CN101966220A - Panaxtrial saponin extract and preparation process thereof - Google Patents
Panaxtrial saponin extract and preparation process thereof Download PDFInfo
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- CN101966220A CN101966220A CN200910069902XA CN200910069902A CN101966220A CN 101966220 A CN101966220 A CN 101966220A CN 200910069902X A CN200910069902X A CN 200910069902XA CN 200910069902 A CN200910069902 A CN 200910069902A CN 101966220 A CN101966220 A CN 101966220A
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- extract
- notoginseng
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- radix notoginseng
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- 239000000284 extract Substances 0.000 title claims abstract description 56
- 229930182490 saponin Natural products 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 150000007949 saponins Chemical class 0.000 title claims abstract description 21
- 239000001397 quillaja saponaria molina bark Substances 0.000 title abstract description 20
- 238000000605 extraction Methods 0.000 title description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 239000012141 concentrate Substances 0.000 claims abstract description 19
- 230000007935 neutral effect Effects 0.000 claims abstract description 19
- PWAOOJDMFUQOKB-WCZZMFLVSA-N ginsenoside Re Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](O[C@@H]2[C@H]3C(C)(C)[C@@H](O)CC[C@]3(C)[C@@H]3[C@@]([C@@]4(CC[C@@H]([C@H]4[C@H](O)C3)[C@](C)(CCC=C(C)C)O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C)(C)C2)O[C@H](CO)[C@@H](O)[C@@H]1O PWAOOJDMFUQOKB-WCZZMFLVSA-N 0.000 claims abstract description 11
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Abstract
The invention discloses panaxtrial saponin extract and a preparation process thereof. An extract Rg1(C42H72O14) accounts for 40 to 70 percent of the total extract; notoginsenoside R1(C47H80O18) accounts for 10 to 30 percent of the total extract; and ginsenoside Re(C48H82O18) accounts for 5 to 10 percent of the total extract. The preparation method of the extract comprises: leaching the raw materials with ethanol; concentrating extract; centrifuging concentrate; drying; passing through a neutral alumina column; eluting with an organic solvent; concentrating eluent; treating concentrate with macroporous anion exchange resin; collecting effluent and eluent; concentrating under reduced pressure to dryness; and obtaining the panaxtrial saponin extract. The extract of the invention has high purity, remarkable treatment effect and stable quality; and the preparation method has desirable separation effect and high yield, makes operation convenient, requires low cost and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of Chinese medicine extract and preparation method thereof, particularly extract protoparaxotriol saporlirs extract and the preparation thereof of Chinese medicine Radix Notoginseng.
Background technology
Radix Notoginseng: having another name called Radix Notoginseng, be the araliaceae ginseng plant, is " panacea " of the Chinese traditional treatment heart, cerebrovascular disease and various mass formed by blood stasis.The Compendium of Material Medica Ming Dynasty in 1578 Li Shizhen (1518-1593 A.D.) work: " it is little sweet and bitter to distinguish the flavor of, quite seemingly the flavor of Radix Ginseng ... so can control all disorders of blood." the supplementary Amplifications of the Compendium of Materia Medica Qing Dynasty in 1765 ZHAO Xue-Min work: " and ginseng qi-tonifying the first, Radix Notoginseng enrich blood the first, flavor with and merit also waits, so claim Panax pseudoginseng, be the most precious person of Chinese medicine." " Chinese medicine voluminous dictionary " (version in 1997) " enrich blood, and blood stasis removing decreases, and the hemostasis nosebleed can be led to and can be mended, and effect is the best, the most precious person in the side's of being medicine by the Radix Notoginseng function.Radix Notoginseng eats something rare, eliminating blood stasis to promote regeneration of blood, and subduing swelling and relieving pain, and have hemostasis not stay blood stasis, new advantage is not hindered in promoting the circulation of blood; But ripe clothes tonification is healthy and strong.”
The pharmacological action of Radix Notoginseng mainly shows as has the protection heart, obviously improves the myocardial oxygen delivery ability, increases coronary flow, the control cerebral ischemia, blood pressure lowering, expansion cardiovascular, anoxia enduring, improve myocardium microcirculation, arrhythmia suppresses effects such as arteriosclerosis and shock; Have good hemostasia effect, energy platelet increasing number, hemopoietic function improvement has and significantly invigorates blood circulation and haemolysis; There is significant analgesia role to show and improves mental activity, strengthen the learning and memory ability; Have slow down aging and antifatigue effect.In addition, Radix Notoginseng promotes the synthetic of protein and DNA, RNA, the liver protecting, functions such as two-ways regulation blood glucose in addition.
Pharmacological testing of Radix Notoginseng and clinical practice are since the '30s in this century, over particularly past more than 20 years, Chinese scholars has been carried out pharmacological research and clinical experiment widely to Radix Notoginseng, has obtained a large amount of new results, makes the field of medical applications of Radix Notoginseng obtain strong expansion.Modern pharmacological research shows that Radix Notoginseng contains polytype chemical constituent, and saponin is one of main effective ingredient of Radix Notoginseng, has multiple pharmacologically active, and saponin is a dammarane type.Total saponin content can reach 8%～12% in the Radix Notoginseng, and wherein contained monomer has 9 kinds of ginsenoside Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, Rg2, Rh etc., but based on Rb1 and Rg1.Sapogenin is panoxadiol and panaxatriol, is height with panaxatriol's content.But the aglycon of Rb1 is 20 (s)-protopanoxadiols, and the aglycon of Rg1 is 20 (s)-Protopanaxatriols.
With Radix Notoginseng monomer saponin Rg1 is that Protopanaxatriol's saponin of representative has stimulating central nervous system, hypermnesis, sets up, and promotes DNA, and RNA is synthetic, effects such as anti-platelet aggregation, and this composition content in Radix Notoginseng is 1.9%.
Rg1 also has the effect of immunomodulator in the Radix Notoginseng, and too high or too low immunoreation is returned to normally, and the lymphocytes in the activating human body, but does not disturb the normal immunoreation of human body.Panax Notoginseng saponin R g1 also can improve rat intestine epithelial cell mitochondrion encoding gene COX I, and the expression of COX II has significant protective effect to hemorrhagic shock enterocyte mitochondrial injury.Rg1 can suppress tumor necrosis factor smooth muscle blood vessel hyperplasia, uses and suppresses the tumor cell draw nutrient, reaches the purpose that suppresses tumor growth.
Rg1 is that estrogen (Estrogen) has similar identical structure with estrogen, can with the estrogen receptor combination, competition suppresses with estrogen production, reduce estrogen and the caused breast carcinoma of receptors bind and reduce incidence rate, Rb1 also has identical effect simultaneously, also has the function of angiogenesis inhibiting.
With Rb1 is the protopanoxadiol saponin of representative, promotes the formation of nerve fiber also to keep its function, prevents sexual hypofunction, suppresses the central nervous system, have antitonic, suppress maincenter calmness, calm the nerves, analgesic, hypnotic effect; Promote serum albumin synthetic, promote cholesteric synthetic and decomposition, suppress neutral fat and decompose anti-hemolysis.This composition content in Radix Notoginseng reaches 1.8%.
Ginsenoside Rb1 in the flower of Radix Notoginseng, Rb3, Rc and Rg3 can work in coordination with colorectal cancer medicine fluorine hybar X (5-Fluorouracil) and induce the colorectal cancer cells apoptosis, to mend the deficiency that the fluorine hybar X can't cell death inducing.
The effect of other composition is as follows in the Radix Notoginseng:
The ginsenoside Rb2 suppresses nervus centralis, promotes DNA, and RNA is synthetic, anti-hemolysis, anti-diabetic.The Ginsenoside Rc suppresses nervus centralis, promotes DNA, and RNA is synthetic, promotes serum albumin synthetic.Ginsenoside Rd's raise immunity, anticancer is grown up.The ginsenoside Rh2 promotes that cancerous cell transformation is non-cancerous cell.Tetracyclic triterpene dammarane type Protopanaxatriol saponins ginsenoside Re suppresses nervus centralis, promotes DNA, and RNA is synthetic.The ginsenoside Rg2 anti-platelet aggregation.Ginsenoside Rh1 promotes that cancerous cell transformation is non-cancerous cell.Arasaponin R1 inducing leukemia cell differentiation.
Because Radix Notoginseng has above advantage, present development and use to Radix Notoginseng also become the focus in the field of medicaments.Chinese patent 200410073881.6 discloses a kind of notoginseng triol saponins compositions and preparation method.This patent adopts macroporous adsorbent resin to separate, and notoginseng triol effectively can not be separated the too high levels of Rb1 in the extract with notoginseng diol.
Chinese patent 200610066204.0 discloses a kind of notoginseng total saponin compounds that is used for the treatment of cardiovascular disease.The extraction process of this patent adopts D type macroporous adsorbent resin to separate the notoginseng total saponin compounds Rg135%-50% that extracts, Rb120%-35% under the process conditions of this patent.Notoginseng triol does not effectively separate with notoginseng diol, the too high levels of notoginseng diol.
Because above technology is separated notoginseng triol and notoginseng diol poor effect, therefore, need improve existing extractive technique, notoginseng triol can effectively be separated with notoginseng diol, prepare the high extract of notoginseng triol content.
Summary of the invention
For addressing the above problem, the inventor is carrying out in the research process protoparaxotriol saporlirs, tests out one group of new notoginseng triol group saponin extract and preparation method thereof, can realize that notoginseng triol saponins and the effective of notoginseng glycol saponins separate.
The purpose of this invention is to provide a kind of Chinese medicine composition that contains notoginseng triol saponins extract for the treatment of cardiovascular and cerebrovascular disease.
For realizing described above-mentioned purpose, the present invention by the following technical solutions:
A kind of notoginseng triol saponins extract wherein contains Rg1 (C
42H
72O
14) content accounts for total extract 40～70%, arasaponin R1 (C
47H
80O
18) content accounts for total extract 10～30%, ginsenoside Re (C
48H
82O
18) content accounts for total extract 5～10%.
Preferably, Rg1 is no less than 50～65%, and arasaponin R1 is no less than 15～25%, and the ginsenoside Re is no less than 5～8%.
Above-mentioned Rg1 (C
42H
72O
14), arasaponin R1 (C
47H
80O
18) and ginsenoside Re's content summation less than 100%.
Preferably, in the extract of the present invention total saponin content is controlled at more than 80%; More preferably, total saponin content is controlled at more than 85%.
Preferably, Rb1 no more than 10% in the extract of the present invention; More preferably, Rb1 no more than 8%.
Preferably, total saponin content is controlled at more than 80% in the extract of the present invention, and Rb1 no more than 10%.
Preferably, total saponin content is controlled at more than 85% in the extract of the present invention, and Rb1 no more than 8%.
Above-mentioned notoginseng triol saponins extract character is faint yellow or chocolate brown powder, bitter in the mouth; Moisture is no more than 10.0%.
Another object of the present invention provides a kind of medicine for the treatment of containing of cardiovascular and cerebrovascular disease above-mentioned notoginseng triol saponins extract.Described medicine is made by above-mentioned notoginseng triol saponins extract and acceptable accessories.
Described medicine acceptable auxiliary can be selected from: mannitol, sorbitol, sodium pyrosulfite, sodium sulfite, sodium thiosulfate, cysteine hydrochloride, TGA, methionine, vitamin C, the EDTA disodium, EDTA calcium sodium, the alkali-metal carbonate of monovalence, acetate, phosphate or its aqueous solution, hydrochloric acid, acetic acid, sulphuric acid, phosphoric acid, aminoacid, sodium chloride, potassium chloride, sodium lactate, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, mannitol, silicon derivative, cellulose and derivant thereof, alginate, gelatin, polyvinylpyrrolidone, glycerol, soil temperature 80, agar, calcium carbonate, calcium bicarbonate, surfactant, Polyethylene Glycol, cyclodextrin, beta-schardinger dextrin-, the phospholipid material, Kaolin, Pulvis Talci, calcium stearate, magnesium stearate etc.
The active component of medicine of the present invention can add various conventional adjuvant required when preparing different dosage form, be prepared into any common formulations as disintegrating agent, lubricant, binding agent etc. with the method for Chinese medicinal of routine, as injectable powder, tablet, pill, powder, granule, capsule, syrup, drop pill, oral liquid and other acceptable dosage form pharmaceutically, as suck agent, electuary, unguentum, sublimed preparation, suspensoid, solution, injection, suppository, ointment, plaster, cream, spray, drop, patch etc.
Another object of the present invention provides a kind of notoginseng triol saponins preparation method of extract.The preparation method of notoginseng triol saponins of the present invention may further comprise the steps:
A. get Radix Notoginseng, be ground into coarse granule, add 4-20 and doubly measure 45%-95% ethanol decoction twice, each 1-3 hour;
B. collecting decoction is evaporated to 1-2 times of volume of medical material amount below 70 ℃;
C. leave standstill to room temperature, 3500-6000rpm, the centrifugal or 100-300 order of 20min filters, and isolates supernatant, and it is standby to be evaporated to dry powder below 70 ℃
D. drying sample is crossed neutral alumina post (sample to be separated and chromatography alumina ration 1: 40～200);
E. use organic solvent and water certain volume than 1: 1～10 eluting, thin layer is judged the eluting terminal point; Preferably, described organic solvent is methanol or ethanol;
F. eluent vacuum decompression below 70 ℃ reclaims organic solvent; Concentrated solution water is diluted to 2～10 times of volumes of medical material;
G. macroporous anion exchange resin on the diluent, resin and medical material 0.5～1: 1g/g, last sample flow velocity is 0.5～1.5BV/h, 5-10 times of column volume, flow velocity 1～1.5BV/h, washing;
H. collect and go up sample effluent and eluent, vacuum decompression below 70 ℃ is concentrated into does or adopts lyophilizing or spray to do, promptly.
Because the under ground portion of Radix Notoginseng is to contain ginsenoside Rg1 and Rb1, the aerial parts of Radix Notoginseng only is separated to the saponin of protopanoxadiol, does not find pentacyclic triterpene saponin, so the used material of the present invention Radix Notoginseng preferably.
In the above-mentioned preparation method, when among the preferred steps a raw material being added ethanol extraction, add 6 times of amount 70% ethanol for the first time, decocted 2.5 hours; Add for the second time 5 times of amount 70% ethanol, decocted 2 hours.
In the above-mentioned preparation method, concentrate at 55-70 ℃ among preferred steps b, c, f and the g; Preferably, 70 ℃ of concentrating under reduced pressure.
In the above-mentioned preparation method, the preferred D941 resin of macroporous anion exchange resin in the step g.
Thin layer chromatography condition: chloroform: ethyl acetate: methanol: water (15: 40: 22: 10) lower floor, launch the back with spray 10% sulphuric acid ethanol, heat 105 ℃ of colour developings.
The active component that preparation method of the present invention is extracted, the content of Rg1 and R1 improves greatly, can realize separating of triol group and glycol group; Glycol saponins Rb1 content is limited in below 10%; Definite ingredients in the total saponin extracts, the composition that structure is clear and definite accounts for more than 80%; Finished product decolouring back color is more shallow than existing technology, the suitable freeze-dried powder of doing.These protoparaxotriol saporlirs extracts have the purity height, good effect, and steady quality, the preparation method separating effect is good simultaneously, the content height, technology is simple, and is easy to operate, with low cost, is fit to suitability for industrialized production.
The specific embodiment
Present embodiment is for the ease of understanding the present invention, and claim that does not limit the present invention in any way and core content.
Embodiment 1
Get Radix Notoginseng 20.0g, be ground into coarse granule, add 6 times of amount 70% alcohol reflux 2 times, 2.5 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in 60 ℃ of 1.5 times of being evaporated to medical material, 4200rpm, 20min is centrifugal, isolate supernatant, 70 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 110, with ethanol and 1: 10 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 70 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.5: 1g/g, last sample flow velocity is 0.5BV/h, 5 times of column volumes, flow velocity 1BV/h, washing; Sample effluent and water lotion in the collection, 70 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 2
Get Radix Notoginseng 20.0, be ground into coarse granule, add 4 times of amount 70% alcohol reflux 2 times, 1 hour for the first time, 1 hour merge extractive liquid, for the second time, extracting solution is in 55 ℃ of 1.5 times of being evaporated to medical material, 4000rpm, 20min is centrifugal, isolate supernatant, 59 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 60, with methanol or ethanol and 1: 6 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 59 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.7: 1g/g, last sample flow velocity is 0.8BV/h, 8 times of column volumes, flow velocity 1.3BV/h, washing; Sample effluent and water lotion in the collection, 59 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 3
Get Radix Notoginseng 100.0g, be ground into coarse granule, add 40 times of amount 70% alcohol reflux 2 times, 3 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in 65 ℃ of 2 times of being evaporated to medical material, 6000rpm, 20min is centrifugal, isolate supernatant, 58 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 70, with ethanol and 1: 6 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 58 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 1: 1g/g, last sample flow velocity is 1.5BV/h, 10 times of column volumes, flow velocity 1.5BV/h, washing; Sample effluent and water lotion in the collection, 58 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 4
Get Radix Notoginseng 50.0g, be ground into coarse granule, add 8 times of amount 50% alcohol reflux 2 times, 2.5 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in 65 ℃ of 1. times of being evaporated to medical material, 5500rpm, 2h is centrifugal, isolate supernatant, 65 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 170, with methanol and 1: 10 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 65 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.5～1: 1g/g, last sample flow velocity is 0.9BV/h, 5 times of column volumes, flow velocity 1.3BV/h, washing; Sample effluent and water lotion in the collection, 65 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 5
Get Radix Notoginseng 30g, be ground into coarse granule, add 10 times of amount 95% alcohol reflux 2 times, 1.5 hours for the first time, 1.5 hours merge extractive liquid, for the second time, extracting solution is in 64 ℃ of 1.5 times of being evaporated to medical material, 4200rpm, 20min is centrifugal, isolate supernatant, 70 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 90, with ethanol and 1: 9 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 60 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.7: 1g/g, last sample flow velocity is 0.7BV/h, 6.5 times of column volumes, flow velocity 1.4BV/h, washing; Sample effluent and water lotion in the collection, 70 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 6
Get Radix Notoginseng 25g, be ground into coarse granule, add 35 times of amount 70% alcohol reflux 2 times, 2.5 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in being evaporated to 1.5 times of medical material below 61 ℃, 4200rpm, 20min is centrifugal, isolate supernatant, 61 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 50, with ethanol and 1: 6 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 61 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.6: 1g/g, last sample flow velocity is 0.5BV/h, 5 times of column volumes, flow velocity 1BV/h, washing; Sample effluent and water lotion in the collection, 61 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 7
Get Radix Notoginseng 40g, be ground into coarse granule, add 30 times of amount 75% alcohol reflux 2 times, 3 hours for the first time, 1 hour merge extractive liquid, for the second time, extracting solution is in 56 ℃ of 1.5 times of being evaporated to medical material, 5000rpm, 20min is centrifugal, isolate supernatant, 63 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 190, with the eluant eluting of methanol or ethanol and water volume ratio 1: 1～10, thin layer is judged the eluting terminal point; 63 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 1: 1g/g, last sample flow velocity is 0.6BV/h, 9 times of column volumes, flow velocity 1.5BV/h, washing; Sample effluent and water lotion in the collection, 63 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 8
Get Radix Notoginseng 80g, be ground into coarse granule, add 25 times of amount 70% alcohol reflux 2 times, 1 hour for the first time, 1 hour merge extractive liquid, for the second time, extracting solution is in 58 ℃ of 1.5 times of being evaporated to medical material, 6000rpm, 20min is centrifugal, isolate supernatant, 66 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 120, with ethanol and 1: 3 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 66 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.8: 1g/g, last sample flow velocity is 1.1BV/h, 10 times of column volumes, flow velocity 1.1BV/h, washing; Sample effluent and water lotion in the collection, 66 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 9
Get Radix Notoginseng 70g, be ground into coarse granule, add 20 times of amount 75% alcohol reflux 2 times, 2.5 hours for the first time, 1.5 hours merge extractive liquid, for the second time, extracting solution is in being evaporated to 1.5 times of medical material below 62 ℃, 4200rpm, 20min is centrifugal, isolate supernatant, 62 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 160, with methanol and 1: 4 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 62 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.7: 1g/g, last sample flow velocity is 0.6BV/h, 7 times of column volumes, flow velocity 1.4BV/h, washing; Sample effluent and water lotion in the collection, 62 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 10
Get Radix Notoginseng 65g, be ground into coarse granule, add 15 times of amount 70% alcohol reflux 2 times, 2 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in 61 ℃ of 1.5 times of being evaporated to medical material, 4500rpm, 20min is centrifugal, isolate supernatant, 64 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 80, with ethanol and 1: 2 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 64 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.6: 1g/g, last sample flow velocity is 0.9BV/h, 9 times of column volumes, flow velocity 1.1V/h, washing; Sample effluent and water lotion in the collection, 64 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 11
Get Radix Notoginseng 55, be ground into coarse granule, add 10 times of amount 80% alcohol reflux 2 times, 2.5 hours for the first time, 2.5 hours merge extractive liquid, for the second time, extracting solution is in 60 ℃ of 1.5 times of being evaporated to medical material, 4600rpm, 20min is centrifugal, isolate supernatant, 60 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 150, with methanol and 1: 1 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 60 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.5: 1g/g, last sample flow velocity is 0.5BV/h, 5 times of column volumes, flow velocity 1.3BV/h, washing; Sample effluent and water lotion in the collection, 60 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 12
Get Radix Notoginseng 15g, be ground into coarse granule, add 12 times of amount 90% alcohol reflux 2 times, 2.5 hours for the first time, 2.5 hours merge extractive liquid, for the second time, extracting solution is in 68 ℃ of 1.5 times of being evaporated to medical material, 4800rpm, 20min is centrifugal, isolate supernatant, 55 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 200, with ethanol and 1: 5 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 55 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.8: 1g/g, last sample flow velocity is 1.2BV/h, 6 times of column volumes, flow velocity 1BV/h, washing; Sample effluent and water lotion in the collection, 55 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 13
Get Radix Notoginseng 45g, be ground into coarse granule, add 18 times of amount 70% alcohol reflux 2 times, 3 hours for the first time, 2 hours merge extractive liquid, for the second time, extracting solution is in 69 ℃ of 1.5 times of being evaporated to medical material, and 300 orders filter, isolate supernatant, 70 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 100, with methanol and 1: 8 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 70 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.9: 1g/g, last sample flow velocity is 1.0BV/h, 8 times of column volumes, flow velocity 1.2BV/h, washing; Sample effluent and water lotion in the collection, 70 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
Embodiment 14
Get Radix Notoginseng 90g, be ground into coarse granule, add 28 times of amount 50% alcohol reflux 2 times, 3 hours for the first time, 2.5 hours merge extractive liquid, for the second time, extracting solution is in 57 ℃ of 1.5 times of being evaporated to medical material, and 200 orders filter, isolate supernatant, 65 ℃ are evaporated to dry powder, cross the neutral alumina post, and sample to be separated and chromatography are used alumina ration 1: 40, with ethanol and 1: 10 eluant eluting of water volume ratio, thin layer is judged the eluting terminal point; 65 ℃ of vacuum decompressions concentrate and reclaim organic solvent, D941 resin decolorization behind the concentrated solution dilute with water, and resin and medical material 0.5: 1g/g, last sample flow velocity is 1.5BV/h, 10 times of column volumes, flow velocity 1.5BV/h, washing; Sample effluent and water lotion in the collection, 70 ℃ of vacuum decompressions are concentrated into to be done or conventional method lyophilizing, spray are done, promptly.
The high effective liquid chromatography for measuring extractive content
The test example
High effective liquid chromatography for measuring Rg1, Rb1, arasaponin R1, ginsenoside Re's content
[assay] is according to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.05% phosphoric acid solution (99: 400) is a mobile phase; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Re peak should be not less than 2500.
The preparation of reference substance solution precision respectively takes by weighing the ginsenoside Rg1, and ginsenoside Re and arasaponin R1 are an amount of.Add methanol and make solution, the arasaponin R1 0.6mg that every 1ml contains ginsenoside Rg1 1.3mg, ginsenoside Re 0.2mg respectively, promptly.
The extract that the preparation embodiment 1 and 2 of need testing solution makes is tested the sample of first and second batch respectively as this.The extract of other embodiment preparation and other adopt the checking through the inventor of extract that preparation method of the present invention obtains, have identical effect with embodiment 1 with 2 sample.
Get in this product powder 0.05g to 25ml volumetric flask, accurate claim surely, add the 20ml dissolve with methanol, supersound process is put and is added methanol constant volume to scale after cold, shakes up, and filters, promptly.
Accurate respectively above-mentioned reference substance solution each 10 μ l and the need testing solution 10 μ l of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The active component that preparation method of the present invention is extracted, the content of Rg1 and R1 improves greatly, can realize separating of triol group and glycol group; Glycol saponins Rb1 content is limited in below 10%; Definite ingredients in the total saponin extracts, the composition that structure is clear and definite accounts for more than 80%; Finished product decolouring back color is more shallow than existing technology, the suitable freeze-dried powder of doing.These protoparaxotriol saporlirs extracts have the purity height, good effect, and steady quality, the preparation method separating effect is good simultaneously, the content height, technology is simple, and is easy to operate, with low cost, is fit to suitability for industrialized production.
Product feature
This product is a pale yellow powder, yield 1～4%, and total saponins is (Rg1+R1+Re) more than 80%
Claims (10)
1. a notoginseng triol saponins extract is characterized in that Rg1 (C
42H
72O
14) content range accounts for total extract 40～70%, arasaponin R1 (C
47H
80O
18) content range accounts for total extract 10～30%, ginsenoside Re (C
48H
82O
18) content range accounts for total extract 5～10%.
2. notoginseng triol saponins extract according to claim 1 is characterized in that Rg1 content accounts for total extract 50～65%, and arasaponin R1 content accounts for total extract 15～25%, and ginsenoside Re's content accounts for total extract 5～10%.
3. notoginseng triol saponins extract according to claim 1 is characterized in that moisture is no more than 10.0% in the extract.
4. according to the described arbitrary notoginseng triol saponins extract of claim 1-3, it is characterized in that content of the total saponins in radix notoginseng is more than 80%, Rb1 no more than 10% in the Radix Notoginseng total arasaponins.
5. arbitrary notoginseng triol saponins extract according to claim 4 is characterized in that content of the total saponins in radix notoginseng is more than 85%, and Rb1 no more than 8% in the Radix Notoginseng total arasaponins.
6. the described notoginseng triol saponins of claim 1 preparation method of extract, may further comprise the steps: with raw material with ethanol extraction, extracting solution concentrates, concentrated solution is centrifugal, and neutral alumina post, organic solvent eluting are crossed in dry back, eluent concentrates the back and goes up the macroporous anion exchange resin processing, collect effluent and eluent, be evaporated to driedly, promptly get arasaponin triol group extract.
7. notoginseng triol saponins preparation method of extract according to claim 6 is characterized in that, may further comprise the steps:
A. get Radix Notoginseng, be ground into coarse granule, add ethanol and decoct twice, each 1-3 hour;
Described when raw material is added ethanol extraction, add raw material 4-20 and doubly measure 45%-95% ethanol and decoct, add 6 times of amount 70% ethanol for the first time, decocted 2.5 hours; Add for the second time 5 times of amount 70% ethanol, decocted 2 hours;
B. collecting decoction, 55-70 ℃ of 1～2 times of volume that is evaporated to the medical material amount;
C. leave standstill to room temperature, 3500-6000rpm, the centrifugal or 100-300 order of 20min filters, and isolating supernatant 55-70 ℃, to be evaporated to dry powder standby;
D. cross the neutral alumina post on the dry powder, organic solvent and water certain volume are collected eluent than 1: 1～10 eluting; Described sample to be separated is 1: 40～200 with chromatography with the alumina weight ratio, and organic solvent and water certain volume are than 1: 1～10 eluting;
E. eluent 55-70 ℃ of vacuum decompression reclaims organic solvent; Concentrated solution water is diluted to 2～10 times of volumes of medical material;
F. macroporous anion exchange resin on the diluent, resin and medical material 0.5～1: 1g/g, last sample flow velocity is 0.5～1.5BV/h, 5-10 times of column volume, flow velocity 1～1.5BV/h, washing;
G. collect and go up sample effluent and eluent, 55-70 ℃ of vacuum decompression is concentrated into does or adopts lyophilizing or spray to do, promptly.
8. notoginseng triol saponins preparation method of extract according to claim 7 is characterized in that the raw material among the step a is a Radix Notoginseng.
9. notoginseng triol saponins preparation method of extract according to claim 7 is characterized in that the decompression temperature among step b, c, e and the g is 70 ℃.
10. the made medicine of the described protoparaxotriol saporlirs extract of claim 1.
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| CN200910069902XA CN101966220A (en) | 2009-07-27 | 2009-07-27 | Panaxtrial saponin extract and preparation process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103372041A (en) * | 2012-04-25 | 2013-10-30 | 天津天士力现代中药资源有限公司 | Component with anticoagulation and preparation method thereof |
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| CN1699397A (en) * | 2004-08-04 | 2005-11-23 | 李明劲 | Process for preparing notoginseng triol saponin and use thereof |
| CN1869050A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of preparing notoginseng saponine Fe and diol group ginseng saponine from netoginseng leaf |
| CN1869056A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
| CN1923228A (en) * | 2005-08-31 | 2007-03-07 | 蔡军 | Pharmaceutical composition comprising notoginseng extract, Danshen extract and ligustrazine |
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2009
- 2009-07-27 CN CN200910069902XA patent/CN101966220A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699397A (en) * | 2004-08-04 | 2005-11-23 | 李明劲 | Process for preparing notoginseng triol saponin and use thereof |
| CN1923228A (en) * | 2005-08-31 | 2007-03-07 | 蔡军 | Pharmaceutical composition comprising notoginseng extract, Danshen extract and ligustrazine |
| CN1869050A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of preparing notoginseng saponine Fe and diol group ginseng saponine from netoginseng leaf |
| CN1869056A (en) * | 2006-06-21 | 2006-11-29 | 海南亚洲制药有限公司 | Method of extracting and separating ginseng saponine mixture from ginseng leaf |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103372041A (en) * | 2012-04-25 | 2013-10-30 | 天津天士力现代中药资源有限公司 | Component with anticoagulation and preparation method thereof |
| CN103372041B (en) * | 2012-04-25 | 2017-10-10 | 天津天士力现代中药资源有限公司 | A kind of component with blood coagulation resisting function and preparation method thereof |
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Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Applicant after: Tasly Pharmaceutical Group Co., Ltd. Address before: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Applicant before: Tianjin Tianshili Pharmaceutical Co., Ltd. |
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Application publication date: 20110209 |