CN108126000A - Arasaponin extracts preparation method in fresh Radix Notoginseng - Google Patents
Arasaponin extracts preparation method in fresh Radix Notoginseng Download PDFInfo
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- CN108126000A CN108126000A CN201810009591.7A CN201810009591A CN108126000A CN 108126000 A CN108126000 A CN 108126000A CN 201810009591 A CN201810009591 A CN 201810009591A CN 108126000 A CN108126000 A CN 108126000A
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- arasaponin
- radix notoginseng
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- fresh radix
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- 241000180649 Panax notoginseng Species 0.000 title claims abstract description 65
- 235000003143 Panax notoginseng Nutrition 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000284 extract Substances 0.000 title claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 170
- 235000019441 ethanol Nutrition 0.000 claims abstract description 90
- 239000011347 resin Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000002250 absorbent Substances 0.000 claims abstract description 18
- 230000002745 absorbent Effects 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims description 54
- 239000012141 concentrate Substances 0.000 claims description 42
- 239000000047 product Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229930189092 Notoginsenoside Natural products 0.000 claims description 8
- 244000131316 Panax pseudoginseng Species 0.000 claims description 8
- 235000003181 Panax pseudoginseng Nutrition 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 229940107131 ginseng root Drugs 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229930182470 glycoside Natural products 0.000 claims description 4
- 150000002338 glycosides Chemical class 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000002002 slurry Substances 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002801 charged material Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 235000021050 feed intake Nutrition 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229930182490 saponin Natural products 0.000 description 4
- 150000007949 saponins Chemical class 0.000 description 4
- 235000017709 saponins Nutrition 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UFNDONGOJKNAES-UHFFFAOYSA-N Ginsenoside Rb1 Natural products CC(=CCCC(C)(OC1OC(COC2OC(CO)C(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CC(O)C45C)C UFNDONGOJKNAES-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000208343 Panax Species 0.000 description 1
- 235000017276 Salvia Nutrition 0.000 description 1
- 240000007164 Salvia officinalis Species 0.000 description 1
- 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 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 description 1
- TXEWRVNOAJOINC-UHFFFAOYSA-N ginsenoside Rb2 Natural products CC(=CCCC(OC1OC(COC2OCC(O)C(O)C2O)C(O)C(O)C1O)C3CCC4(C)C3C(O)CC5C6(C)CCC(OC7OC(CO)C(O)C(O)C7OC8OC(CO)C(O)C(O)C8O)C(C)(C)C6CCC45C)C TXEWRVNOAJOINC-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 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 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000036407 pain Effects 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000009692 xuesetong Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Mycology (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses arasaponins in a kind of fresh Radix Notoginseng to extract preparation method.The method of the present invention adds ethyl alcohol homogenate using fresh Radix Notoginseng as raw material, by fresh Radix Notoginseng, and filtering is concentrated into macroporous absorbent resin in no alcohol taste, refines, activated carbon decolorizing, and target product is obtained after dry.The present invention uses fresh Radix Notoginseng to be extracted for raw material, and equal slurry processes improve arasaponin yield, and cold soaking improves each component content of arasaponin, reduces the loss of Radix Notoginseng arasaponin in drying process, crushing process and high temperature reflux extraction process.Its method is easy, can be widely applied in arasaponin industrial production.
Description
Technical field
The present invention relates to a kind of extraction preparation methods of arasaponin in fresh Radix Notoginseng, belong to active components of plants extraction
Preparing technical field.
Background technology
Radix Notoginseng is Chinese tradition rare traditional Chinese medicine, is panax araliaceae plant Panax notoginseng (Burk.)
The dry root and rhizome of F.H.Chen there is hemostasis to enrich blood, the work(of the row stasis of blood of promoting blood circulation, swelling and pain relieving, bidirectional modulation blood glucose, blood fat
Effect, main product is in Yunnan Wenshan Prefecture, therefore named mountain of papers Radix Notoginseng also known as literary state Radix Notoginseng.Radix Notoginseng main component is：Arasaponin, Radix Notoginseng
Element, flavonoids, notoginseng polysaccharide, volatile oil etc..Wherein most important active ingredient be arasaponin, total saposins (PNS) content
Up to 12%, arasaponin, main component is：Ginsenoside Rb1, ginsenoside Rg1, notoginsenoside R etc..Radix Notoginseng is total
Saponin(e is widely used, main to use the drug applied to cardiovascular and cerebrovascular disease class, in health products, such as " " Xuesaitong Injection " " " composite salvia dropping
The main medicinal active ingredient of ball " is arasaponin.At present, the recovery rate of arasaponin is low in production, influence factor
For：
(1) influence of drying mode and drying temperature to content of the total saponins in radix notoginseng during fresh notoginseng drying.It is usually new
The drying mode of fresh Radix Notoginseng is dried for naturally dry and drying chamber.Naturally dry drying time is long, and drying chamber drying temperature is higher, all
The content of arasaponin can be influenced, is allowed to lose.
(2) influence of the mechanical crushing to arasaponin extract yield and content.Crude drug used in arasaponin extraction
Essentially dry medicinal material, needs to crush before feeding intake.Mechanical temperature can be increased by crushing for a long time, so as to make arasaponin ingredient
Chemical change occurs and inactivates.And Chang Yinwei crushing is inhomogenous in producing, and the drug-eluting rate for causing partial particulate big is low, and
Affect the yield and content of arasaponin.
(3) influence of the extracting method to arasaponin extract yield and content.
The method that existing arasaponin extraction uses mainly has：Decocting cooking method, Alcohol refluxing method, percolation, ultrasonic extraction
Deng.And more common method is Alcohol refluxing method in producing, methods and techniques are with more mature, but recovery rate is not high, former
Because：A. Radix Notoginseng contains much starch, is easily gelatinized in hot water and ethanol system, causes impurity content high, is purified to later separation
It brings tired, also easily leads to content of the total saponins in radix notoginseng or purity is relatively low；B. the consumption of alcohol reflux Extraction solvent is big, and extraction time is more, adds
The thermal concentration time is long, and arasaponin is easy to inactivate as heat-sensitive materials, and causes yield and content low.
Invention content
In view of the deficiencies of the prior art, the present invention provides arasaponin extraction preparation method in a kind of fresh Radix Notoginseng, uses
With solve the problem of arasaponin easily inactivate, the high arasaponin purity of impurity content it is low.
The technical solution adopted by the present invention is as follows：
1. arasaponin extracts preparation method in fresh Radix Notoginseng, it is characterised in that includes the following steps：
(1) add 8-10 times to measure 75% ethyl alcohol homogenate fresh Radix Notoginseng, 12-24h is stood after homogenate, filter to get filtrate I, filter residue
Add 5-8 times times of 75% ethyl alcohol homogenate of amount, 12-24h is stood after homogenate, filter to get filtrate II, merging filtrate I and filtrate II filter
It is clarified to filtrate；
(2) filtrate≤60 DEG C are concentrated into no alcohol taste under -0.08Mpa and obtain concentrate；
(3) add 5-8 times to measure water dilution upper macroporous absorbent resin concentrate, 5-8 times of inventory is added to measure water, is washed, then is added
It measures ethyl alcohol for 6-8 times and rushes glycosides, ethanol eluate is concentrated into no alcohol taste after crossing decolorizing resin, adds 2-3 times of amount of alcohol of concentrate, adds and feed intake
3%-6% activated carbons are measured, reflux 15-30min decolorations filter, are concentrated into medicinal extract proportion as 1.13-1.20, obtain target product；
(4) target product≤60 DEG C are dried in vacuo to obtain arasaponin.
2. arasaponin extracts preparation method in fresh Radix Notoginseng as described in technical solution 1, it is characterised in that：Step
(3) arasaponin described in is more than 88.0%, and yield is higher than 3.5%.
3. arasaponin extracts preparation method in fresh Radix Notoginseng as described in technical solution 1, it is characterised in that：Macropore is inhaled
Attached resin is D101 or AB-8 macroporous absorbent resins.
4. arasaponin extracts preparation method in fresh Radix Notoginseng as described in technical solution 1, it is characterised in that：Step
(3) concentration of alcohol is 70%-85%v/v in the ethanol eluate described in.
5. arasaponin extracts preparation method in a kind of fresh Radix Notoginseng as described in technical solution 1, it is characterised in that：Step
Suddenly the activated carbon decolorizing concentration of alcohol described in (3) is 95% ethyl alcohol v/v.
6. arasaponin extracts preparation method in a kind of fresh Radix Notoginseng, it is characterised in that includes the following steps：
(1) the 75%v/v ethyl alcohol homogenates of fresh 8-10 times of three seven weight are added in fresh Radix Notoginseng, 12- is stood after homogenate
For 24 hours, it filters to get filtrate I, the 75%v/v ethyl alcohol homogenates of 5-8 times of filter residue weight is added in filter residue, 12-24h, mistake are stood after homogenate
Filtrate II, merging filtrate I and filtrate II are filtered to obtain, filters to filtrate and clarifies to obtain filtrate III；
(2) filtrate III is concentrated into no alcohol taste under temperature≤60 DEG C and 0.08Mpa and obtains concentrate I；
(3) the upper macroporous absorbent resin of water dilution of 5-8 times of I weight of concentrate is added in concentrate I, adds fresh three seven weight
5-8 times of water, washing, then the 70%-85%v/v ethyl alcohol of fresh 6-8 times of three seven weight is added to rinse to obtain ethanol eluate, ethyl alcohol is washed
De- liquid, which is crossed after decolorizing resin, to be concentrated into no alcohol taste and obtains concentrate II, and 2-3 times of II weight of concentrate is added in concentrate II
95% ethyl alcohol v/v ethyl alcohol, adds in fresh three seven weights 3%-6% activated carbons, and reflux 15-30min decolorations filter, are concentrated into leaching
Cream proportion is 1.13-1.20, obtains target product；
(4) target product is dried in vacuo to obtain arasaponin in temperature≤60 DEG C.
7. arasaponin extracts preparation method in a kind of fresh Radix Notoginseng according to claim 6, it is characterised in that：
Step (3) macroporous absorbent resin is D101 macroporous absorbent resins or AB-8 macroporous absorbent resins.
8. arasaponin extraction system in a kind of fresh Radix Notoginseng according to any claim in claim 6 to 8
Preparation Method, it is characterised in that：Before the fresh Radix Notoginseng extraction notoginsenoside, 75%v/v ethyl alcohol will be used to soak after fresh pseudo-ginseng root slices
It is not sealed.
It during present invention elution, is first washed with water, then with the purpose that alcohol is washed is that washing can remove water-soluble substances such as polysaccharide, then
Arasaponin is eluted with alcohol to achieve the purpose that isolate and purify；Since return time is shorter during except color, will not destroy effectively into
Point.
The present invention using fresh Radix Notoginseng as extraction arasaponin raw material, fresh Radix Notoginseng as raw material avoid because of
Drying process, crushing process and component damages caused by refluxing extraction process, energy Enough remain arasaponin to greatest extent
Total component content.Those skilled in the art do not use fresh Radix Notoginseng generally as extraction raw material, in addition to being limited by the place of production, time
System, is also influenced, fresh Radix Notoginseng is not easy to store, and needs the fresh-keeping preservation of freezer by condition of storage；The present invention stores new for convenience
Fresh Radix Notoginseng can will be sealed after fresh pseudo-ginseng root slices with the submergence of 75% ethyl alcohol.
The present invention adds in ethyl alcohol homogenate under room temperature or low temperature in fresh Radix Notoginseng, will not be because of temperature height, content of starch
The reasons such as height cause the ingredient inactivation of notoginsenoside or gelatinization to cause the content of notoginsenoside too low.
Compared with prior art, the present invention also has the advantages that：The present invention directly adds ethyl alcohol equal with fresh Radix Notoginseng
Slurry extraction arasaponin, reduces Radix Notoginseng arasaponin in drying process, crushing process and high temperature reflux extraction process
Loss, by measuring arasaponin total content ＞ 90.0%, each component content contains not less than National Pharmacopeia regulation injection
Amount.
Specific embodiment
Technical scheme of the present invention is described in further details with reference to specific embodiment, but following embodiment is not
It is limitation of the invention.
Embodiment 1
Using fresh Radix Notoginseng to feed intake, the 75%v/v ethyl alcohol that fresh three seven weights, 10 times of weight are added in fresh Radix Notoginseng is equal
Slurry is stood for 24 hours after homogenate, filters to get filtrate I, and the 75%v/v ethyl alcohol homogenates of filter residue 8 times of weight of weight, homogenate are added in filter residue
After stand for 24 hours, filter to get filtrate II, merging filtrate I and filtrate II filter to filtrate and clarifies to obtain filtrate III；By filtrate III in temperature
It is concentrated into no alcohol taste under≤60 DEG C of degree and 0.08Mpa and obtains concentrate I；Concentrate I weight, 8 times of weight amounts are added in concentrate I
The upper D101 macroporous absorbent resins of water dilution, add fresh three seven weights, 8 times of weight waters (i.e. plus water of 8 times of weight of charged material weight),
Washing, then the 75%v/v ethyl alcohol of fresh three seven weights, 8 times of weight is added to rush glycosides and obtains ethanol eluate, ethanol eluate crosses decoloration tree
No alcohol taste is concentrated into after fat and obtains concentrate II, the 95%v/v ethyl alcohol of concentrate II weight, 3 times of weight is added in concentrate II, is added
Fresh three seven weight (i.e. charged material weight), 6% activated carbon, reflux 30min decolorations, filters, it is 1.20 to be concentrated into medicinal extract proportion, is obtained
Target product；Target product is dried in vacuo to obtain arasaponin in temperature≤60 DEG C.Arasaponin total content content is
89.8%, each component content provides injection content not less than National Pharmacopeia.
Embodiment 2
Using fresh Radix Notoginseng to feed intake, the 75%v/v ethyl alcohol that fresh three seven weights, 8 times of weight are added in fresh Radix Notoginseng is equal
Slurry is stood for 24 hours after homogenate, filters to get filtrate I, and the 75%v/v ethyl alcohol homogenates of filter residue 6 times of weight of weight, homogenate are added in filter residue
After stand for 24 hours, filter to get filtrate II, merging filtrate I and filtrate II filter to filtrate and clarifies to obtain filtrate III；By filtrate III in temperature
It is concentrated into no alcohol taste under≤60 DEG C of degree and 0.08Mpa and obtains concentrate I；Concentrate I is added in the water of I 6 times of weight of weight of concentrate
AB-8 macroporous absorbent resins in dilution add the water of 6 times of weight of charged material weight, washing, then add the 85%v/ of 6 times of weight of charged material weight
V ethyl alcohol rushes glycosides and obtains ethanol eluate, and ethanol eluate, which is crossed after decolorizing resin, to be concentrated into no alcohol taste and obtain concentrate II, in concentrate II
Concentrate II weight, 3 times of weight 95%v/v ethyl alcohol are added in, add 4% activated carbon of charged material weight, reflux 30min decolorations filter, dense
It is 1.16 to be reduced to medicinal extract proportion, obtains target product；Target product is dried in vacuo to obtain arasaponin in temperature≤60 DEG C.Radix Notoginseng
Total saposins total content is 89.4%, and each component content provides injection content not less than National Pharmacopeia.
Embodiment 3
Using fresh Radix Notoginseng to feed intake, the 75%v/v ethyl alcohol that fresh three seven weights, 8 times of weight are added in fresh Radix Notoginseng is equal
Slurry stands 12h after homogenate, filters to get filtrate I, and the 75%v/v ethyl alcohol homogenates of filter residue 5 times of weight of weight, homogenate are added in filter residue
After stand 12h, filter to get filtrate II, merging filtrate I and filtrate II filter to filtrate and clarifies to obtain filtrate III；By filtrate III in temperature
It is concentrated into no alcohol taste under≤60 DEG C of degree and 0.08Mpa and obtains concentrate I；Concentrate I is added in the water of I 5 times of weight of weight of concentrate
D101 macroporous absorbent resins in dilution add the water of 5 times of weight of charged material weight, washing, then add the 80%v/v of 6 times of amounts of charged material weight
Ethyl alcohol rinses to obtain ethanol eluate, and ethanol eluate, which is crossed after decolorizing resin, to be concentrated into no alcohol taste and obtain concentrate II, in concentrate II
The 95%v/v ethyl alcohol of concentrate II weight, 3 times of weight is added in, adds 3% activated carbon of charged material weight, reflux 20min decolorations filter,
It is 1.13 to be concentrated into medicinal extract proportion, obtains target product；Target product is dried in vacuo to obtain arasaponin in temperature≤60 DEG C.Three
Seven total saposins total contents are 89.6%, and each component content provides injection content not less than National Pharmacopeia.
Embodiment 4
Using fresh Radix Notoginseng as raw material, the 75%v/v of fresh three seven weights, 10 times of weight is added in fresh Radix Notoginseng 10.0kg
Ethyl alcohol homogenate is stood for 24 hours after homogenate, filters to get filtrate I, and the 75%v/v ethyl alcohol that filter residue 8 times of weight of weight are added in filter residue is equal
Slurry is stood for 24 hours after homogenate, filters to get filtrate II, and merging filtrate I and filtrate II filter to filtrate and clarifies to obtain filtrate III；By filtrate
III is concentrated into no alcohol taste under temperature≤60 DEG C and 0.08Mpa obtains concentrate I；8 times of I weight of concentrate is added in concentrate I
The upper D101 macroporous absorbent resins of water dilution or AB-8 macroporous absorbent resins of weight add the water of fresh three seven weights, 8 times of weight, water
It washes, then the 80%v/v ethyl alcohol of fresh three seven weights, 8 times of weight is added to rinse to obtain ethanol eluate, ethanol eluate crosses decolorizing resin
After be concentrated into no alcohol taste and obtain concentrate II, the 95%v/v ethyl alcohol of concentrate II weight, 3 times of weight is added in concentrate II, is added
Enter fresh three seven weights, 6% activated carbon, reflux 30min decolorations filter, it is 1.20 to be concentrated into medicinal extract proportion, obtains target product；It will
Target product is dried in vacuo to obtain arasaponin 355.7g in temperature≤60 DEG C.Arasaponin total content be 90.8%, respectively into
Content is divided to provide injection content not less than National Pharmacopeia.
Comparative example 1
(1) fresh pseudo-ginseng 10.0kg is taken, is cleaned, is dried, air-dries or dry；(2) by pseudo-ginseng root slices, 75%v/v is used
Ethanol solution thermal extraction, extracting solution recycling ethyl alcohol, the aqueous solution for adding in pseudo-ginseng root slices 6 times of weight of weight are diluted to without apparent oiliness
Material floats, filtering, obtain clear aqueous solution；(3) by D101 large pore resin absorption columns on the clear aqueous solution of step 2, then
It is washed 1 time with the aqueous solution of pH=4~6, is then eluted with the ethanol solution of 40~80v%；(4) eluent is collected, recycles second
Alcohol, is concentrated under reduced pressure into dry, obtains white powder product notoginsenoside 256.5g.
Comparative example 2
Comparative example 2 is cleaned except fresh pseudo-ginseng 10.0kg is taken, dries, air-dries or dry, with the Radix Notoginseng for air-drying or drying
It is sliced outside for raw material, remaining operating procedure is same as Example 4.Obtain white powder product notoginsenoside 277.0g.
It is as shown in table 1 to compare each content results of arasaponin that comparative example and embodiment 4 obtain.
The comparison result of 1 comparative example of table and embodiment 4
As shown in Table 1, the arasaponin product weight and content of the total saponins in radix notoginseng that embodiment 4 obtains are above comparing
Example, 1 arasaponin of comparative example is easy to inactivate as heat-sensitive materials using thermal extraction method, and cause yield and content compared with
It is low, it is easily gelatinized in hot water and ethanol system, leads to impurity content height.Comparative example 2 is air-dried or is dried using fresh Radix Notoginseng
Pseudo-ginseng root slices extraction notoginsenoside, extracting method is same as Example 4, but is fresh Radix Notoginseng in embodiment 4 as raw material
Avoid because of drying process, crushing process and component damages caused by refluxing extraction process, thus 4 yield of embodiment and it is each effectively
Component content is higher than comparative example 2, also above comparative example 1.
Claims (8)
1. arasaponin extracts preparation method in fresh Radix Notoginseng, it is characterised in that includes the following steps：
(1) add 8-10 times to measure 75% ethyl alcohol homogenate fresh Radix Notoginseng, 12-24h is stood after homogenate, filter to get filtrate 1, filter residue adds 5-
8 times times of 75% ethyl alcohol homogenates of amount stand 12-24h after homogenate, filter to get filtrate 2, and merging filtrate 1 and filtrate 2 are filtered to filtrate
Clarification；
(2) filtrate≤60 DEG C are concentrated into no alcohol taste under -0.08Mpa and obtain concentrate；
(3) add 5-8 times to measure water dilution upper macroporous absorbent resin concentrate, 5-8 times of inventory is added to measure water, is washed, then adds 6-8 times
Amount ethyl alcohol rushes glycosides, and ethanol eluate is concentrated into no alcohol taste after crossing decolorizing resin, adds 2-3 times of amount of alcohol of concentrate, adds inventory
3%-6% activated carbons, reflux 15-30min decolorations, filter, and are concentrated into medicinal extract proportion as 1.13-1.20, obtain target product；
(4) target product≤60 DEG C are dried in vacuo to obtain arasaponin.
2. arasaponin extraction preparation method in fresh Radix Notoginseng as described in claim 1, it is characterised in that：In step (3)
The arasaponin is more than 88.0%, and yield is higher than 3.5%.
3. arasaponin extraction preparation method in fresh Radix Notoginseng as described in claim 1, it is characterised in that：Macroporous absorption tree
Fat is D101 or AB-8 macroporous absorbent resins.
4. arasaponin extraction preparation method in fresh Radix Notoginseng as described in claim 1, it is characterised in that：In step (3)
Concentration of alcohol is 70%-85%v/v in the ethanol eluate.
5. arasaponin extraction preparation method in a kind of fresh Radix Notoginseng as described in claim 1, it is characterised in that：Step
(3) the activated carbon decolorizing concentration of alcohol described in is 95% ethyl alcohol v/v.
6. arasaponin extracts preparation method in a kind of fresh Radix Notoginseng, it is characterised in that includes the following steps：
(1) the 75%v/v ethyl alcohol homogenates of fresh 8-10 times of three seven weight are added in fresh Radix Notoginseng, 12-24h is stood after homogenate,
It filters to get filtrate I, the 75%v/v ethyl alcohol homogenates of 5-8 times of filter residue weight is added in filter residue, 12-24h is stood after homogenate, filters
Filtrate II, merging filtrate I and filtrate II filter to filtrate and clarify to obtain filtrate III；
(2) filtrate III is concentrated into no alcohol taste under temperature≤60 DEG C and 0.08Mpa and obtains concentrate I；
(3) the upper macroporous absorbent resin of water dilution of 5-8 times of I weight of concentrate is added in concentrate I, adds fresh three seven weights 5-8
Water again, washing, then the 70%-85%v/v ethyl alcohol of fresh 6-8 times of three seven weight is added to rinse to obtain ethanol eluate, ethanol elution
Liquid, which is crossed after decolorizing resin, to be concentrated into no alcohol taste and obtains concentrate II, and the 95% of 2-3 times of II weight of concentrate is added in concentrate II
Ethyl alcohol v/v ethyl alcohol, adds in fresh three seven weights 3%-6% activated carbons, and reflux 15-30min decolorations filter, are concentrated into medicinal extract ratio
Weight is 1.13-1.20, obtains target product；
(4) target product is dried in vacuo to obtain arasaponin in temperature≤60 DEG C.
7. arasaponin extracts preparation method in a kind of fresh Radix Notoginseng according to claim 6, it is characterised in that：Step
(3) macroporous absorbent resin is D101 macroporous absorbent resins or AB-8 macroporous absorbent resins.
8. arasaponin extracts preparation side in a kind of fresh Radix Notoginseng according to any claim in claim 6 to 8
Method, it is characterised in that：It is close by 75%v/v ethyl alcohol is used to submerge after fresh pseudo-ginseng root slices before the fresh Radix Notoginseng extraction notoginsenoside
Envelope preserves.
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| CN111096990A (en) * | 2020-02-19 | 2020-05-05 | 昆明邦宇制药有限公司 | Method for extracting panax notoginseng saponins from fresh panax notoginseng |
| CN113116949A (en) * | 2020-01-15 | 2021-07-16 | 四川森科制药有限公司 | Extraction process of panax notoginseng saponins |
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| CN102145034A (en) * | 2011-04-14 | 2011-08-10 | 云南文山七丹药业股份有限公司 | Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract |
| CN103565866A (en) * | 2012-07-30 | 2014-02-12 | 昆明制药集团股份有限公司 | Preparation method of panax notoginseng saponins |
| CN104490967A (en) * | 2014-12-06 | 2015-04-08 | 云南云药医药研究有限公司 | High-efficiency high-yield preparation method of panax notoginseng extract |
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| CN102145034A (en) * | 2011-04-14 | 2011-08-10 | 云南文山七丹药业股份有限公司 | Fresh radix notoginseng extract, preparation method and medicinal prescription of fresh radix notoginseng extract |
| CN103565866A (en) * | 2012-07-30 | 2014-02-12 | 昆明制药集团股份有限公司 | Preparation method of panax notoginseng saponins |
| CN104490967A (en) * | 2014-12-06 | 2015-04-08 | 云南云药医药研究有限公司 | High-efficiency high-yield preparation method of panax notoginseng extract |
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| CN113116949A (en) * | 2020-01-15 | 2021-07-16 | 四川森科制药有限公司 | Extraction process of panax notoginseng saponins |
| CN111096990A (en) * | 2020-02-19 | 2020-05-05 | 昆明邦宇制药有限公司 | Method for extracting panax notoginseng saponins from fresh panax notoginseng |
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