CN1699397A - Process for preparing notoginseng triol saponin and use thereof - Google Patents
Process for preparing notoginseng triol saponin and use thereof Download PDFInfo
- Publication number
- CN1699397A CN1699397A CN 200510075040 CN200510075040A CN1699397A CN 1699397 A CN1699397 A CN 1699397A CN 200510075040 CN200510075040 CN 200510075040 CN 200510075040 A CN200510075040 A CN 200510075040A CN 1699397 A CN1699397 A CN 1699397A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- protoparaxotriol saporlirs
- preparation
- kilogram
- notoginseng
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 229930182490 saponin Natural products 0.000 title claims abstract description 27
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 22
- 241000180649 Panax notoginseng Species 0.000 title claims abstract description 20
- 235000003143 Panax notoginseng Nutrition 0.000 title claims abstract description 19
- -1 triol saponin Chemical class 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 168
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 30
- 244000131316 Panax pseudoginseng Species 0.000 claims description 25
- 235000003181 Panax pseudoginseng Nutrition 0.000 claims description 25
- 238000002360 preparation method Methods 0.000 claims description 20
- 235000017709 saponins Nutrition 0.000 claims description 19
- 239000000796 flavoring agent Substances 0.000 claims description 18
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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 claims description 18
- 150000007949 saponins Chemical class 0.000 claims description 14
- YURJSTAIMNSZAE-UHFFFAOYSA-N UNPD89172 Natural products C1CC(C2(CC(C3C(C)(C)C(O)CCC3(C)C2CC2O)OC3C(C(O)C(O)C(CO)O3)O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O YURJSTAIMNSZAE-UHFFFAOYSA-N 0.000 claims description 13
- 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 claims description 13
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Landscapes
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Abstract
The invention discloses a process for preparing notoginseng triol saponin and use thereof, which includes following steps: crushing the notoginseng, and adding ethanol solution whose concentration is 50 to 90% to immerse and percoalte the notoginseng, and then collecting the percoalted liquid and reducing pressure to concentrate the same, and then using distilled water to dilute the concentrated liquid, and then slowly filling the liquid into the large-hole absorption resin separating column, and using 40% ethanol to elute, and then collecting the 40% ethanol elutriant and refining the same to obtain notoginseng triol saponin. The notoginseng triol saponin extracted by the provided process contains all triol saponin in the notoginseng, wherein contains 156 to 79 % ginsenosiderx Rg, 5.0 to 7.5 % of ginsenosiderx Re, 11 to 14 % triol saponin R1, 78 to 98 % of notoginseng triol saponin. The notoginseng triol saponin can be used in treatment for cardiocerebrovascular embolic disease, and has advantages including high content, stable quality, good colour, low cost, and its organic solvent residual amount complies with drug standard.
Description
Invention field
The invention relates to a kind of extracting method and application thereof of medicinal plant, more particularly about a kind of preparation method and application thereof of from pseudo-ginseng, extracting protoparaxotriol saporlirs.
Background technology
Pseudo-ginseng is a Chinese medicine commonly used in the traditional Chinese medicine, and Chinese Pharmacopoeia is put down in writing its function and is the stasis of blood, hemostasis, detumescence, the analgesia of loosing.
Protoparaxotriol saporlirs is that the single medicinal material pseudo-ginseng (has another name called pseudo-ginseng, Panax pseudoginseng) saponin extract is a pseudo-ginseng blood-circulation-invigovating stagnation resolvation efficient part, contains triol saponins whole in the pseudo-ginseng, major ingredient is ginsenoside Rg1, Re, reaches arasaponin R1, and a spot of Rb1, Rd etc. are arranged.
Pseudo-ginseng another name pseudo-ginseng, Panax pseudoginseng for Araliaceae Panax Panaxnotoginseng (Burk) F.H.Chen rhizome, originate in Yunnan, Guangxi.Pseudo-ginseng is one of conventional Chinese medicine, and the main component of its biological activity and pharmacological action is a saponins.The pharmacological results shows that Radix Notoginseng total arasaponins can increase blood flow volume, vasodilation, reduction arteriotony and myocardial consumption of oxygen, improves the human body function and reaches the anoxybiotic tolerance, and effects such as the platelet aggregation of supression, reduction blood viscosity are arranged.
The Treatment of Blood Stasis Syndrome, the traditional Chinese medical science have the therapy and the experience of many preciousnesses, and pseudo-ginseng is one of them important drugs.Aspect cardiovascular and cerebrovascular diseases (as atherosclerosis and thrombotic diseases), the status of antiplatelet class medicine causes attracting attention of people day by day, wherein representative is the inhibitors of cyclooxygenases acetylsalicylic acid, it stops synthesizing of the interior TX of thrombocyte, also influence simultaneously PG, but, be the weakness of its band essence also just because of this irreversible inhibition to enzyme causes hemorrhage risk.People wait in expectation and a kind of TX are had more the platelet aggregation inhibitor of specificity, also are the focuses in current this class medicine research.Protoparaxotriol saporlirs only influences the activity of TX and does not influence the activity of PG, has shown its effect characteristics.The foreign scholar found in recent years that the ginsenoside Rg1 had antiplatelet effects, and 50 milligrams of normal humans are effective.Scholar's inference that its mechanism of action has is to act on platelet membrane TXA
2Acceptor and TXA
2The joint portion and position afterwards.The scholar who has thinks to act on inhibition suprarenin and second increase of intracellular calcium mutually that zymoplasm causes, is different from acetylsalicylic acid.
Since nearly more than ten years, cardiovascular and cerebrovascular diseases has become the important diseases of serious harm people's health, and sickness rate is trend of rising year by year.In order better to develop the traditional Chinese medicine resource of China, improve the inner quality and the market competitiveness of Chinese medicine preparation, herbal species sure to curative effect, that security is good is developed, and will have important practical significance.
The inventor after years of research and found that, many compositions in the Radix Notoginseng total arasaponins to platelet aggregation-against, prevent that thrombosis from being invalid, real effective is protoparaxotriol saporlirs etc., the preparation method of relevant protoparaxotriol saporlirs, specification of quality, character, the relevant pharmacological action that this patent the is related and effect of human body be there is no report.
Summary of the invention
One of purpose of the present invention is to overcome the defective that prior art exists, and a kind of production method of extracting protoparaxotriol saporlirs from pseudo-ginseng is provided.
Second purpose of the present invention provides the preparation method of the protoparaxotriol saporlirs of a kind of energy prevention and treatment cardiovascular and cerebrovascular embolism class diseases.
The 3rd purpose of the present invention provides a kind of application of protoparaxotriol saporlirs.
These and other objects of the present invention will further embody and illustrate by following detailed.
The preparation method of protoparaxotriol saporlirs of the present invention comprises the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be alcohol immersion 12-30 hour of 50-90%, evenly the diacolation bucket is inserted in compacting then;
B, 60% ethanol percolation to the effluent liquid of doubly measuring with medicinal material amount 6-12 do not have the saponin(e reaction, and flow velocity is every kilogram of medicinal material of 3-7 ml/min;
C, be 0.04-0.1Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, will be concentrated into the percolate that does not have behind the alcohol flavor and add water to 3-6 and doubly measure, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal material of 3-7 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
Further, the preparation method of protoparaxotriol saporlirs of the present invention comprises the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be alcohol immersion 20-28 hour of 60-90%, evenly the diacolation bucket is inserted in compacting then;
B, 60% ethanol percolation to the effluent liquid of doubly measuring with medicinal material amount 8-10 do not have the saponin(e reaction, and flow velocity is every kilogram of medicinal material of 4-6 ml/min;
C, be 0.05-0.06Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, will be concentrated into the percolate that does not have behind the alcohol flavor and add water to 5-6 and doubly measure, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal material of 4-6 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
Be preferably, the preparation method of protoparaxotriol saporlirs of the present invention comprises the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be 60% alcohol immersion 24 hours, evenly the diacolation bucket is inserted in compacting then;
B, do not have the saponin(e reaction with 60% ethanol percolation to the effluent liquid of 10 times of amounts of medicinal material amount, flow velocity is every kilogram of medicinal materials of 5 ml/min;
C, be 0.06Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, the percolate that will be concentrated into after nothing alcohol is distinguished the flavor of add water to 5 times of amounts, and be centrifugal, gets the clear liquid upper prop, and rate of addition is every kilogram of medicinal materials of 5 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
In the preparation method of protoparaxotriol saporlirs of the present invention, soak solution flows to end neat liquid level earlier during diacolation, and the back drips 60% ethanol, and flow velocity is suitable up and down in control, can not do post; After washing with 8-10 times of water gaging in the column chromatography step, doubly measure 40% ethanol with 8-10 again and wash, control drips with take-off rate and suits mutually, dried post can not occur equally; Protoparaxotriol saporlirs is collected since first colour band, differentiates control collection protoparaxotriol saporlirs part with TLC, waits not develop the color to be and finishes.
In the present invention, used macroporous adsorbent resin separator column was soaked 12 hours with 1% hydrochloric acid or sulfuric acid ethanol liquid, it is extremely neutral with distilled water flushing to continue, and can reuse; The post footpath of macroporous adsorbent resin with the ratio of post height is: 30: 160, described macroporous adsorbent resin was the styrene type interpolymer, and model is D-101.
All the notoginseng triol saponins in the pseudo-ginseng have been comprised with the protoparaxotriol saporlirs extract that preparation method of the present invention extracted, wherein ginsenoside Rg1, Re and arasaponin R1 content are followed successively by 58-74%, 5.5-8.0%, 11.0-14.0, total amount is 78-89%, the Determination of Residual Organic Solvents of product reaches the pharmaceutical grade standard, benzene is less than 2ppm, and toluene, diethylbenzene are respectively less than 20ppm.Prepared protoparaxotriol saporlirs can be used for treating the cardiovascular and cerebrovascular embolism class diseases.
With protoparaxotriol saporlirs content height, steady quality that method of the present invention is extracted, color and luster is good, will can satisfy the requirement of modernized Chinese medicine fully with its Chinese medicine preparation that is raw material is made, and cost is low, the protoparaxotriol saporlirs loss is few; Compare with traditional solvent extration, do not use toxicity and volatile organic solvent in the technical process, safe and reliable, simplified production technique greatly.
The protoparaxotriol saporlirs that extracts with method of the present invention has significant protective effect to experimental cerebral ischemia, cerebral infarction animal, and can obviously improve its function and behavior disorder.Reduce cerebral vascular resistance, increase dog ICAF amount.Both can suppress ADP, AA, collagen-induced rat platelet aggregation, and can suppress the human body platelet of ADP, AA, PAF and thrombin induction again and assemble.Simultaneously can reduce rat whole blood viscosity and pcv, suppress thrombosis.And has an effect of microcirculation improvement.
The present invention adopts the elite-notoginseng triol saponins in the Radix Notoginseng total arasaponins, therefore the medicine of the more common employing Radix Notoginseng total arasaponins of curative effect is much higher, and the bioavailability height, carry and administration, easy administration and absorption fast, statistics according to the study, curative effect is more common to be that the Chinese medicine of main component is high more than 50% with the Radix Notoginseng total arasaponins.
Below in conjunction with embodiment in detail the present invention is described in detail, can not limits the scope of the invention but embodiment only is used for explanation.
In the present invention, if not refer in particular to, all part, per-cents are weight unit, and all equipment and starting material etc. all can be buied from market or the industry is commonly used.
Embodiment
Example 1: the chemical ingredients of protoparaxotriol saporlirs (PTS)
1., arasaponin C
1, D
1Separation
Thin layer silica gel (production of 10-40 μ Haiyang Chemical Plant, Qingdao) dry column-packing (¤ 42*400mm).PTS is dissolved in rare alcohol, admixes thin layer silica gel, and low temperature dries, and the capital of packing into mutually for launching solvent, divides the sample receptor to receive 20 milliliters every part under chloroform-methanol-water (65: 35: 10) automatically.Thin-layer chromatography is identified, upward launch on point sample, the horizontal development groove at efficient thin-layer silicon offset plate (Haiyang Chemical Plant, Qingdao's production), launch the developping agent system that solvent is same as column chromatography, dry after the expansion, ethanol solution of sulfuric acid spraying, 105 ℃ were toasted 5 minutes, or the baking of electric heating blower hot blast, got the identical stream part of chromatogram spot and merged, the Rf value is consistent with the reference substance ginsenoside Rg1, and steaming desolventizes.
2., ginsenoside Rg1's evaluation
Through ethanol-butanone recrystallization, drying, the sample that obtains after tested fusing point, ultimate analysis, through external spectrum
13The c nuclear magnetic resonance spectroscopy and TLC and HPLC stratographic analysis, this compound is consistent with standard substance, and is consistent with literature value, definite from protoparaxotriol saporlirs isolating monomeric compound be the ginsenoside Rg1.
(a) fusing point 190-192 ℃
191-192.5℃
(b) ultimate analysis:
The analyzer room, the court adopts the CH automatic analyser to measure
Molecular formula C
42H
72O
14.2H
2O
Theoretical value (%): C60.22 H9.15
Experimental value (%): C60.27 H9.28
Consistent with ginsenoside Rg1's molecular formula, C, H test result.
(c) infrared spectroscopy spectrum
Infrared spectrometer (IR171D FTIR)
The infrared spectrogram of sample and reference substance ginsenoside Rg
1Unanimity.
Max
IRVKBr?cm
-1，3400(-OH)，1630(c＝c)
(d)
13The C nuclear magnetic resonance spectrum
Beijing Bruker AM-500 of medicine institute instrument test
Sample and reference substance ginsenoside Rg
1 13The CNMR collection of illustrative plates is identical.
The chemical displacement value of saponin(e aglycon and sugar.Both unanimities.
Table 5-7 ginsenoside Rg
1And arasaponin C
1 13The CNMR chemical displacement value
E, chromatogram are identified
Need testing solution: arasaponin C
1(separating obtained) methanol solution 2 mg/ml, PTS methanol solution 2 mg/ml.
Reference substance solution: the ginsenoside Rg1, Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, methanol solution 2 mg/ml.
The TLS method: get trial-product and reference substance solution and go up point sample 7 μ l at high-efficient silica gel plate (Haiyang Chemical Plant, Qingdao's production), launch on the horizontal development instrument, exhibition is apart from 8-9 centimetre, and taking-up is dried, the spraying of 10% vitriol oil ethanolic soln, and 105 ℃ were toasted arasaponin C 5 minutes
1Identical with ginsenoside Rg1's Rf value.The Rf value that contains main component among the PTS is identical with the ginsenoside Rg1.
The HPLC method
Arasaponin C
1, ginsenoside Rg1's reference substance is tested on the LC-6AHPLC instrument of Tianjin, island
Post: WATERS Carbhydrate ¤ 3.9*300 millimeter
Post is pressed: 98 kilograms per centimeter
2
Chart speed: 3 mm/min
Moving phase: acetonitrile-water (85: 15)
The result shows arasaponin C
1Be a simplification compound, its retention time is identical with the ginsenoside Rg1.
Above data and PLC, the qualitative evaluation of HPLC separate the arasaponin C that obtains from Radix Notoginseng
1Be the ginsenoside Rg
1
Chemical name: (3 β, 6 α, 12 β)-3,12-dihydroxydamanar-24-ene-6,20-d:ylbis-β-D-Glucopyrannoside, i.e. (3 β, 6 α, 12 β)-3, rattle away agate alkane-24-alkene-6,20-of 12-dihydroxyl is two--β-D-glucopyranoside.
Structural formula is:
R
1＝R
2＝Glu
3. the chemical constitution of PTS
Producing trial-production production product content mean value is: Rg1:64.92%, Re:7.79%, R
1: 12.6%, summation is 85.31%.
The chemical constitution of PTS is measured Rg1, D with the TLCS method
1, Rb
1Spot, dual wavelength scanning.
Rg1 is that reference substance calculates, and sees Table 1
The chemical constitution (%) of table 1PTS
| Lot number | ??Rg 1 | ??D 1 | ??Rb 1 | Moisture | 732[H] adsorptive |
| ??040409 | ??65.2 | ??19.6 | ??6.2 | ??4.6 | ??3.7 |
| ??040414 | ??68.1 | ??20.8 | ??4.2 | ??6.0 | ??2.5 |
| On average | ??66.6 | ??20.2 | ??5.2 | ??5.4 | ??3.1 |
Qualitative showing: contain small amount of coloring matter among the PTS, sugar and some amino acid, PTS is water-soluble, through absorption with macroporous adsorbent resin, the water lotion that does not the contain saponin(e 732[H of q.s that flows through] resin column, effluent liquid does not become ninhydrin reaction, be concentrated into dried more seldom yellow substance, claim inaccurate weight, with ammoniacal liquor wash-out 732 resin columns, be concentrated into dried, wherein contain amino acid, be dried to constant weight, calculate per-cent with the PTS amount that drops into and see Table 2, this material contains Threonine through amino acidanalyser (WATERS-HPLC-AAA system) analysis, Serine, L-Ala, phenylalanine, Histidine, seven kinds of AA such as tryptophane.
Table 2PTS moisture content (official method mensuration)
| Lot number | ??040326 | ??040409 | ??040414 | ??040427 | On average |
| Moisture % | ??5.4 | ??4.6 | ??6.1 | ??6.6 | ??5.7 |
In a word: it is total and about 85% to measure the content composition among the PTS, notoginseng glycol saponin class (Rb
1, the Rd class) about 6%, 732[H] the resin absorption thing, about 2-3% such as amino acid, peptide, moisture 5-7%.
4. arasaponin D1 is accredited as the mixture of known composition ginsenoside Re and arasaponin R1 by analysis.
4, the physico-chemical property of PTS
Outward appearance: protoparaxotriol saporlirs is the yellowish brown powder, and nothing is smelt, mildly bitter flavor.
Solubleness: press Chinese Pharmacopoeia (version appendix 9 solubility test methods in 2000) test, the solubleness of PTS is water-soluble, Diluted Alcohol; Be slightly soluble in ethanol, methyl alcohol; The atomic acetone that is dissolved in.In ethyl acetate, almost insoluble in chloroform, the sherwood oil.
Fusing point: this product is a mixture, and the melting range fluctuation is bigger, between four batch sample m.p.180-184 ℃.
Lot number: 040326m.p.180-184 ℃
040409m.p.180.0-182.5℃
040414m.p.182.0-184.0℃
040427m.p.181.0-183.0℃
5, scale-up
Scale-up, the five batches every batch 4 kilograms of pseudo-ginseng that feed intake, the result is as follows:
Table 3 protoparaxotriol saporlirs scale-up data
| Lot number | Charging capacity (Kg) | Output (Kg) | Yield (%) | Content (%) | ||
| The ginsenoside Rg | Panax Notoginseng saponin R | The ginsenoside Re | ||||
| ??040307 | ??4.0 | ??201.0 | ??5.02 | ??62.51 | ??15.65 | ??7.86 |
| ??040313 | ??4.0 | ??192.0 | ??4.8 | ??63.27 | ??14.37 | ??8.42 |
| ??040316 | ??4.0 | ??201.0 | ??5.0 | ??68.27 | ??14.17 | ??8.31 |
| ??040303 | ??4.0 | ??197.5 | ??4.9 | ??64.16 | ??15.79 | ??7.83 |
| ??040310 | ??4.0 | ??206.0 | ??5.15 | ??60.95 | ??15.52 | ??7.70 |
Ten batches produce the trial product yield and the assay result as follows:
Table 4 protoparaxotriol saporlirs production trial-production yield contains scale
| Sequence number | Lot number | Charging capacity (Kg) | Dried cream (Kg) | Yield (%) | Content (%) | ||
| ??Rg 1 | ??Re | ??R 1 | |||||
| ??1 | ??930801 | ??15 | ??0.5 | ??3.33 | ??69.18 | ??8.18 | ??12.14 |
| ??2 | ??930802 | ??15 | ??0.5 | ??3.33 | ??72.81 | ??8.08 | ??13.86 |
| ??3 | ??930803 | ??15 | ??0.8 | ??5.33 | ??62.42 | ??7.90 | ??13.9 |
| ??4 | ??930804 | ??15 | ??0.62 | ??4.13 | ??62.56 | ??5.88 | ??12.60 |
| ??5 | ??930805 | ??15 | ??0.6 | ??4.0 | ??61.83 | ??7.10 | ??13.69 |
| ??6 | ??930806 | ??15 | ??0.8 | ??5.33 | ??63.27 | ??7.45 | ??13.06 |
| ??7 | ??930901 | ??15 | ??0.8 | ??5.33 | ??66.87 | ??7.61 | ??12.18 |
| ??8 | ??930902 | ??15 | ??0.8 | ??5.33 | ??60.0 | ??5.56 | ??13.17 |
| ??9 | ??930903 | ??36 | ??1.6 | ??4.44 | ??61.41 | ??7.58 | ??12.1 |
| ??10 | ??930904 | ??14 | ??0.8 | ??4.71 | ??61.79 | ??7.50 | ??11.2 |
| Mean value | Criticize in 1-10 | ??0.78 | ??4.53 | ??64.28 | ??7.68 | ??12.79 | |
| Criticize in 3-10 | ??0.853 | ??4.83 | ??62.60 | ??7.57 | ??12.59 | ||
Example 2: prepare protoparaxotriol saporlirs according to the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, added concentration and be 60% alcohol immersion 14 hours, even then, the diacolation bucket is inserted in compacting;
B, do not have the saponin(e reaction with 60% ethanol percolation to the effluent liquid of 6 times of amounts of medicinal material amount, flow velocity is every kilogram of medicinal materials of 3 ml/min, and soak solution flows to end neat liquid level earlier during diacolation, and the back drips 60% ethanol, and flow velocity is suitable up and down in control, can not do post;
C, be 0.04Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, the percolate that will be concentrated into after nothing alcohol is distinguished the flavor of add water to 3 times of amounts, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal materials of 3 ml/min, after washing with 9 times of water gagings, wash with 9 times of amount 40% ethanol again, control drips suitable mutually with take-off rate, dried post can not occur, and protoparaxotriol saporlirs is collected since first colour band, differentiate control collection protoparaxotriol saporlirs part with TLC, wait not develop the color to be and finish;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery;
F, used macroporous adsorbent resin separator column are with 1% salt sulfuric acid ethanol liquid soaked overnight, and it is extremely neutral with distilled water flushing to continue, and can reuse, and the post footpath of macroporous adsorbent resin with the ratio of post height is: 30: 160, be the styrene type interpolymer, and model is D-101.
Example 3: prepare protoparaxotriol saporlirs according to the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, added concentration and be 90% alcohol immersion 28 hours, even then, the diacolation bucket is inserted in compacting;
B, do not have the saponin(e reaction with 60% ethanol percolation to the effluent liquid of 12 times of amounts of medicinal material amount, flow velocity is every kilogram of medicinal materials of 7 ml/min, and soak solution flows to end neat liquid level earlier during diacolation, and the back drips 60% ethanol, and flow velocity is suitable up and down in control, can not do post;
C, be 0.08Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, the percolate that will be concentrated into after nothing alcohol is distinguished the flavor of add water to 6 times of amounts, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal materials of 7 ml/min, after washing with 8 times of water gagings, wash with 8 times of amount 40% ethanol again, control drips suitable mutually with take-off rate, dried post can not occur, and protoparaxotriol saporlirs is collected since first colour band, differentiate control collection protoparaxotriol saporlirs part with TLC, wait not develop the color to be and finish;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery;
F, used macroporous adsorbent resin separator column wash with 1% sulfuric acid ethanol liquid, until extremely neutral with distilled water flushing, can reuse, and the post footpath of macroporous adsorbent resin with the ratio of post height is: 30: 160, be the styrene type interpolymer, and model is D-101.
Example 4: prepare protoparaxotriol saporlirs according to the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, added concentration and be 75% ethanol submergence bubble 24 hours, evenly the diacolation bucket is inserted in compacting then;
B, do not have the saponin(e reaction with 60% ethanol percolation to the effluent liquid of 10 times of amounts of medicinal material amount, flow velocity is every kilogram of medicinal materials of 5 ml/min, and soak solution flows to end neat liquid level earlier during diacolation, and the back drips 60% ethanol, and flow velocity is suitable up and down in control, can not do post;
C, be 0.06Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, the percolate that will be concentrated into after nothing alcohol is distinguished the flavor of add water to 5 times of amounts, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal materials of 5 ml/min, after washing with 10 times of water gagings, wash with 10 times of amount 40% ethanol again, control drips suitable mutually with take-off rate, dried post can not occur, and protoparaxotriol saporlirs is collected since first colour band, differentiate control collection protoparaxotriol saporlirs part with TLC, wait not develop the color to be and finish;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery;
F, used macroporous adsorbent resin separator column wash with 1% sulfuric acid ethanol liquid, until extremely neutral with distilled water flushing, can reuse, and the post footpath of macroporous adsorbent resin with the ratio of post height is: 30: 160, be the styrene type interpolymer, and model is D-101.
Show that by the protoparaxotriol saporlirs pharmacodynamics test this product has significant protective effect to experimental cerebral ischemia, cerebral infarction animal, and can obviously improve its function and behavior disorder.Reduce cerebral vascular resistance, increase dog ICAF amount.Both can suppress AD, PAA, collagen-induced rat platelet aggregation, and can suppress the human body platelet of ADP, AA, PAF and thrombin induction again and assemble.Can reduce the rat whole blood viscosity simultaneously and, suppress thrombosis through cell pack.And has an effect of microcirculation improvement.
Example 5: protoparaxotriol saporlirs blocks the provide protection that causes cerebral infarction to the rat mesencephalic arteries
One, test objective
This test uses the disconnected intraluminal middle cerebral artery occlusion in rats of burning to cause the method for cerebral infarction, observes protoparaxotriol saporlirs (prevention administration group; Block back drug treatment group) disordered brain function that local cerebral ischemia is caused and the influence of infarction size.For this medicine treatment ischemic cerebrovascular disease of clinical application provides the pharmacology foundation.
Two, test materials:
Medicine: protoparaxotriol saporlirs: light brown powder, ginsenoside Rg
1Content 68.3%, lot number: 040316, provide by plant chamber, the court, be made into the solution use of finite concentration (50,25,12.5 mg/ml) before the experiment with distilled water.
Nimodipine: Tianjin central authorities pharmaceutical factory produces.Being made into certain density suspension with 0.5% mucialga of arabic gummy before the experiment, to do positive control medicinal.
Animal: rat: male Wistar, body weight 250～300 gram is provided by the court's Animal House, conformity certification number: accurate No. 001 of the real moving facility in Tianjin.
Three, method and result:
1. prevention administration experiment:
Be divided into 5 groups at random by animal body is heavy, 10 every group, gastric infusion.
(1) ischemic control group: gavage 4 milliliters/kilogram/days of distilled water, (2) positive drug control group: nimodipine: 50 milligrams/kilogram/days, (3) (4) (5) group gavages 200,100,50 milligrams/kilogram/days of protoparaxotriol saporlirss respectively, each organizes equal successive administration 7 days, in the last administration after 2 hours, 350 milligrams of/kilogram anesthesia of abdominal injection Chloral Hydrate are by blocking-up big white mouse mesencephalic arteries method
[1]Expose the right side arteria cerebri media, under operating microscope (Shanghai medical optical instrument factory), arteria cerebri media is burnt disconnected with electric knife, postoperative steams again and raises, and room temperature remains on 26～27 ℃, 24 hours laggard action thing behavior scorings the results are shown in Table 1, with this index as disordered brain function.Broken end is got brain then, confirms to put into cool brine after the blocking-up of animal brain medium sized artery under operating microscope, after 10 minutes, gets olfactory bulb, cerebellum and low brain stem.Be cut into 5 along coronal-plane, brain section placed contain 1.5 milliliter of 4% TCC and 0.1 milliliter of 1MK
2HPO
45 milliliters of staining fluids in, lucifuge, after 37 ℃ of temperature are incubated 30 minutes, take out and put into 10% formalin solution, keep in Dark Place, healthy tissues is rose, ischemic region is white in color, and white is organized carefully to dig down weigh, and calculates the per-cent that blocking tissue's weight accounts for hemicerebrum weight, with this ratio evaluate efficacy, the results are shown in Table 5.
Standards of grading
[2]As follows:
1. carry the mouse tail, about 1 chi of built on stilts is observed two forelimb active situation.Intact animal two forelimbs protract, symmetry, and operation back ischemic brain hemisphere offside forelimb inward turning and interior receipts, visual range degree difference was commented 0～4 fen;
2. with on the sliding ground of animal horizontalization, push away both shoulders respectively, check resistance to side shifting, normal rat bilateral resistance symmetry, the resistance descender according to decline degree difference, is chosen as 0～3 fen when the operation offside promotes
3. tractive two forelimbs are normal symmetrical, and myasthenia of limbs before the offside of operation back was commented 0～3 fen.
4. animal have do not stop to a side person of turn-taking, add 1 fen.
According to above standard scoring, full marks are 11 minutes.Mark is high more, and the behavior disorder of animal is serious more.
Table 5 prevention administration protoparaxotriol saporlirs is to the influence of behavior disorder due to the blocking-up intraluminal middle cerebral artery occlusion in rats
* * P＜0.001 (comparing with the ischemic control group) adopts the statistical study-t value method of two groups of means to carry out statistical treatment.
Adopt blind method to mark, result's ischemic control group behavior disorder as seen from Table 5 is the most serious, and protoparaxotriol saporlirs height, middle dosage group are obviously improved behavior disorder, and low dose group does not have obvious influence, and nimodipine also obviously reduces behavior scoring.
Table 6 prevention administration protoparaxotriol saporlirs is to the influence of blocking-up intraluminal middle cerebral artery occlusion in rats cerebral infarct size
* P＜0.05, * * P＜0.01 (with the ischemic control group relatively)
From table 6 result as seen, protoparaxotriol saporlirs and nimodipine prevention administration is plugged with obvious curative effects to the cerebral infarction that the blocking-up intraluminal middle cerebral artery occlusion in rats causes.Cerebral infarction organizes per-cent to reduce 54.2% (P＜0.01), 44.6% (P＜0.05), 25%, 33.3% (P＜0.05) respectively, and the result who improves with behavior is consistent.
2. treatment administration experiment
Get 50 of healthy white rats, 350 milliliters of/kilogram anesthesia of abdominal injection Chloral Hydrate, the same method is carried out intraluminal middle cerebral artery occlusion in rats blocking-up operation, and postoperative steams again raises, and in postoperative 4 hours rat is divided into 5 groups by the mild symptoms weight average, and 10 every group, gastric infusion.1. ischemic control group: gavage 4 milliliters of/kilogram days of distilled water, 2. positive drug control group: 50 milliliters/kilogram/days of nimodipines, 3., 4., 5. organize and gavage 200,100,50 milliliters/kilogram/days of protoparaxotriol saporlirss respectively, each organizes equal successive administration six days, and after grouping, every morning is carried out behavior scoring to animal, continuous six days, the results are shown in Table 7, in the 7th day the animal broken end is got brain, the same method is calculated the per-cent that blocking tissue's weight accounts for hemicerebrum weight, the results are shown in Table 8.
Table 7 protoparaxotriol saporlirs is to the influence of behavior disorder due to the blocking-up intraluminal middle cerebral artery occlusion in rats
| Group | Number of animals | Dosage (mg/k g/ day) | Behavior scoring | ||||||
| Before the administration | After the administration | ||||||||
| The 1st day | The 2nd day | The 3rd day | The 4th day | The 5th day | The 6th day | ||||
| The ischemic control group | ??10 | ??8.20± ????0.89 | ??7.90± ????0.91 | ??7.70± ????1.1 | ??7.60± ????1.1 | ??7.45± ????1.1 | ??7.20± ????1.24 ??(n＝9)+ | ??7.0± ????1.20 ??(n＝8)* | |
| ??PTS | ??10 | ??200 | ??8.20± ????0.73 | ??7.60± ????1.0 | ??6.96± ????1.3 | ??6.15± ????1.1 | ??6.0± ????1.0 | ??5.50± ????0.62 | ??5.20± ????0.98 |
| ??PTS | ??10 | ??100 | ??8.20± ????0.98 | ??7.65± ????1.4 | ??7.05± ????1.8 | ??6.25± ????2.0 | ??6.90± ????1.9 | ??5.80± ????1.96 | ??5.40± ????1.99 |
| ??PTS | ??10 | ??50 | ??8.22± ????0.67 | ??7.83± ????0.5 | ??7.67± ????0.6 | ??7.28± ????0.8 | ??7.06± ????0.9 | ??6.78± ????1.28* | ??6.56± ????1.04** |
| Nimodipine | ??10 | ??50 | ??8.15± ????0.89 | ??7.5± ????1.3 | ??6.95± ????1.4 | ??6.20± ????1.3 | ??6.15± ????1.1 | ??5.75± ????1.36 | ??5.35± ????1.20 |
* P＜0.05, * * P＜0.01 (comparing with the ischemic control group) t value method are carried out statistical treatment, and n is a number of animals.
From table 7 result as seen, the protoparaxotriol saporlirs high dose group was obviously improved behavior disorder in the 5th, 6 days in administration, in, low dose group has and reduces behavior scoring trend, but do not have the statistics difference, nimodipine also obviously reduced behavior scoring in the 5th, 6 day.
Table 8 protoparaxotriol saporlirs is to the influence of blocking-up intraluminal middle cerebral artery occlusion in rats cerebral infarct size
* P＜0.05 (with the comparison of ischemic control group)
Table 8 result as seen, protoparaxotriol saporlirs and nimodipine also have tangible curative effect to the cerebral infarction that causes of blocking-up intraluminal middle cerebral artery occlusion in rats, cerebral infarction organize per-cent to reduce 37.1% (P＜0.05), 28.8%, 14.3%, 31% (P＜0.05) and behavior respectively to improve the result consistent.
Four, brief summary:
1, protoparaxotriol saporlirs prevention administration (200,100,50 milligrams/kilogram/days), the continuous gastric infusion of nimodipine (50 milligrams/kilogram/days) 7 days, make the blocking-up intraluminal middle cerebral artery occlusion in rats due to cerebral infarction be plugged with obvious curative effects, cerebral infarction organizes per-cent to reduce 54.2% (P＜0.01), 44.6% (P＜0.05), 25%, 33.3% (P＜0.05) respectively, obviously improves its behavior disorder.
2, the treatment group (200,100,50 milligrams/kilogram/days) of administration, the continuous gastric infusion of nimodipine (50 milligrams/kilogram/days) were 6 days after protoparaxotriol saporlirs blocked, make that blocking tissue's per-cent of cerebral infarction has reduced 37.1% (P＜0.05), 28.8%, 14.3%, 31% (P＜0.05) respectively due to the blocking-up intraluminal middle cerebral artery occlusion in rats, also obviously improve the behavior disorder of cerebral infarction rat.
Experimental result shows that protoparaxotriol saporlirs has provide protection to the rat local cerebral ischemia.
Claims (10)
1, a kind of preparation method of protoparaxotriol saporlirs is characterized in that comprising the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be alcohol immersion 12-30 hour of 50-90%, evenly the diacolation bucket is inserted in compacting then;
B, 60% ethanol percolation to the effluent liquid of doubly measuring with medicinal material amount 6-12 do not have the saponin(e reaction, and flow velocity is every kilogram of medicinal material of 3-7 ml/min;
C, be 0.04-0.1Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, will be concentrated into the percolate that does not have behind the alcohol flavor and add water to 3-6 and doubly measure, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal material of 3-7 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
2, the preparation method of protoparaxotriol saporlirs according to claim 1 is characterized in that comprising the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be alcohol immersion 20-28 hour of 60-90%, evenly the diacolation bucket is inserted in compacting then;
B, 60% ethanol percolation to the effluent liquid of doubly measuring with medicinal material amount 8-10 do not have the saponin(e reaction, and flow velocity is every kilogram of medicinal material of 4-6 ml/min;
C, be 0.05-0.06Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 50-55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, will be concentrated into the percolate that does not have behind the alcohol flavor and add water to 5-6 and doubly measure, centrifugal, get the clear liquid upper prop, rate of addition is every kilogram of medicinal material of 4-6 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
3, the preparation method of protoparaxotriol saporlirs according to claim 1 is characterized in that comprising the following steps:
A, get pseudo-ginseng and pulverized sieve No. one, add concentration and be 60% alcohol immersion 24 hours, evenly the diacolation bucket is inserted in compacting then;
B, do not have the saponin(e reaction with 60% ethanol percolation to the effluent liquid of 10 times of amounts of medicinal material amount, flow velocity is every kilogram of medicinal material of 4-5 ml/min;
C, be 0.06Mpa in vacuum tightness, concentrating under reduced pressure percolate when temperature is 55 ℃ reclaims ethanol, and the soup after concentrating does not have the alcohol flavor, and relative density is at 1.06-1.12;
D, the percolate that will be concentrated into after nothing alcohol is distinguished the flavor of add water to 5 times of amounts, and be centrifugal, gets the clear liquid upper prop, and rate of addition is every kilogram of medicinal materials of 5 ml/min;
E, behind the washed resin post, use 40% ethanol elution, collect 40% ethanol eluate, filter, concentrating under reduced pressure, vacuum-drying in the time of 55 ℃ grinds to form powdery.
4, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, soak solution flows to end neat liquid level earlier when it is characterized in that diacolation, and the back drips 60% ethanol, and flow velocity is suitable up and down in control.
5, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, after it is characterized in that in the column chromatography step washing, doubly to measure 40% ethanol with 8-10 again and wash with 8-10 times of water gaging, control drips with take-off rate and suits mutually, dried post can not occur.
6, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, it is characterized in that protoparaxotriol saporlirs collects since first colour band, differentiate that with TLC control collects the protoparaxotriol saporlirs part, wait not develop the color to be and finish.
7, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, it is characterized in that used macroporous adsorbent resin separator column with 1% acidic alcohol or 1% sulfuric acid ethanol liquid soaked overnight, continue with distilled water flushing to neutral, can reuse.
8, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, it is characterized in that macroporous adsorbent resin is the styrene type interpolymer, model is D-101, its post footpath is 30: 160 with the ratio of post height.
9, according to the preparation method of the described protoparaxotriol saporlirs of claim 1-3, it is characterized in that the protoparaxotriol saporlirs extract that is extracted has comprised all the notoginseng triol saponins in the pseudo-ginseng, wherein ginsenoside Rg1, Re and arasaponin R1 content are followed successively by 58-74%, 5.5-8.0%, 11.0-14.0, total amount is 78-89%, the Determination of Residual Organic Solvents of product reaches the pharmaceutical grade standard, benzene is less than 2ppm, and toluene, divinylbenzene are respectively less than 20ppm.
10,, it is characterized in that can be used for treating the cardiovascular and cerebrovascular embolism class diseases according to the application of the prepared protoparaxotriol saporlirs of one of claim 1-9.
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