% methanol-eluted fractions thing; Namely this 90% methanol-eluted fractions thing obtains Rhizoma Et Radix Notopterygii extractum coarse powder through drying under reduced pressure;
Silica gel column chromatography be separated: add in described Rhizoma Et Radix Notopterygii extractum coarse powder its quality 2 ~ 5 times of volume fractions be 80 ~ 100% methanol solution dissolve, after silica gel column chromatography is separated, with the chloroform-methanol mixed solvent eluting of 5 ~ 10 times of column volumes, fraction is collected by every part of 500 ~ 1000mL, and detect through thin layer chromatography, wherein developing solvent be chloroform, the mixed solvent that mixes by the volume ratio of 5:5 of methanol, developer is the concentrated sulphuric acid alcoholic solution of volumetric concentration 10%, and merging Rf value is the fraction of 0.1 ~ 0.8; Described Rf value be the fraction of 0.1 ~ 0.8 through drying under reduced pressure, obtain the Rhizoma Et Radix Notopterygii extract powder in yellow powder.
Described step (1) middle alcohol extraction condition refers to that solid-liquid ratio is 1kg:10 ~ 20L, temperature is 60 DEG C ~ 95 DEG C, extraction time is 1 ~ 3 time, extraction time is 1 ~ 3h at every turn.
Described step (1), described step (2), described step (3) and described step (4) in drying under reduced pressure condition all refer to that vacuum is 0.06 ~ 0.09MPa, temperature is 50 ~ 65 DEG C.
Described step (3) middle resin column is the one in HP20 type resin column, HP20SS type resin column or MCI type resin column.
Described step (4) middle chloroform-methanol mixed solvent refers to the solvent that chloroform and methanol mix by the volume ratio of 8:2 ~ 2:8.
Described step (4) middle silicagel column is of a size of 30mm ~ 60mm × 60mm ~ 100mm.
The Rhizoma Et Radix Notopterygii extract powder that the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as above obtains is preparing the application in drugs against colon cancer or health food; it is characterized in that: this Rhizoma Et Radix Notopterygii extract powder makes all kinds of inhibitor against colon carcinoma cells pharmaceutical formulation with pharmaceutically acceptable any carrier according to a conventional method as active component, or make all kinds of health-related food with acceptable any carrier in Food Science according to a conventional method as active component.
The present invention compared with prior art has the following advantages:
1, the present invention adopts 95% alcoholic solution or methanol solution to extract, and dissolving can be recycled, and average unit cost is cheap, and easily scale is implemented.
2, the present invention adopts ethyl acetate extract in liquid liquid apportion design enrichment Rhizoma Et Radix Notopterygii, and solvent is cheap, and can regeneration cycle use, and is easy to scale.
3, resin column of the present invention can regeneration cycle use, and resin has effect of decolouring simultaneously, and the response rate is higher.
4, the present invention adopts silica gel column chromatography to be separated, and can directly volatility class component in Rhizoma Et Radix Notopterygii be separated with target compound, removes the strong polar impurity of part simultaneously.
5, ingredient requirement of the present invention is not high, on open market or wild raw material, is easy to batch and gets the raw materials ready.
6, present invention process is simple, repeatability is better, stable and controllable for quality, the Rhizoma Et Radix Notopterygii extract powder obtained, through two-dimentional preparative hplc separation and purification and NMR hydrogen spectrum, carbon analysis of spectrum, judges main containing isoimperatorin, bergapton and other coumarin kind compounds successively.
7, the Rhizoma Et Radix Notopterygii extract powder that obtains of the present invention after tested, has the effect of good inhibitor against colon carcinoma cells.
(1) experimental technique adopts international MTT assay method to carry out: first, and 96 porocyte plates inoculate 2 × 10
4the colon cancer cell HCT116 of individual exponential phase, 3 multiple holes, after cell attachment; Add variable concentrations testing sample again, 7 drug concentration gradient are set altogether, are respectively: this Rhizoma Et Radix Notopterygii extract powder sample sets of 1.0 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, 20 μ g/mL, 30 μ g/mL, 40 μ g/mL and 50 μ g/mL; After 72 hours, in 96 orifice plate corresponding apertures, add the MTT solution 20 μ L of 5mg/mL, continue to cultivate 3h; Discard supernatant in 96 orifice plates, add 100 μ LDMSO and dissolve, use the light absorption value under microplate reader detection 570nm wavelength and calculate the half-inhibition concentration IC of testing sample to Growth of Colon Cancer Cells
50.
(2) experimental result shows,
embodiment 1 ~ 3group Rhizoma Et Radix Notopterygii extract powder all has obvious inhibitory action to colon cancer cell line, and be followed successively by 39.6 μ g/mL, 38.9 μ g/mL, 39.3 μ g/mL, meansigma methods is 39.3 μ g/mL.
Detailed description of the invention
embodiment 1a large-scale preparation method for inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder, comprises the following steps:
Extract: after 5.0Kg Rhizoma Et Radix Notopterygii pulverizing medicinal materials to 60 order, add volume fraction be 95% alcoholic solution or methanol solution carry out alcohol extraction, obtain filtrate after filtration; This filtrate vacuum be 0.06MPa, temperature be the condition of 65 DEG C under through drying under reduced pressure to paste, obtain Notopterol extract 984.6g.
Wherein: alcohol extraction condition refers to that solid-liquid ratio is 1kg:10L, temperature is 95 DEG C, extraction time is 3 times, extraction time is 1h at every turn.
(2) liquid liquid distributes enrichment: the analytical pure aqueous dispersion of its quality 30 times of Notopterol extract, obtains dispersion liquid; This dispersion liquid extraction into ethyl acetate 3 times of its 30 times of volumes, merges and obtains acetic acid ethyl acetate extract; Acetic acid ethyl acetate extract vacuum be 0.06MPa, temperature obtains Rhizoma Et Radix Notopterygii ethyl acetate extract 378.1g through drying under reduced pressure under being the condition of 65 DEG C.
(3) resin column chromatography remove impurity: the volume fraction adding its quality 2 times in Rhizoma Et Radix Notopterygii ethyl acetate extract be 20% methanol solution dissolve, then be separated through resin column, and with aqueous solution, volume fraction be successively 90% methanol solution carry out gradient elution by the column volume of 2 times, collect 90% methanol-eluted fractions thing; This 90% methanol-eluted fractions thing vacuum be 0.06MPa, namely temperature obtain Rhizoma Et Radix Notopterygii extractum coarse powder 328.6g through drying under reduced pressure under being the condition of 65 DEG C.
Wherein: resin column is HP20 type resin column.Rhizoma Et Radix Notopterygii ethyl acetate extract and resin ratio are 1g:30mL.
Silica gel column chromatography be separated: add in Rhizoma Et Radix Notopterygii extractum coarse powder its quality 5 times of volume fractions be 80% methanol solution dissolve, after silica gel column chromatography is separated, with the chloroform-methanol mixed solvent eluting of 5 times of column volumes, fraction is collected by every part of 500mL, and detect through thin layer chromatography, wherein developing solvent be chloroform, the mixed solvent that mixes by the volume ratio (mL/mL) of 5:5 of methanol, developer is the concentrated sulphuric acid alcoholic solution of volumetric concentration 10%, and merging Rf value is the fraction of 0.1 ~ 0.8; Rf value be 0.1 ~ 0.8 fraction vacuum be 0.06MPa, temperature be the condition of 65 DEG C under through drying under reduced pressure, obtain the Rhizoma Et Radix Notopterygii extract powder 227.4g in yellow powder.
Wherein: chloroform-methanol mixed solvent refers to the solvent that chloroform and methanol mix by the volume ratio (mL/mL) of 2:8.
Silicagel column is of a size of 30mm × 60mm.
embodiment 2a large-scale preparation method for inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder, comprises the following steps:
Extract: after 10.0Kg Rhizoma Et Radix Notopterygii pulverizing medicinal materials to 120 order, add volume fraction be 95% alcoholic solution or methanol solution carry out alcohol extraction, obtain filtrate after filtration; This filtrate vacuum be 0.09MPa, temperature be the condition of 50 DEG C under through drying under reduced pressure to paste, obtain Notopterol extract 1921.9g.
Wherein: alcohol extraction condition refers to that solid-liquid ratio is 1kg:20L, temperature is 60 DEG C, extraction time is 1 time, extraction time is 3h at every turn.
(2) liquid liquid distributes enrichment: the analytical pure aqueous dispersion of its quality 50 times of Notopterol extract, obtains dispersion liquid; This dispersion liquid extraction into ethyl acetate 3 times of its 50 times of volumes, merges and obtains acetic acid ethyl acetate extract; Acetic acid ethyl acetate extract vacuum be 0.09MPa, temperature obtains Rhizoma Et Radix Notopterygii ethyl acetate extract 738.6g through drying under reduced pressure under being the condition of 50 DEG C.
(3) resin column chromatography remove impurity: the volume fraction adding its quality 5 times in Rhizoma Et Radix Notopterygii ethyl acetate extract be 5% methanol solution dissolve, then be separated through resin column, and with aqueous solution, volume fraction be successively 90% methanol solution carry out gradient elution by the column volume of 5 times, collect 90% methanol-eluted fractions thing; This 90% methanol-eluted fractions thing vacuum be 0.09MPa, namely temperature obtain Rhizoma Et Radix Notopterygii extractum coarse powder 648.3g through drying under reduced pressure under being the condition of 50 DEG C.
Wherein: resin column is HP20SS type resin column.Rhizoma Et Radix Notopterygii ethyl acetate extract and resin ratio are 1g:30mL.
Silica gel column chromatography be separated: add in Rhizoma Et Radix Notopterygii extractum coarse powder its quality 2 times of volume fractions be 100% methanol solution dissolve, after silica gel column chromatography is separated, with the chloroform-methanol mixed solvent eluting of 10 times of column volumes, fraction is collected by every part of 1000mL, and detect through thin layer chromatography, wherein developing solvent be chloroform, the mixed solvent that mixes by the volume ratio (mL/mL) of 5:5 of methanol, developer is the concentrated sulphuric acid alcoholic solution of volumetric concentration 10%, and merging Rf value is the fraction of 0.1 ~ 0.8; Rf value be 0.1 ~ 0.8 fraction vacuum be 0.09MPa, temperature be the condition of 50 DEG C under through drying under reduced pressure, obtain the Rhizoma Et Radix Notopterygii extract powder 442.9g in yellow powder.
Wherein: chloroform-methanol mixed solvent refers to the solvent that chloroform and methanol mix by the volume ratio (mL/mL) of 8:2.
Silicagel column is of a size of 60mm × 100mm.
embodiment 3a large-scale preparation method for inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder, comprises the following steps:
Extract: after 20.0Kg Rhizoma Et Radix Notopterygii pulverizing medicinal materials to 80 order, add volume fraction be 95% alcoholic solution or methanol solution carry out alcohol extraction, obtain filtrate after filtration; This filtrate vacuum be 0.08MPa, temperature be the condition of 60 DEG C under through drying under reduced pressure to paste, obtain Notopterol extract 3829.6g.
Wherein: alcohol extraction condition refers to that solid-liquid ratio is 1kg:15L, temperature is 80 DEG C, extraction time is 2 times, extraction time is 2h at every turn.
(2) liquid liquid distributes enrichment: the analytical pure aqueous dispersion of its quality 40 times of Notopterol extract, obtains dispersion liquid; This dispersion liquid extraction into ethyl acetate 3 times of its 40 times of volumes, merges and obtains acetic acid ethyl acetate extract; Acetic acid ethyl acetate extract vacuum be 0.08MPa, temperature obtains Rhizoma Et Radix Notopterygii ethyl acetate extract 1464.8g through drying under reduced pressure under being the condition of 60 DEG C.
(3) resin column chromatography remove impurity: the volume fraction adding its quality 3 times in Rhizoma Et Radix Notopterygii ethyl acetate extract be 15% methanol solution dissolve, then be separated through resin column, and with aqueous solution, volume fraction be successively 90% methanol solution carry out gradient elution by the column volume of 3 times, collect 90% methanol-eluted fractions thing; This 90% methanol-eluted fractions thing vacuum be 0.08MPa, namely temperature obtain Rhizoma Et Radix Notopterygii extractum coarse powder 1287.6g through drying under reduced pressure under being the condition of 60 DEG C.
Wherein: resin column is MCI type resin column.Rhizoma Et Radix Notopterygii ethyl acetate extract and resin ratio are 1g:30mL.
Silica gel column chromatography be separated: add in Rhizoma Et Radix Notopterygii extractum coarse powder its quality 3 times of volume fractions be 90% methanol solution dissolve, after silica gel column chromatography is separated, with the chloroform-methanol mixed solvent eluting of 8 times of column volumes, fraction is collected by every part of 800mL, and detect through thin layer chromatography, wherein developing solvent be chloroform, the mixed solvent that mixes by the volume ratio (mL/mL) of 5:5 of methanol, developer is the concentrated sulphuric acid alcoholic solution of volumetric concentration 10%, and merging Rf value is the fraction of 0.1 ~ 0.8; Rf value be 0.1 ~ 0.8 fraction vacuum be 0.08MPa, temperature be the condition of 60 DEG C under through drying under reduced pressure, obtain the Rhizoma Et Radix Notopterygii extract powder 869.3g in yellow powder.
Wherein: chloroform-methanol mixed solvent refers to the solvent that chloroform and methanol mix by the volume ratio (mL/mL) of 5:5.
Silicagel column is of a size of 50mm × 80mm.
Above-mentioned
embodiment 1 ~ 3obtained Rhizoma Et Radix Notopterygii extract powder refers to preparing the application in drugs against colon cancer or health food: this Rhizoma Et Radix Notopterygii extract powder makes all kinds of inhibitor against colon carcinoma cells pharmaceutical formulation with pharmaceutically acceptable any carrier according to a conventional method as active component, or makes all kinds of health-related food with acceptable any carrier in Food Science according to a conventional method as active component.
Claims (7)
1. a large-scale preparation method for inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder, comprises the following steps:
Extract: after the order of Rhizoma Et Radix Notopterygii pulverizing medicinal materials to 60 ~ 120, add volume fraction be 95% alcoholic solution or methanol solution carry out alcohol extraction, obtain filtrate after filtration; This filtrate to paste, obtains Notopterol extract through drying under reduced pressure;
(2) liquid liquid distributes enrichment: the analytical pure aqueous dispersion of its quality 30 ~ 50 times of described Notopterol extract, obtains dispersion liquid; This dispersion liquid extraction into ethyl acetate 3 times of its 30 ~ 50 times of volumes, merges and obtains acetic acid ethyl acetate extract; Described acetic acid ethyl acetate extract obtains Rhizoma Et Radix Notopterygii ethyl acetate extract through drying under reduced pressure;
(3) resin column chromatography remove impurity: the volume fraction adding its quality 2 ~ 5 times in described Rhizoma Et Radix Notopterygii ethyl acetate extract be 5 ~ 20% methanol solution dissolve, then be separated through resin column, and with aqueous solution, volume fraction be successively 90% methanol solution carry out gradient elution by the column volume of 2 ~ 5 times, collect 90% methanol-eluted fractions thing; Namely this 90% methanol-eluted fractions thing obtains Rhizoma Et Radix Notopterygii extractum coarse powder through drying under reduced pressure;
Silica gel column chromatography be separated: add in described Rhizoma Et Radix Notopterygii extractum coarse powder its quality 2 ~ 5 times of volume fractions be 80 ~ 100% methanol solution dissolve, after silica gel column chromatography is separated, with the chloroform-methanol mixed solvent eluting of 5 ~ 10 times of column volumes, fraction is collected by every part of 500 ~ 1000mL, and detect through thin layer chromatography, wherein developing solvent be chloroform, the mixed solvent that mixes by the volume ratio of 5:5 of methanol, developer is the concentrated sulphuric acid alcoholic solution of volumetric concentration 10%, and merging Rf value is the fraction of 0.1 ~ 0.8; Described Rf value be the fraction of 0.1 ~ 0.8 through drying under reduced pressure, obtain the Rhizoma Et Radix Notopterygii extract powder in yellow powder.
2. the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1, is characterized in that: described step (1) middle alcohol extraction condition refers to that solid-liquid ratio is 1kg:10 ~ 20L, temperature is 60 DEG C ~ 95 DEG C, extraction time is 1 ~ 3 time, extraction time is 1 ~ 3h at every turn.
3. the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1; it is characterized in that: described step (1), described step (2), described step (3) and described step (4) in drying under reduced pressure condition all refer to that vacuum is 0.06 ~ 0.09MPa, temperature is 50 ~ 65 DEG C.
4. the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1, is characterized in that: described step (3) middle resin column is the one in HP20 type resin column, HP20SS type resin column or MCI type resin column.
5. the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1, is characterized in that: described step (4) middle chloroform-methanol mixed solvent refers to the solvent that chloroform and methanol mix by the volume ratio of 8:2 ~ 2:8.
6. the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1, is characterized in that: described step (4) middle silicagel column is of a size of 30mm ~ 60mm × 60mm ~ 100mm.
7. the Rhizoma Et Radix Notopterygii extract powder that the large-scale preparation method of a kind of inhibitor against colon carcinoma cells Rhizoma Et Radix Notopterygii extract powder as claimed in claim 1 obtains is preparing the application in drugs against colon cancer or health food; it is characterized in that: this Rhizoma Et Radix Notopterygii extract powder makes all kinds of inhibitor against colon carcinoma cells pharmaceutical formulation with pharmaceutically acceptable any carrier according to a conventional method as active component, or make all kinds of health-related food with acceptable any carrier in Food Science according to a conventional method as active component.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912614A (en) * | 2019-02-25 | 2019-06-21 | 中国人民解放军北部战区总医院 | Rhizoma Et Radix Notopterygii alcohol extract, Notopterol, Rhizoma Et Radix Notopterygii phenol and application thereof |
Citations (2)
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|---|---|---|---|---|
| US20110177178A1 (en) * | 2007-11-14 | 2011-07-21 | Uxmal S.A., Chile | Extracts of Deschampsia antarctica Desv. with antineoplastic activity |
| CN103012424A (en) * | 2012-12-27 | 2013-04-03 | 成都普思生物科技有限公司 | Separation and purification method of notopterol monomer |
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2015
- 2015-09-15 CN CN201510586059.8A patent/CN105106259A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110177178A1 (en) * | 2007-11-14 | 2011-07-21 | Uxmal S.A., Chile | Extracts of Deschampsia antarctica Desv. with antineoplastic activity |
| CN103012424A (en) * | 2012-12-27 | 2013-04-03 | 成都普思生物科技有限公司 | Separation and purification method of notopterol monomer |
Non-Patent Citations (1)
| Title |
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| 张雪霞: "羌活的抗肿瘤活性成分研究", 《河北医科大学硕士学位论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912614A (en) * | 2019-02-25 | 2019-06-21 | 中国人民解放军北部战区总医院 | Rhizoma Et Radix Notopterygii alcohol extract, Notopterol, Rhizoma Et Radix Notopterygii phenol and application thereof |
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