CN102125590B - Ginsenoside Rg1-containing pseudo-ginseng active ingredient as well as preparation method and application thereof - Google Patents
Ginsenoside Rg1-containing pseudo-ginseng active ingredient as well as preparation method and application thereof Download PDFInfo
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- YURJSTAIMNSZAE-HHNZYBFYSA-N ginsenoside Rg1 Chemical compound O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YURJSTAIMNSZAE-HHNZYBFYSA-N 0.000 title claims abstract description 10
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- CBEHEBUBNAGGKC-UHFFFAOYSA-N ginsenoside Rg1 Natural products CC(=CCCC(C)(OC1OC(CO)C(O)C(O)C1O)C2CCC3(C)C2C(O)CC4C5(C)CCC(O)C(C)(C)C5CC(OC6OC(CO)C(O)C(O)C6O)C34C)C CBEHEBUBNAGGKC-UHFFFAOYSA-N 0.000 title claims abstract description 7
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Landscapes
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a ginsenoside Rg1-containing pseudo-ginseng active ingredient. The active ingredient mainly comprises a plurality of compounds such as ginsenoside Rg1, Yesanchinoside H and the like. The active ingredient is prepared by the following steps of: heating, extracting and concentrating medicinal materials; separating the medicinal materials through a reversed-phase silica gel column; eluting; concentrating and drying eluent; continuously separating by using a preparative liquid phase chromatography; collecting a solution; and concentrating and drying the solution to obtain the active ingredient. The pseudo-ginseng active ingredient can be applied to preparing medicaments for treating and preventing cardiovascular diseases. In the invention, the method is rationally designed, the active ingredient can be quickly and accurately obtained, and the quality of the medicament can be easily controlled during production.
Description
Technical field
The invention belongs to the field of Chinese medicines, relate to Radix Notoginseng active component of a kind of ginsenoside Rg1 of containing and preparation method thereof, this active component is pressed in the reversed-phase column and is separated through extracting, and preparation liquid phase separation and obtaining can be used for preparing the medicine of treating cardiovascular disease.
Background technology
Cardiovascular disease is the first healthy killer of harm humans; In recent years; Along with the variation of China's population senescence and people's work, life, dietary structure and environment etc., the incidence rate of cardiovascular and cerebrovascular diseases such as coronary heart disease also increases year by year, and the people's physical and mental health in serious threat.Many active substances have resisting myocardial ischemia, anoxia functions in the natural product, and some of them have been developed to treatment coronary heart disease and anginal new drug.Thereby from natural product, seek active substance with resisting myocardial ischemia, anoxia physiologically active, be one of effective way of discovery, developing new drug.China's medicinal organism resource is very abundant, and its biological active substances is research and finds new drug guide chemicals, the natural treasure-house of developing new drug.At present; China extracts active substance from natural product; Be used to be developed to treatment coronary heart disease, safety is good, toxicity is low new drug also seldom, from natural product, extract active substance, be developed to and have resisting myocardial ischemia; Be used to treat coronary heart disease and anginal new drug, have significant application value and wide development prospect.
Radix Notoginseng is the dry root of panax araliaceae plant Panax notoginseng (Burk.) F. H. Chen.The traditional Chinese medical science is thought, its sweet in the mouth, little hardship are warm in nature, return liver, stomach warp.Have the dissipating blood stasis hemostasis, the effect of subduing swelling and relieving pain is applicable to the treatment spitting of blood, spits blood, and epistaxis is had blood in stool, metrorrhagia, and traumatic hemorrhage, the breast abdomen twinges, tumbling and swelling etc.Modern study shows; Mainly contain ginsenoside (Ginsenosides) Rb1, Rd, Re, Rg1, Rg2, Rh in the Radix Notoginseng; 20-O-glucose Ginsenoside Rf; Arasaponin (Notoginsenoside) R1, R2, R3, R4, Herba Gynostemmatis Saponin (Gypeno-side) X VII still contains the panaxosideRb2.Also contain volatile oil;
arranged and
-guaiene (
-;
-guaiene); Have in addition
-copaene (
-copaene),
-guaiene, chamigrene (cuparene),
-;
-; γ-elemene (
-;
-;
-elemene),
-Cananga odorata oil alkene (
-muurolene),
-gurjunene (
-gurjunene), methyl palmitate, ethyl palmitate, heptadecadienoic acid methyl ester, octadecadienoic ethyl ester, phthalic acid di tert butyl carbonate (benzene-diformic acid ditert-butylate), octadecadienoic acid, isopropylbenzene, ring 12 carbon ketone (cy-clodode-canone), 1-methyl-4-peroxide methyl mercapto [2; 2,2] octane, the tetradecane, hexadecane, heptadecane, octadecane, nonadecane, larane, 21 alkane, docosane.The dencichine (N-oxalo-L-
,
-diaminopro-pionic acid) that contains a kind of tool styptic activity in the aqueous extract.Other contains Quercetin; Radix Notoginseng flavone B;
-sitosterol;
-sitosterol-D-glycoside; Sucrose.
Summary of the invention
The object of the present invention is to provide a kind of Radix Notoginseng active component that mainly contains the ginsenoside Rg1, obtain: pseudo-ginseng is pulverized the back add ethyl acetate and ethanol, heating extraction through following method for preparing; Medicinal residues add ethanol water and extract, and extracting solution is condensed into extractum, with the reverse phase silica gel post it are separated; At first use low concentration methanol as mobile phase, get eluent I, abandon it; Use high concentration methanol then instead as mobile phase, get eluent II, with getting sample behind the eluent II concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography; The separation condition of preparative hplc: chromatographic column is a preparative column, and mobile phase is water and acetonitrile, gradient elution, and Radix Notoginseng active component of the present invention mainly contains the ginsenoside Rg
1, several kinds of chemical compounds such as Yesanchinoside H.
Specifically prepare through following method: get pseudo-ginseng, it is pulverized back adding volume ratio is ethyl acetate and the ethanol of 1:1, reflux 1 hour; Extract 2 times, filtrating merge extracting solution I, medicinal residues add 70% alcoholic solution; Reflux 1 hour is extracted 2 times, filtrating merge extracting solution II; II is condensed into extractum with extracting solution, with 50% dissolve with methanol solution extractum, adopts ODS-C
18Post separates it, at first uses 5% methanol solution as mobile phase, gets eluent I, uses 60% methanol solution then instead as mobile phase, gets eluent II, gets sample behind the concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography: the separation condition of preparative hplc: chromatographic column is Agilent preparative column (Zorbax SB-C
18; 21.2mm
250mm), mobile phase is water A and acetonitrile B, and the gradient elution program is following: during 0min, mobile phase A is 90% water, and Mobile phase B is 10% acetonitrile solution; During 15min, mobile phase A is 72% water, and Mobile phase B is 28% acetonitrile solution; During 20min, mobile phase A is 72% water, and Mobile phase B is 28% acetonitrile solution; Flow velocity is 10ml/min, and column temperature is a room temperature; Sample separates through preparative liquid chromatography, collects solution in 13.4 ~ 17.8min time period, and solution obtains active component behind concentrate drying.
Another object of the present invention is to provide the application of this Radix Notoginseng active component in preparation treatment and angiocardiopathy preventing medicine.Prove that through pharmacological evaluation Radix Notoginseng active component provided by the invention has protective effect to myocardial cell.
Radix Notoginseng active component provided by the invention adds the adjuvant of accepting on the pharmaceutics as active component, processes preparation according to the method for preparing of the preparation of putting down in writing on the pharmaceutics.
The dosage form of medicine is a liquid preparation fire solid preparation, comprises injection, drip liquid, injectable powder, granule, tablet, electuary, powder, oral liquid, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, sucks agent, granule, pill, unguentum, sublimed preparation, spray, drop pill, disintegrating agent, oral cavity disintegration tablet, micropill etc.
Radix Notoginseng active component provided by the invention can be in the application in preparation treatment, the angiocardiopathy preventing medicine.Method for preparing provided by the invention is reasonable in design, can obtain effective ingredient rapidly and accurately, is easier to the quality control of medicine aborning.
The specific embodiment
To combine embodiment further explain flesh and blood of the present invention and beneficial effect below, this embodiment only is used to the present invention is described but not limitation of the present invention.
The preparation of embodiment one Radix Notoginseng active component
Pseudo-ginseng is pulverized the back add ethyl acetate and ethanol, heating extraction, medicinal residues add ethanol water and extract; Extracting solution is condensed into extractum, it is separated, at first use low concentration methanol as mobile phase with the reverse phase silica gel post; Get eluent I, abandon it, use high concentration methanol then instead as mobile phase; Get eluent II, with getting sample behind the eluent II concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography; The separation condition of preparative hplc: chromatographic column is a preparative column, and mobile phase is water and acetonitrile, gradient elution.
The preparation of embodiment two Radix Notoginseng active components
Get pseudo-ginseng, it is pulverized the back, and to add volume ratio be ethyl acetate and the ethanol of 1:1, and reflux 1 hour is extracted 2 times, filtrate merge extracting solution I.Medicinal residues add 70% alcoholic solution, and reflux 1 hour is extracted 2 times, filtrating merge extracting solution II, II is condensed into extractum with extracting solution, with 50% dissolve with methanol solution extractum, the employing ODS-C
18Post separates it, at first uses 5% methanol solution as mobile phase, gets eluent I, uses 60% methanol solution then instead as mobile phase, gets eluent II, gets sample behind the concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography: the separation condition of preparative hplc: chromatographic column is Agilent preparative column (Zorbax SB-C
18; 21.2mm
250mm), mobile phase is water A and acetonitrile B, and the gradient elution program is following: during 0min, mobile phase A is 90% water, and Mobile phase B is 10% acetonitrile solution; During 15min, mobile phase A is 72% water, and Mobile phase B is 28% acetonitrile solution; During 20min, mobile phase A is 72% water, and Mobile phase B is 28% acetonitrile solution; Flow velocity is 10ml/min, and column temperature is a room temperature; Sample separates through preparative liquid chromatography, collects solution in 13.4 ~ 17.8min time period, and solution obtains active component behind concentrate drying.
The preparation of embodiment three dropping pill formulations
Get Radix Notoginseng active component 0.5g and 10.5g Polyethylene Glycol-20000 mix homogeneously, heating and melting moves in the drop pill drip irrigation behind the change material, and in ℃ liquid paraffin of medicine liquid droplet to 6 ~ 8, oil removing makes 400 of drop pill.
The preparation of embodiment four lyophilized injectable powders
Get Radix Notoginseng active component 0.5g, glucose 4.5g, sodium thiosulfate 0.9g and distilled water 1000ml, behind the said components mix homogeneously, 400 of packing, lyophilization promptly gets.
The active appraisal experiment of embodiment five Radix Notoginseng components
1. the Radix Notoginseng component is to H
2O
2The protective effect of injury of myocardium cell
In vitro culture H
9C
2Myocardial cell, culture fluid are that DMEM (high sugar)+10%FBS (G)+1% non essential amino acid+0.1% pair is anti-.The trophophase cell of taking the logarithm places on the 96 porocyte culture plates, behind constant temperature culture 24 h, adds 200 μ mol/mL H
2O
2Injury of myocardium cell 30 min, the Radix Notoginseng component that adds final concentration again and be 50 μ g/mL is hatched 24 h, adopts mtt assay to measure cell viability.The result shows that this component is to H
2O
2The protective rate of injury of myocardium cell is 11.29%.
2. the Radix Notoginseng component is to the protective effect of hypoxia-reoxygenation induced injured myocardium cell
In vitro culture H
9C
2Myocardial cell, culture fluid are that DMEM (high sugar)+10%FBS (G)+1% non essential amino acid+0.1% pair is anti-.The trophophase cell of taking the logarithm places on the 96 porocyte culture plates, behind constant temperature culture 24 h, in the anoxia cell, cultivates 6 h.After anoxia finished, taking out the Tissue Culture Plate adding was the Radix Notoginseng component of 50 μ g/mL through the final concentration of sugar-free Hank ' s dilution, under the normal cultured condition, hatches 6h hour, gets cell culture supernatant and measures lactic acid dehydrogenase (LDH) content.The result shows that this component is 13.04% to the myocardial cell protection rate of anoxia reoxygenation injury.
Claims (4)
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| CN101665527A (en) * | 2008-09-02 | 2010-03-10 | 河北以岭医药研究院有限公司 | Ginsenoside, preparation method thereof and use thereof |
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Non-Patent Citations (1)
| Title |
|---|
| 寻晓红.人参皂甙的研究进展.《中国现代医学杂志》.2003,第13卷(第15期),43-44. * |
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