CN102145034A - Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract - Google Patents

Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract Download PDF

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CN102145034A
CN102145034A CN 201110093879 CN201110093879A CN102145034A CN 102145034 A CN102145034 A CN 102145034A CN 201110093879 CN201110093879 CN 201110093879 CN 201110093879 A CN201110093879 A CN 201110093879A CN 102145034 A CN102145034 A CN 102145034A
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ginsenoside
radix notoginseng
saponin
extract
resin
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高明菊
崔秀明
赵爱
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Wenshan sanqi research institute
YUNNAN WENSHAN QIDAN PHARMACEUTICAL CO Ltd
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Wenshan sanqi research institute
YUNNAN WENSHAN QIDAN PHARMACEUTICAL CO Ltd
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Abstract

The invention provides a radix notoginseng extract which is extracted from fresh radix notoginseng as a raw material, and a preparation method of the radix notoginseng extract and a medicinal prescription prepared from the radix notoginseng extract as an active component. The radix notoginseng extract of the invention comprises the following components: 4-10%radix notoginseng saponin R1, 23-36% ginseng saponin Rg1, 2-5% ginseng saponin Re, 27-39% ginseng saponin Rb1 and 3-10% ginseng saponin Rd, wherein the radix notoginseng saponin R1, the ginseng saponin Rg1, the ginseng saponin Re, the ginseng saponin Rb1 and the ginseng saponin Rd account for 65-95% of the total weight. The radix notoginseng extract prepared by the method in the invention has few impurities, and total saponin component is high in impurity. The medicinal prescription prepared by the radix notoginseng extract as the active component has good curative effect and high safety.

Description

A kind of Radix Notoginseng extract and preparation method thereof and its pharmaceutical formulation
Technical field
The invention belongs to medical technical field, particularly, relate to a kind of Radix Notoginseng extract, is the pharmaceutical formulation of active component with it, extracts the method for Radix Notoginseng total arasaponins from bright Radix Notoginseng.
Background technology
Radix Notoginseng Panax notoginseng (Buck) F. H. Chen is the araliaceae ginseng plant, and good reputations such as " Radix Stephaniae Sinicae (Radix Stephaniae Dielsianae) ", " southern part of the country SHENCAO " are arranged, and is China's rare Chinese medicine, also is the Chinese material medicine resource that shows unique characteristics in Yunnan, main product Yunnan mountain of papers.Mountain of papers becomes the original producton location of Chinese medicine notoginseng planting with its special natural condition advantage, and its output accounts for more than 90% of national total output.
Experts and scholars both domestic and external have carried out comparatively systematic research to the chemical constituent of Radix Notoginseng, have been separated to multiple dammarane type triterpene saponin at present from Radix Notoginseng, that is: ginsenoside (ginsenoside) Rb 1, Rb 2,, Rc, Rd, Rg 1, Re,, Rg 2, Rh 1, Rg 3, 20-(O)-glucose ginsenoside Rf, F 1, Ra 3, arasaponin (notoginsenoside) R 1, R 2, R 3, R 4, R 6, R8, R9, A, B, C, D, E, G, H, I, J, K, L, M, O, P, Q, L, S, T, blue saponin (gypenoside) XVII of glue thigh.Add that other position of Radix Notoginseng separates the chemical compound that obtains, separated in the Radix Notoginseng saponins compound that obtains reached 70 surplus kind.But its main component is a Radix Notoginseng total arasaponins still, comprises Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd, R in the Radix Notoginseng main root 1+ Rg 1+ Rb 1〉=5%, and R in the Radix Notoginseng reed head 1+ Rg 1+ Rb 1Three's content sum is greater than 10%.
The method of Radix Notoginseng common extraction total saponins in producing has: cold-maceration, alcohol reflux, water extraction; Solvent for use is ethanol, water; The raw materials used dry product raw material that is.Content of starch reaches about 70% in the Radix Notoginseng, generally should not adopt water or low-concentration ethanol to extract, in order to avoid gelatinizing.Therefore the alcohol reflux extraction is the optimum selection of this method.The tradition Radix Notoginseng is extracted and all adopts dry product to extract.The ethanol of many employings 60% or 70% extracts, but because the difference that technological parameter is selected in the leaching process can directly cause Radix Notoginseng total arasaponins effective ingredient kind and content difference very big.The dry product water content must be smaller or equal to 14% by China's pharmacopeia requirement.It is about 20% that bright arasaponin content is higher than the dry product Radix Notoginseng, and bright product Radix Notoginseng water content about 70%.Therefore, be that raw material extracts active component than being a comparatively ideal selection with dry product as raw material with bright Radix Notoginseng.
Summary of the invention
The purpose of this invention is to provide the bright Radix Notoginseng of a kind of usefulness is the high Radix Notoginseng extract of saponin content that raw material extracts.
It is the method for feedstock production Radix Notoginseng extract that another object of the present invention provides the bright Radix Notoginseng of a kind of usefulness.
A further object of the present invention provides the pharmaceutical preparation that a kind of extract that is extracted by bright Radix Notoginseng is made.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
Radix Notoginseng extract, it contains Panax Notoginseng saponin R 14~10%, ginsenoside Rg 123~36%, ginsenoside Re 2~5%, ginsenoside Rb 127~39%, the ginsenoside Rd 3~10%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~95% of total amount.
Preferred Radix Notoginseng extract, it contains Panax Notoginseng saponin R 14~7%, ginsenoside Rg 123~30%, ginsenoside Re 2~3.5%, ginsenoside Rb 127~35%, the ginsenoside Rd 4~7%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~85% of total amount.
Preferred Radix Notoginseng extract, it contains Panax Notoginseng saponin R 17~8%, ginsenoside Rg 127~34%, ginsenoside Re 3~4%, ginsenoside Rb 133~36%, the ginsenoside Rd 6~8%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 80~90% of total amount.
The present invention provides Radix Notoginseng extract simultaneously, and it contains Panax Notoginseng saponin R 14~10%, ginsenoside Rg 123~36%, ginsenoside Re 2~5%, ginsenoside Rb 127~39%, the ginsenoside Rd 3~10%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~95% of total amount, extract and get by following method:
Adopting bright Radix Notoginseng is raw material; earlier Radix Notoginseng main root or reed head are broken into the granule of 6-10mm or are cut into the thin slice of thickness at 1-3mm; 70%~95% ethanol of doubly measuring with 6-8 extracted 6-10 hour through the hot reflux circulation; place and filter; the collection filtrate decompression concentrates, and through macroporous adsorptive resins absorption, uses the 70-80% ethanol elution then; eluent decolouring back concentrating under reduced pressure, drying.
The percent of above-described each component is percetage by weight.
The present invention provides the method for preparing above-mentioned any described Radix Notoginseng extract in addition: adopting bright Radix Notoginseng main root or Radix Notoginseng clip is raw material; earlier Radix Notoginseng main root or reed head are broken into the granule of 6-10mm or are cut into the thin slice of thickness at 1-3mm; 70%~95% ethanol of doubly measuring with 6-8 extracted 6-10 hour through the hot reflux circulation; place and filter; the collection filtrate decompression concentrates, and through macroporous adsorptive resins absorption, uses the 70-80% ethanol elution then; eluent decolouring back concentrating under reduced pressure, drying.
Macroporous adsorbent resin adopts the D101 macroporous resin in the described method; D941 resin and medicinal charcoal two-step bleaching are adopted in decolouring; Concentrate and adopt haplo-effect concentrator.
The present invention's method more specifically can be described as:
(1) getting fresh Radix Notoginseng main root or reed head is broken into the granule of coarse powder 6-10mm or is cut into the thin slice of thickness at 1-3mm, doubly measuring the circulation of 70%~95% alcohol heat reflux with 6-8 extracted 6-10 hour, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.20-0.30g crude drug/ml, mixing, precipitate 12-18 hour, centrifugal removal impurity filters;
(2) described (1) step gained filtrate is that the flow velocity of 1.0-1.4BV/H is through the D101 macroporous resin adsorption with the flow velocity, the purified water of doubly measuring with resin volume 1-4 is crossed post and is removed impurity then, flow velocity 2-4BV/h, discard water liquid, doubly measure with the speed eluting of flow velocity 2-4BV/h with the alcoholic solution 3-5 of 70-80% and to collect loss of thick fluid liquid, detect no saponin outflow to TLC till;
(3) be that 6 flow velocitys that rise to 9 liters/min are crossed the D941 resin decolorization with (2) step gained eluent with flow velocity again, after finishing on the eluent, adding resin 1-3 doubly measures the ethanol of 70-80% with identical flow velocity flushing resin column, till flowing out to the no saponin of TLC detection, merges first flow liquid and eluent;
(4) medicinal charcoal that adds crude drug weight 4-6% after (3) step filters carbon removal in 45~55 ℃ of insulation decolourings 30~40 minutes under this temperature, and concentrating under reduced pressure reclaims ethanol, being concentrated into relative density is 1.05-1.20, centrifugal, remove insoluble matter, last drying under reduced pressure.
The present invention also provides the pharmaceutical formulation of being made by Radix Notoginseng extract of the present invention, and described pharmaceutical formulation is injection, lyophilized injectable powder, infusion solution, capsule, granule or tablet.
At present, the conventional extracting method of Radix Notoginseng total arasaponins is dry product medical material merceration and alcohol reflux, water extraction, again through adsorbent resin enrichment total saponins composition, and the composition of adsorbent resin enrichment mostly is the higher arasaponin R1 of content, the ginsenoside Rg1, the ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd; The inventive method has been used bright Radix Notoginseng raw material, is optimized extracting solvent simultaneously, and the Radix Notoginseng total arasaponins composition purity height that makes extraction, it is higher to extract yield.Therefore bright product extraction method is the advantage place of this method.
Radix Notoginseng extract of the present invention can be made different pharmaceutical formulations by Radix Notoginseng extract or Radix Notoginseng extract with pharmaceutic adjuvant, such as injection, lyophilized injectable powder, infusion solution, capsule, granule or tablet according to preparation method well known in the art.
Described pharmaceutic adjuvant is sodium chloride, glucose, starch, dextrin, sucrose, Pulvis Talci, magnesium stearate.
The present invention adopts high performance liquid chromatograph, carry out the method for gradient elution with acetonitrile and water as mobile phase the composition in Radix Notoginseng extract and the preparation is differentiated detection, chromatographic peak after 5 minutes, main chromatographic peak with the Radix Notoginseng total arasaponins reference extract is proofreaied and correct, and the similarity of Radix Notoginseng extract and preparation thereof is more than 0.95.
Particularly, the present invention adopts high performance liquid chromatograph, carry out the method for gradient elution with acetonitrile and aqueous solution as mobile phase saponin constituent in Radix Notoginseng extraction and the preparation thereof is carried out HPLC discriminating detection, the peak sequence of each composition is followed successively by: arasaponin R1, the ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd.
To sum up, compared with prior art, Radix Notoginseng extract of the present invention and preparation thereof and extracting method thereof have the following advantages:
1, Radix Notoginseng extract purity height, of light color, impurity is few.
2, through the Radix Notoginseng extract of the inventive method preparation than the high 1-2% of traditional method yield.
3, the content of Radix Notoginseng extract yield, content and the preparation that gets through the inventive method preparation is apparently higher than the sample of conventional method preparation, and total saponin content can promote 10~25%.
When 4, the Radix Notoginseng extract content that gets through the inventive method preparation promotes, the corresponding minimizing of impurity component.With icp ms inorganic elements in the Radix Notoginseng extract is measured, the result, heavy metal and harmful element content are less than 0.0007 ‰; With gas chromatograph the macroporous adsorbent resin organic residue in the Radix Notoginseng extract is detected, the result does not detect n-hexane, benzene, toluene, xylol, o-Dimethylbenzene, styrene, 1,2-diethylbenzene and divinylbenzene.
5, by results such as depressor substance inspection, irritated inspection, undue toxicity's inspection, pyrogen test, haemolysis and cohesion inspection, irritant tests, show by the preparation security of this Radix Notoginseng extract preparation higher.
The specific embodiment:
With test example of the present invention excellent effect of the present invention is described below:
Test example 1:
The present invention is the optimised process selection test that raw material extracts Radix Notoginseng extract with bright Radix Notoginseng:
1, concentration of alcohol is selected: the bright granule that bright Radix Notoginseng rhizome is broken into 6-10mm with disintegrating machine, select three factors, four levels to test and investigate hot reflux extraction time (h), consumption of ethanol (doubly), concentration of ethanol (%) is as the investigation factor, with dry extract extraction ratio and five monomer saponin content (R1, Rg1, Rb1, Re, Rd) % serves as to investigate index, selects (3 for use 4) orthogonal table tests.The factor level arrangement sees the following form.
Figure 2011100938795100002DEST_PATH_IMAGE001
By the value of testing result as can be known, serve as to investigate index with yield of extract, five monomers (R1+Rg1+Rb1+ Re+Rd) content sum, the optimum extraction process condition is that 6~10 hours extraction times, concentration of alcohol are that 70%~95% ethanol, ethanol consumption are 6~8 times.
2, the selection of macroporous resin:
At present macroporous resin has different models, but commonly used be D101, HPD-100,2 kinds of resins all can enrichment, the separation and purification Radix Notoginseng total arasaponins, and is 400-500m for the non-polar macroporous resin and the surface area of polystyrene structure 2/ g, and be the most frequently used kind in the present stage production.So select for use the D101 macroporous resin to handle.
3, the selection of elution requirement:
Factors such as flow velocity when the present invention has also investigated behind the selection of eluant, the selection of going up column liquid concentration, the upper prop with distilled water fast towards doubly amount, the eluting of doubly amount, the eluant of post, these five factors are all influential to the purification of Radix Notoginseng total arasaponins.
Figure 961573DEST_PATH_IMAGE002
The optimum washing engaging condition of having selected to extract in the elution process through above orthogonal test the present invention is: the purified water of doubly measuring with resin volume 1-4 is crossed post and is removed impurity, flow velocity 2-4BV/h, discard water liquid, doubly measure with the speed eluting of flow velocity 2-4BV/h with the ethanol 3-5 of 70-80% and to collect loss of thick fluid liquid, till detecting no saponin outflow.
4, the selection of decolorizing resin:
Prove that through test of many times D101 macroporous resin separating effect is good really, but decolorizing effect is bad.So the present invention has selected active carbon and aluminium oxide to decolour, but both when decolouring flow velocity very slow, and DeGrain, aluminium oxide wherein loses very big in decolouring.And decolour with macroporous weakly basic anion exchange resin D-941 pillar, decolorizing effect is best, with other three kinds compare.Following table is exactly the comparison of four kinds of decolorizing effects.
Figure 2011100938795100002DEST_PATH_IMAGE003
Through above four kinds of decoloring material evidences, last the present invention has selected macroporous weakly basic anion exchange resin D-941 to decolour, and decolorizing effect is better, and the total saponins color is white partially.
Consider to extract product and can be used for the parenteralia product, therefore should consider dispeling of magazine such as thermal source in the extraction process process, therefore knowhow adopts medicinal charcoal to carry out the processing of other impurity routinely.Medicinal charcoal through experimentation proof 4-6% decoloured 30~40 minutes in 45~55 ℃ of insulations, filtered carbon removal under this temperature, filtered carbon removal, was the best service condition of medicinal charcoal.
According to above-mentioned test, determining the present invention is optimum extraction and the characterization processes that raw material extracts Radix Notoginseng extract with bright Radix Notoginseng:
(1) getting fresh Radix Notoginseng main root or reed head is broken into the granule of coarse powder 6-10mm or is cut into the thin slice of thickness at 1-3mm, doubly measuring the circulation of 70%~95% alcohol heat reflux with 6-8 extracted 6-10 hour, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.20-0.30g crude drug/ml, mixing, precipitate 12-18 hour, centrifugal removal impurity filters;
(2) described (1) step gained filtrate is that the flow velocity of 1.0-1.4BV/H is through the D101 macroporous resin adsorption with the flow velocity, the purified water of doubly measuring with resin volume 1-4 is crossed post and is removed impurity then, flow velocity 2-4BV/h, discard water liquid, doubly measure with the speed eluting of flow velocity 2-4BV/h with the alcoholic solution 3-5 of 70-80% and to collect loss of thick fluid liquid, detect no saponin outflow to TLC till;
(3) be that 6 flow velocitys that rise to 9 liters/min are crossed the D941 resin decolorization with (2) step gained eluent with flow velocity again, after finishing on the eluent, adding resin 1-3 doubly measures the ethanol of 70-80% with identical flow velocity flushing resin column, till flowing out to the no saponin of TLC detection, merges first flow liquid and eluent;
(4) medicinal charcoal that adds crude drug weight 4-6% after (3) step filters carbon removal in 45~55 ℃ of insulation decolourings 30~40 minutes under this temperature, and concentrating under reduced pressure reclaims ethanol, being concentrated into relative density is 1.05-1.20, centrifugal, remove insoluble matter, last drying under reduced pressure.
(5) adopt high performance liquid chromatograph, carry out the method for gradient elution with acetonitrile and water as mobile phase the composition in Radix Notoginseng extract and the preparation is differentiated detection, chromatographic peak after 5 minutes, main chromatographic peak with the Radix Notoginseng total arasaponins reference extract is proofreaied and correct, and the similarity of Radix Notoginseng extract and preparation thereof is more than 0.95.The peak sequence of each composition is followed successively by: arasaponin R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd.
Further specify essentiality content of the present invention with embodiments of the invention below, but do not limit the present invention with this.
Embodiment 1:
1) get a fresh Radix Notoginseng reed 200kg, be broken into the granule of coarse powder 6-10mm, extracted 6 hours with 6 times of amount 80% alcohol heat reflux, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.20g crude drug/ml, and mixing precipitates 12 hours, and centrifugal removal impurity filters.Described filtrate is that the flow velocity of 1.2BV/H is through the D101 macroporous resin adsorption with the flow velocity, get express developed with the purified water of 1 times of amount of resin volume then, cross post and remove impurity, discard water liquid, 4 times of amounts of ethanol with 70% are collected loss of thick fluid liquid with the speed eluting of flow velocity 2BV/h, till flowing out to the no saponin of TLC detection.Be that the flow velocity of 6 liters/min is crossed the D941 resin decolorization with eluent with flow velocity again, the ethanol that add 2 times of amounts of resin 70-80% merge just flow liquid and eluent with identical flow velocity flushing resin column, detect no saponin outflow to TLC till; The medicinal charcoal that adds crude drug weight 4% then filters carbon removal in 45 ℃ of insulation decolourings 30 minutes under this temperature, concentrating under reduced pressure reclaims ethanol, is concentrated into relative density and is 1.05, and is centrifugal, removes insoluble matter, last drying under reduced pressure.Crushing packing gets Radix Notoginseng extract 16kg.
After testing, the composition of the Radix Notoginseng extract of present embodiment is:
Arasaponin R1 7.95%, the ginsenoside Rg1 31.58%, and the ginsenoside Re 4.23%, and the ginsenoside Rb1 30.77%, and the ginsenoside Rd 5.82%, R1+Rg1+Re+Rb1+Rd=80.35%, above-described each constituent content is percetage by weight.
Other Performance Detection is as follows:
1) visual inspection, this product are off-white powder.
2) this product is added water and make the solution that contains Radix Notoginseng total arasaponins 25mg among every 1ml, photograph solution colour inspection technique (" an appendix XI of Chinese pharmacopoeia A) check that compare with yellow No. 4 standard color solutions, the color that the test sample pipe presents is not deeper than control tube.
3) related substance inspection (" an appendix IX of Chinese pharmacopoeia S) all meet the requirements.
4) get test sample 0.1g, with 70% ethanol and the 2% aqueous solution of nitric acid 9ml dilution of 1ml, ultrasonic 10min, standby.Be mixed with 0,1,10 respectively with 7% ethanol and 2% nitric acid mixed solution, 100ppb complex element standard; Hg prepares with 1%HCI, 1.2ppb; 2%HNO3 and 7% alcohol mixed solution are working curve zero point.Use 1.0ug/ml Li, Se, Ge, Y, In, Tb, mark in the Bi multielement mixes adopts virtual internal standard to proofread and correct.Icp ms checks that the total amount of 18 heavy metal species such as Be, B, AI and harmful element is 0.58mg/kg. as a result
5) the macroporous adsorbent resin organic residue is checked
Measure according to residual solution algoscopy (two appendix VIIIP second methods of Chinese Pharmacopoeia version in 2010).
Chromatographic condition and system suitability test: with bonding/cross-linked polyethylene glycol is immobile phase, adopts fused-silica capillary column (30m * 0.25mm * 0.25 μ m); Flame ionization ditector, column temperature, temperature programming, initial temperature is 60 ℃, keeps 16 minutes, is warming up to 200 ℃ for 20 ℃ with per minute again, keeps 300 ℃ of detector temperatures 2 minutes; 240 ℃ of injector temperatures; Carrier gas is a nitrogen, and flow velocity is per minute 1.0ml.Headspace sampling, head space bottle equilibrium temperature is 90 ℃, equilibration time is 30 minutes.Number of theoretical plate calculates with the o-Dimethylbenzene peak should be not less than 40000, and each peak-to-peak separating degree to be measured should be up to specification.
The preparation of contrast solution: precision takes by weighing n-hexane, benzene, toluene, xylol, o-Dimethylbenzene, styrene, 1,2-diethylbenzene and divinylbenzene reference substance are an amount of, add N, N-dimethylbenzene acetamide is made the solution that contains 20 μ g, 4 μ g, 20 μ g, 20 μ g, 20 μ g, 20 μ g, 20 μ g, 20 μ g among every 1ml respectively, product storing solution in contrast.The above-mentioned storing solution 2ml of accurate absorption puts in the 50ml measuring bottle, adds 25%N, and the N-dimethylacetamide solution is diluted to scale, shakes up, and precision is measured 5ml, puts in the 20ml head space bottle, and the sealing bottleneck is obtained.
The preparation of need testing solution: get the about 0.1g of this product, the accurate title, decide, and puts in the 20ml head space bottle, the accurate 25% N,N-dimethylacetamide solution 5ml that adds, and the sealing bottleneck is obtained.
Algoscopy precision is respectively measured head space gas 1ml, injects chromatograph of liquid,, obtains with calculated by peak area by external standard method.
As a result, benzene, n-hexane, toluene, xylol, o-Dimethylbenzene, styrene, 1,2-diethylbenzene and divinylbenzene all do not detect.
Embodiment 2:
Get fresh Radix Notoginseng main root 200kg, thinly slice thickness at 1-3mm, extracted 8 hours with 7 times of amount 80% alcohol heat reflux, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.25g crude drug/ml, and mixing precipitates 15 hours, and centrifugal removal impurity filters.Described filtrate is that the flow velocity of 1.3BV/H is through the D101 macroporous resin adsorption with the flow velocity, get, cross post express developed with the purified water of 2 times of amounts of resin volume then and remove impurity, discard water liquid, 4 times of amounts of alcoholic solution with 75% are collected loss of thick fluid liquid with the speed eluting of flow velocity 3BV/h, till flowing out to the no saponin of TLC detection.Be that the flow velocity of 7.5 liters/min is crossed the D941 resin decolorization with eluent with flow velocity again, the ethanol that adds 2 times of amounts 75% of resin merges just flow liquid and eluent with identical flow velocity flushing resin column, detect no saponin outflow to TLC till; The medicinal charcoal that adds crude drug weight 5% then filters carbon removal in 50 ℃ of insulation decolourings 35 minutes under this temperature, concentrating under reduced pressure reclaims ethanol, is concentrated into relative density and is 1.1, and is centrifugal, removes insoluble matter, last drying under reduced pressure.Crushing packing gets Radix Notoginseng extract 15kg.
Adopt the method for embodiment 1 to detect, the composition of the Radix Notoginseng extract of present embodiment is:
Arasaponin R1 8.76%, the ginsenoside Rg1 34.91%, and the ginsenoside Re 4.61%, and the ginsenoside Rb1 32.23%, and the ginsenoside Rd 7.57%, R1+Rg1+Re+Rb1+Rd=88.08%, above-described each constituent content is percetage by weight.
Embodiment 3:
Get fresh Radix Notoginseng main root 200kg, thinly slice thickness at 1-3mm, extracted 10 hours with 8 times of amount 95% alcohol heat reflux, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.30g crude drug/ml, and mixing precipitates 18 hours, and centrifugal removal impurity filters.Described filtrate is that the flow velocity of 1.4BV/H is through the D101 macroporous resin adsorption with the flow velocity, cross post with the purified water of 3 times of amounts of resin volume then and remove impurity, flow velocity 4BV/h, discard water liquid, 5 times of amounts of ethanol with 80% are collected loss of thick fluid liquid with the speed eluting of flow velocity 4BV/h, till flowing out to the no saponin of TLC detection.Be that the flow velocity of 9 liters/min is crossed the D941 resin decolorization with eluent with flow velocity again, the ethanol that add 3 times of amounts of resin 70-80% merge just flow liquid and eluent with identical flow velocity flushing resin column, detect no saponin outflow to TLC till; The medicinal charcoal that adds crude drug weight 6% then filters carbon removal in 55 ℃ of insulation decolourings 40 minutes under this temperature, concentrating under reduced pressure reclaims ethanol, is concentrated into relative density and is 1.20, and is centrifugal, removes insoluble matter, last drying under reduced pressure.Crushing packing gets Radix Notoginseng extract 18kg.
Adopt the method for embodiment 1 to detect, the composition of the Radix Notoginseng extract of present embodiment is:
Arasaponin R1 8.01%, the ginsenoside Rg1 35.55%, and the ginsenoside Re 5.36%, and the ginsenoside Rb1 35.81%, and the ginsenoside Rd 8.21%, R1+Rg1+Re+Rb1+Rd=92.94%, above-described each constituent content is percetage by weight.
Embodiment 4:
Get the Radix Notoginseng extract 200g that embodiment 2 obtains, dissolve in right amount with water for injection, add the decolouring of 0.5% needle-use activated carbon, filter, add the injection water to 2000ml, transfer pH to 7.0, filter, lyophilization promptly gets lyophilized injectable powder.
Embodiment 5:
Get the Radix Notoginseng extract 100g that embodiment 2 obtains, dissolve in right amount, add the decolouring of 0.5% needle-use activated carbon, filter, add the injection water, transfer pH to 6.5, filter to 2000ml with water for injection, fill, sterilization promptly gets small-volume injection.
Embodiment 6:
Get the Radix Notoginseng extract 4g that embodiment 2 obtains,,, filter, add the chlorination sodium injection, transfer pH to 6.5, filter to 1000ml with the decolouring of 0.5% needle-use activated carbon with the dissolving of 0.9% sodium chloride injection, fill, sterilization promptly gets bulk capacity injection.
Embodiment 7:
Get the Radix Notoginseng extract 4g that embodiment 2 obtains, dissolve in right amount,, filter, add 5% glucose injection, transfer pH to 6.5, filter to 1000ml with the decolouring of 0.5% needle-use activated carbon with 5% glucose injection, fill, sterilization promptly gets bulk capacity injection.
Embodiment 8:
Get the Radix Notoginseng extract 40g that embodiment 1 obtains, it further is ground into fine powder, add Radix Notoginseng extract amount 76% starch, mixing is made granule, adds to incapsulate after Radix Notoginseng extract amount 4% cunningization powder mixes evenly, promptly gets capsule.
Embodiment 9:
The Radix Notoginseng extract 100g that treating excess syndrome example 1 obtains further is ground into fine powder with it, adds 70% dextrin, and mixing is made granule, tabletting behind the magnesium stearate mix homogeneously of adding inventory 0.5%-1% Pulvis Talci and inventory 0.2%-0.5%, and packing promptly gets tablet.

Claims (10)

1. Radix Notoginseng extract is characterized in that it contains Panax Notoginseng saponin R 14~10%, ginsenoside Rg 123~36%, ginsenoside Re 2~5%, ginsenoside Rb 127~39%, the ginsenoside Rd 3~10%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~95% of total amount.
2. Radix Notoginseng extract according to claim 1 is characterized in that it contains Panax Notoginseng saponin R 14~7%, ginsenoside Rg 123~30%, ginsenoside Re 2~3.5%, ginsenoside Rb 127~35%, the ginsenoside Rd 4~7%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~85% of total amount.
3. Radix Notoginseng extract according to claim 1 is characterized in that it contains Panax Notoginseng saponin R 17~8%, ginsenoside Rg 127~34%, ginsenoside Re 3~4%, ginsenoside Rb 133~36%, the ginsenoside Rd 6~8%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 80~90% of total amount.
4. Radix Notoginseng extract is characterized in that it contains Panax Notoginseng saponin R 14~10%, ginsenoside Rg 123~36%, ginsenoside Re 2~5%, ginsenoside Rb 127~39%, the ginsenoside Rd 3~10%, wherein Panax Notoginseng saponin R 1, the ginsenoside Rg 1, ginsenoside Re, ginsenoside Rb 1, the ginsenoside Rd accounts for 65~95% of total amount, extract and get by following method:
Adopting bright Radix Notoginseng is raw material; earlier Radix Notoginseng main root or reed head are broken into the granule of 6-10mm or are cut into the thin slice of thickness at 1-3mm; 70%~95% ethanol of doubly measuring with 6-8 extracted 6-10 hour through the hot reflux circulation; place and filter; the collection filtrate decompression concentrates, and through macroporous adsorptive resins absorption, uses the 70-80% ethanol elution then; eluent decolouring back concentrating under reduced pressure, drying.
5. the method for preparing any described Radix Notoginseng extract of claim 1-4; it is characterized in that; adopting bright Radix Notoginseng main root or Radix Notoginseng clip is raw material, earlier Radix Notoginseng main root or reed head is broken into the granule of 6-10mm or is cut into the thin slice of thickness at 1-3mm, and 70%~95% ethanol of doubly measuring with 6-8 extracted 6-10 hour through the hot reflux circulation; place and filter; the collection filtrate decompression concentrates, and through macroporous adsorptive resins absorption, uses the 70-80% ethanol elution then; eluent decolouring back concentrating under reduced pressure, drying.
6. method according to claim 4 is characterized in that, described macroporous adsorbent resin adopts the D101 macroporous resin.
7. method according to claim 4 is characterized in that, D941 resin and medicinal charcoal two-step bleaching are adopted in described decolouring.
8. according to each described method of claim 5-7, it is characterized in that described concentrated employing haplo-effect concentrator.
9. according to each described method of claim 5-7, it is characterized in that:
(1) getting fresh Radix Notoginseng main root or reed head is broken into the granule of coarse powder 6-10mm or is cut into the thin slice of thickness at 1-3mm, doubly measuring the circulation of 70%~95% alcohol heat reflux with 6-8 extracted 6-10 hour, reclaim ethanol to there not being the alcohol flavor, thin up becomes 0.20-0.30g crude drug/ml, mixing, precipitate 12-18 hour, centrifugal removal impurity filters;
(2) described (1) step gained filtrate is that the flow velocity of 1.0-1.4BV/H is through the D101 macroporous resin adsorption with the flow velocity, the purified water of doubly measuring with resin volume 1-4 is crossed post and is removed impurity then, flow velocity 2-4BV/h, discard water liquid, doubly measure with the speed eluting of flow velocity 2-4BV/h with the alcoholic solution 3-5 of 70-80% and to collect loss of thick fluid liquid, detect no saponin outflow to TLC till;
(3) be that 6 flow velocitys that rise to 9 liters/min are crossed the D941 resin decolorization with (2) step gained eluent with flow velocity again, after finishing on the eluent, adding resin 1-3 doubly measures the ethanol of 70-80% with identical flow velocity flushing resin column, till flowing out to the no saponin of TLC detection, merges first flow liquid and eluent;
(4) medicinal charcoal that adds crude drug weight 4-6% after (3) step filters carbon removal in 45~55 ℃ of insulation decolourings 30~40 minutes under this temperature, and concentrating under reduced pressure reclaims ethanol, being concentrated into relative density is 1.05-1.20, centrifugal, remove insoluble matter, last drying under reduced pressure.
10. the pharmaceutical formulation of being made by claim 1 or 2 or 3 or 4 described Radix Notoginseng extracts, described pharmaceutical formulation is injection, lyophilized injectable powder, infusion solution, capsule, granule or tablet.
CN 201110093879 2011-04-14 2011-04-14 Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract Pending CN102145034A (en)

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CN108126000B (en) * 2017-03-16 2020-10-30 楚雄云植药业有限公司 Method for extracting and preparing panax notoginseng saponins from fresh panax notoginseng

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