patents.google.com

CN107693559A - The preparation method of Notogineng Extract - Google Patents

️Fri Feb 16 2018

CN107693559A - The preparation method of Notogineng Extract - Google Patents

The preparation method of Notogineng Extract Download PDF

Info

Publication number

CN107693559A

CN107693559A CN201711209777.9A CN201711209777A CN107693559A CN 107693559 A CN107693559 A CN 107693559A CN 201711209777 A CN201711209777 A CN 201711209777A CN 107693559 A CN107693559 A CN 107693559A Authority

China

Prior art keywords

extract

preparation

pseudo

ginseng

notogineng

Prior art date

2017-11-27

Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)

Pending

Application number

CN201711209777.9A

Other languages

Chinese (zh)

Inventor

葛玲玲

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

HAOCHENG PHARMACEUTICAL CO Ltd GUAIZHOU

Original Assignee

HAOCHENG PHARMACEUTICAL CO Ltd GUAIZHOU

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

2017-11-27

Filing date

2017-11-27

Publication date

2018-02-16

2017-11-27 Application filed by HAOCHENG PHARMACEUTICAL CO Ltd GUAIZHOU filed Critical HAOCHENG PHARMACEUTICAL CO Ltd GUAIZHOU

2017-11-27 Priority to CN201711209777.9A priority Critical patent/CN107693559A/en

2018-02-16 Publication of CN107693559A publication Critical patent/CN107693559A/en

Status Pending legal-status Critical Current

Links

239000000284 extract Substances 0.000 title claims abstract description 66
238000002360 preparation method Methods 0.000 title claims abstract description 33
KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 45
244000131316 Panax pseudoginseng Species 0.000 claims abstract description 41
235000003181 Panax pseudoginseng Nutrition 0.000 claims abstract description 40
238000000605 extraction Methods 0.000 claims abstract description 30
XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
239000011347 resin Substances 0.000 claims abstract description 16
229920005989 resin Polymers 0.000 claims abstract description 16
238000002425 crystallisation Methods 0.000 claims abstract description 14
230000008025 crystallization Effects 0.000 claims abstract description 14
XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 45
238000010438 heat treatment Methods 0.000 claims description 22
239000012141 concentrate Substances 0.000 claims description 21
239000000706 filtrate Substances 0.000 claims description 21
LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
239000013078 crystal Substances 0.000 claims description 16
239000003480 eluent Substances 0.000 claims description 12
241000180649 Panax notoginseng Species 0.000 claims description 10
235000003143 Panax notoginseng Nutrition 0.000 claims description 10
239000000287 crude extract Substances 0.000 claims description 9
239000012044 organic layer Substances 0.000 claims description 9
239000000843 powder Substances 0.000 claims description 9
229930182490 saponin Natural products 0.000 claims description 9
150000007949 saponins Chemical class 0.000 claims description 9
235000017709 saponins Nutrition 0.000 claims description 9
238000001816 cooling Methods 0.000 claims description 6
238000001914 filtration Methods 0.000 claims description 6
239000010410 layer Substances 0.000 claims description 6
238000010828 elution Methods 0.000 claims description 5
238000001704 evaporation Methods 0.000 claims description 3
230000008020 evaporation Effects 0.000 claims description 3
239000004744 fabric Substances 0.000 claims description 3
239000007788 liquid Substances 0.000 claims description 2
239000012265 solid product Substances 0.000 claims description 2
238000003810 ethyl acetate extraction Methods 0.000 claims 1
238000001694 spray drying Methods 0.000 claims 1
238000004519 manufacturing process Methods 0.000 abstract description 8
238000000034 method Methods 0.000 abstract description 7
239000002904 solvent Substances 0.000 abstract description 5
241000411851 herbal medicine Species 0.000 abstract description 3
238000001179 sorption measurement Methods 0.000 abstract description 3
238000002386 leaching Methods 0.000 abstract description 2
238000011017 operating method Methods 0.000 abstract description 2
230000008569 process Effects 0.000 abstract description 2
239000003223 protective agent Substances 0.000 abstract description 2
239000008346 aqueous phase Substances 0.000 description 7
239000012074 organic phase Substances 0.000 description 7
238000003756 stirring Methods 0.000 description 6
239000003643 water by type Substances 0.000 description 6
241000208340 Araliaceae Species 0.000 description 5
239000008280 blood Substances 0.000 description 5
210000004369 blood Anatomy 0.000 description 5
235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 4
235000003140 Panax quinquefolius Nutrition 0.000 description 4
230000000052 comparative effect Effects 0.000 description 4
239000003814 drug Substances 0.000 description 4
230000000694 effects Effects 0.000 description 4
239000007789 gas Substances 0.000 description 4
235000008434 ginseng Nutrition 0.000 description 4
239000000047 product Substances 0.000 description 4
239000004480 active ingredient Substances 0.000 description 3
239000003463 adsorbent Substances 0.000 description 3
230000017531 blood circulation Effects 0.000 description 3
238000001035 drying Methods 0.000 description 3
238000011010 flushing procedure Methods 0.000 description 3
239000012452 mother liquor Substances 0.000 description 3
QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
230000008719 thickening Effects 0.000 description 3
IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
235000005979 Citrus limon Nutrition 0.000 description 2
244000131522 Citrus pyriformis Species 0.000 description 2
208000032843 Hemorrhage Diseases 0.000 description 2
239000002253 acid Substances 0.000 description 2
230000000740 bleeding effect Effects 0.000 description 2
230000003727 cerebral blood flow Effects 0.000 description 2
238000005516 engineering process Methods 0.000 description 2
230000001737 promoting effect Effects 0.000 description 2
230000001681 protective effect Effects 0.000 description 2
239000008213 purified water Substances 0.000 description 2
239000002893 slag Substances 0.000 description 2
238000005507 spraying Methods 0.000 description 2
FBFMBWCLBGQEBU-GYMUUCMZSA-N 20-gluco-ginsenoside-Rf Natural products O([C@](CC/C=C(\C)/C)(C)[C@@H]1[C@H]2[C@H](O)C[C@H]3[C@](C)([C@]2(C)CC1)C[C@H](O[C@@H]1[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O2)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1C(C)(C)[C@@H](O)CC[C@]31C)[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 FBFMBWCLBGQEBU-GYMUUCMZSA-N 0.000 description 1
244000025254 Cannabis sativa Species 0.000 description 1
206010011224 Cough Diseases 0.000 description 1
LLPWNQMSUYAGQI-QBQUQATFSA-N Ginsenoside R1 Natural products O([C@](CC/C=C(\C)/C)(C)[C@@H]1[C@H]2[C@@H](O)C[C@H]3[C@](C)([C@]2(C)CC1)C[C@H](O[C@@H]1[C@H](O[C@@H]2[C@@H](O)[C@@H](O)[C@@H](O)CO2)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1C(C)(C)[C@@H](O)CC[C@]31C)[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O1 LLPWNQMSUYAGQI-QBQUQATFSA-N 0.000 description 1
208000031354 Hyphema Diseases 0.000 description 1
229930189092 Notoginsenoside Natural products 0.000 description 1
241000208343 Panax Species 0.000 description 1
208000007536 Thrombosis Diseases 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
206010046788 Uterine haemorrhage Diseases 0.000 description 1
210000001015 abdomen Anatomy 0.000 description 1
239000013543 active substance Substances 0.000 description 1
230000003321 amplification Effects 0.000 description 1
230000009286 beneficial effect Effects 0.000 description 1
150000001875 compounds Chemical class 0.000 description 1
201000010099 disease Diseases 0.000 description 1
208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
229940079593 drug Drugs 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
229930182470 glycoside Natural products 0.000 description 1
150000002338 glycosides Chemical class 0.000 description 1
208000035861 hematochezia Diseases 0.000 description 1
230000023597 hemostasis Effects 0.000 description 1
239000011261 inert gas Substances 0.000 description 1
238000011031 large-scale manufacturing process Methods 0.000 description 1
239000002075 main ingredient Substances 0.000 description 1
239000002398 materia medica Substances 0.000 description 1
230000007721 medicinal effect Effects 0.000 description 1
238000012986 modification Methods 0.000 description 1
230000004048 modification Effects 0.000 description 1
229910052757 nitrogen Inorganic materials 0.000 description 1
LLPWNQMSUYAGQI-UHFFFAOYSA-N notoginsenoside r1 Chemical compound C1CC(C2(CC(C3C(C)(C)C(O)CCC3(C)C2CC2O)OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)CO3)O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O LLPWNQMSUYAGQI-UHFFFAOYSA-N 0.000 description 1
238000003199 nucleic acid amplification method Methods 0.000 description 1
206010033675 panniculitis Diseases 0.000 description 1
238000000746 purification Methods 0.000 description 1
239000001397 quillaja saponaria molina bark Substances 0.000 description 1
239000002994 raw material Substances 0.000 description 1
238000011084 recovery Methods 0.000 description 1
238000011160 research Methods 0.000 description 1
210000001525 retina Anatomy 0.000 description 1
210000000697 sensory organ Anatomy 0.000 description 1
238000000926 separation method Methods 0.000 description 1
238000002791 soaking Methods 0.000 description 1
239000000344 soap Substances 0.000 description 1
208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
238000013517 stratification Methods 0.000 description 1
210000004304 subcutaneous tissue Anatomy 0.000 description 1
238000006467 substitution reaction Methods 0.000 description 1
239000013589 supplement Substances 0.000 description 1
230000008961 swelling Effects 0.000 description 1
238000012360 testing method Methods 0.000 description 1
210000003462 vein Anatomy 0.000 description 1
239000009306 yunnan baiyao 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
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/12—Carboxylic acids; Salts or anhydrides thereof
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
- 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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
- 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

Landscapes

Health & Medical Sciences (AREA)
Natural Medicines & Medicinal Plants (AREA)
Chemical & Material Sciences (AREA)
Life Sciences & Earth Sciences (AREA)
Animal Behavior & Ethology (AREA)
Public Health (AREA)
Medicinal Chemistry (AREA)
Pharmacology & Pharmacy (AREA)
Epidemiology (AREA)
Engineering & Computer Science (AREA)
Veterinary Medicine (AREA)
General Health & Medical Sciences (AREA)
General Chemical & Material Sciences (AREA)
Chemical Kinetics & Catalysis (AREA)
Oil, Petroleum & Natural Gas (AREA)
Alternative & Traditional Medicine (AREA)
Biotechnology (AREA)
Botany (AREA)
Medical Informatics (AREA)
Microbiology (AREA)
Mycology (AREA)
Medicines Containing Plant Substances (AREA)

Abstract

The invention provides a kind of preparation method of Notogineng Extract; it is related to Chinese herbal medicine extractive technique field; in the preparation method of Notogineng Extract provided by the invention; pseudo-ginseng is extracted using water as solvent; and protective agent citric acid is added in leaching process, so as to reduce the probability that arasaponin is oxidized in extraction process；Meanwhile extracted by using the mode of secondary extraction, extraction operating procedure can not only be simplified, additionally it is possible to reduce the consumption for solvent, save the production time and reduce production cost.In addition, the present invention is separated and purified to arasaponin using steps such as resin adsorption and extractive crystallizations, it is not only easy to operate, and separative efficiency is high, cost is low, the cycle is short, while the purity of product arasaponin is also higher, suitable for industrialized production and popularization.

Description

The preparation method of Notogineng Extract

Technical field

The present invention relates to Chinese herbal medicine extractive technique field, more particularly, to a kind of preparation method of Notogineng Extract.

Background technology

Pseudo-ginseng also known as pseudo-ginseng, it is Umbellales Araliaceae, is distributed mainly on the ground such as Yunnan, Guangxi, Jiangxi, Sichuan.Together Name Chinese medicine pseudo-ginseng is using the root of plant pseudo-ginseng as medicinal effects, has the effect of dissipate stasis of blood hemostasis, detumescence ding-tong.Cure mainly and cough up Blood, spit blood, bleeding from five sense organs or subcutaneous tissue, have blood in stool, uterine bleeding, traumatism and bleeding, chest and abdomen shouting pain, fall servant's swelling and pain.Just it is acknowledged as having significantly since ancient times Promoting blood circulation and removing blood stasis, detumescence ding-tong effect, there is " invaluable ", the good reputation in " southern part of the country god grass ".Because pseudo-ginseng is all panax species, And its effective active matter is higher than and more than ginseng, therefore " king in ginseng " is referred to as by modern Chinese herbal medicine medicine scholar again.Clearly Work towards pharmacy《A Supplement to the Compendium of Materia Medica》Described in：" ginseng qi-tonifying first, pseudo-ginseng enrich blood first, taste with and work(also etc., therefore claim people Radix notoginseng, it is the most precious person in Chinese medicine." China and foreign countries of becoming famous Chinese patent drug " Yunnan Baiyao " and " Pien Tze Huang ", i.e., based on pseudo-ginseng Raw material is wanted to be made.

Modern Pharmaceutics research shows that the main active substances in pseudo-ginseng are that (its Main Ingredients and Appearance is arasaponin：Ginseng Saponin(e Rb1, ginsenoside Rg1, ginsenoside R1), promoting blood circulation is cured mainly, is promoted blood circulation active, has and suppresses platelet aggregation and increasing Add the effect of cerebral blood flow (CBF), it is more to can be widely applied to cerebrovascular sequelae, thrombosis of central vein of retina, hyphema etc. Kind disease.It is organic in extraction process but existing notoginsenoside extracting method mainly the methods of passing through alcohol extracting is extracted Solvent consumption is larger, and has that extraction process is complicated, efficiency is low, cost is high, can not large-scale production the shortcomings of.Therefore, study The Novel purification method of arasaponin has important practical significance.

In view of this, it is special to propose the present invention.

The content of the invention

The first object of the present invention is to provide a kind of preparation method of Notogineng Extract, the system of Notogineng Extract of the present invention Content of the total saponins in radix notoginseng >=80% of Notogineng Extract made from Preparation Method, while preparation method of the present invention also has operation letter Just the advantages of, separative efficiency is high, and with short production cycle and cost is low.

A kind of preparation method of Notogineng Extract provided by the invention, the preparation method comprise the following steps：

(a) after pseudo-ginseng being ground into 100~200 mesh fine powders, add water and citric acid to heat extraction, filtering, collect respectively Filter residue and filtrate, filter residue add water and citric acid to heat extraction, are filtrated to get filtrate, secondary filtrate is merged, obtains pseudo-ginseng again Extract solution；

(b) pseudo-ginseng extract solution is adsorbed with resin, then by elution, concentration, obtains concentrate；

(c) concentrate adds ethyl acetate to extract, then collected organic layer and water layer respectively；Water layer adds ethyl acetate again Extraction, collected organic layer；Then the organic layer collected twice is merged, obtains extract；Then, extract is concentrated and dried, Obtain pseudo-ginseng crude extract；

(d) by pseudo-ginseng crude extract add water dissolve by heating after cooling crystallization, obtain crystal；

(e) under the conditions of gas shield, crystal is dried, then crush be fine powder, that is, obtain content of the total saponins in radix notoginseng >= 80% Notogineng Extract.

Further, in step (a), the dosage of citric acid by addition water quality 2%~3%.

Further, in step (b), the resin is AB-8, LX-8, LX-16, or HPD826 resins.

Further, in step (b), the eluent of the elution is ethanol.

Further, in step (b), the concentration is heating concentration.

Further, the temperature of the heating concentration is 60~70 DEG C.

Further, in step (c), the volumetric usage of ethyl acetate is 3~5 times of the volume of concentrate.

Further, in step (c), the extract, which is concentrated and dried, is：Extract heating evaporation is concentrated, consolidated to gained Body product is dried；

Or the extract is concentrated and dried and is：First extract is concentrated, it is then that gained extraction concentrate spraying is dry It is dry.

Further, in step (d), the temperature of the heating is 70~80 DEG C.

Preferably, the temperature of the cooling crystallization is 4~6 DEG C, and the time is 36~48h.

Further, in step (e), the aperture of screen cloth is 30~70 mesh.

Compared with prior art, beneficial effects of the present invention are：

In the preparation method of Notogineng Extract provided by the invention, pseudo-ginseng is extracted using water as solvent, and is soaking Protective agent citric acid is added during carrying, so as to reduce the probability that arasaponin is oxidized in extraction process；Meanwhile Extracted by using the mode of secondary extraction, extraction operating procedure can not only be simplified, additionally it is possible to reduced for solvent Consumption, has saved the production time and has reduced production cost.

In addition, in preparation method of the present invention, arasaponin is divided using steps such as resin adsorption and extractive crystallizations From and purifying, not only easy to operate, and separative efficiency is high, cost is low, the cycle is short, while the purity of product arasaponin It is higher, suitable for industrialized production and popularization.

Embodiment

Technical scheme is clearly and completely described below in conjunction with embodiment, it is clear that described reality It is part of the embodiment of the present invention to apply example, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects Enclose.

According to an aspect of the present invention, a kind of preparation method of Notogineng Extract, the preparation method include following step Suddenly：

(b) pseudo-ginseng extract solution is adsorbed with resin, then by elution, concentration, obtains concentrate；

(d) by pseudo-ginseng crude extract add water dissolve by heating after cooling crystallization, obtain crystal；

(e) under the conditions of gas shield, crystal is dried, then crush be fine powder, that is, obtain content of the total saponins in radix notoginseng >= 80% Notogineng Extract.

In the preferred embodiment of the present invention, in step (a), the dosage of citric acid by addition water quality 2%~3%.The use of citric acid can play the protective effect to arasaponin, avoid arasaponin in production process It is oxidized and influences yield.

Preferably, the water for extraction is purified water, and carrying out extraction with purified water can avoid for compound components of panax notoginseng Pollution；Likewise it is preferred that, the dosage of water is 10 times of pseudo-ginseng quality.

Preferably, the temperature of step (a) the heating extraction is 80 DEG C, and the time is 40~60 minutes.

In the preferred embodiment of the present invention, in step (b), the resin is AB-8, LX-8, LX-16, or HPD826 resins.

By resin adsorption, arasaponin can be adsorbed in resin surface and inside, so as to realize arasaponin Initial gross separation.

In the preferred embodiment of the present invention, in step (b), the eluent is ethanol.

Preferably, in the step (b), eluted by 60~70% ethanol of concentration as eluent.

In the preferred embodiment of the present invention, in step (b), the concentration is heating concentration.

In above-mentioned preferred embodiment, the temperature of the heating concentration is 60~70 DEG C.

Preferably, the step of step (b) eluent concentration is：Eluent is heated into 60~70 DEG C to be concentrated, And the density for being concentrated into solution reaches 1.05~1.12Kg/m³, obtain concentrate.

In the preferred embodiment of the present invention, in step (c), the volumetric usage of ethyl acetate is the volume of concentrate 3~5 times.

Preferably, the step of step (c) extraction is to add in extractor concentrate, be then preferably added extraction The ethyl acetate of 3~5 times of volumes of liquid is taken, then preferably stirs 10min under the conditions of rotating speed is 50~60rpm, then preferably Standing 30min, then respectively collect stratification after solution in aqueous phase and organic phase.

In the preferred embodiment of the present invention, in step (c), the extract, which is concentrated and dried, is：By extract Heating evaporation concentrates, and is dried to gained solid product；

Or the extract is concentrated and dried and is：First extract is concentrated, it is then that gained extraction concentrate spraying is dry It is dry.

In the preferred embodiment of the present invention, in step (d), the temperature of the heating is 70~80 DEG C.

Preferably, the temperature of the cooling crystallization is 4~6 DEG C, and the time is 36~48h.

Preferably, the drying of crystal is carried out in the drying box under conditions of gas shield, and protective gas used is excellent Choosing for nitrogen or inert gas；

Preferably, the drying is carried out under the conditions of 40~60 DEG C, and the dry time is 12~36h.

In the preferred embodiment of the present invention, in step (e), the aperture of screen cloth is 30~70 mesh.

Preferably, the preparation method of Notogineng Extract of the present invention, the preparation method specifically comprise the following steps：

(a) after pseudo-ginseng being ground into 100~200 mesh fine powders, 8~12 times of volume purified waters and 2~3% lemon are added Acid is heated to 70~90 DEG C, extracts 30~60min, collects filter residue and filtrate respectively；

Filter residue carries out secondary extraction according to as above condition, and filtrate is then collected by filtration, and filtrate will merge twice, and obtain pseudo-ginseng Extract solution；

(b) by pseudo-ginseng extract solution with blade diameter length ratio 1:10 macroreticular resin chromatographic column, then with the 60 of 2~5 times of column volumes~ 70% alcohol flushing, not adsorbent, then 60~70% ethanol rinse with 3 times of column volumes is removed, by active ingredient solution Suction is got off, and collects eluent 500mL

Then, the eluent being collected into carries out heating concentration, and thickening temperature is 60~70 DEG C, and is concentrated into concentrated solution density For 1.05~1.12Kg/m³, obtain concentrate；

(c) concentrate adds the ethyl acetate of 5 times of volumes, and 10~20min is stirred under the conditions of rotating speed is 50~60rpm, 20~40min is stood, upper lower leaf, collects aqueous phase and organic phase respectively；

Aqueous phase the same terms reextraction, merges organic phase twice, obtains ethyl acetate solution；

(d) pseudo-ginseng crude extract is added into crystallization bottle, adds 3 times of purified waters, 70~90 DEG C of heating stirrings are filtered off to complete molten Except filter residue, filtrate is cooled to 4~8 DEG C, 30~60h of crystallization, filters off except mother liquor obtains arasaponin crystal；

(e) under nitrogen part, 50~60 DEG C of dry 24~48h, crystal is obtained, 40~60 mesh is crossed after then crystal is crushed Sieve, that is, obtain the Notogineng Extract of content of the total saponins in radix notoginseng >=80%.

Technical scheme is described further below in conjunction with embodiment and comparative example.

Embodiment 1

A kind of preparation method of Notogineng Extract, the preparation method comprise the following steps：

(a) after 200g pseudo-ginseng being ground into 100~200 mesh fine powders, 10 times of volume purified waters and 2% citric acid are added 80 DEG C are heated to, extracts 45min, collects filter residue and filtrate respectively；

Filter residue carries out secondary extraction according to as above condition, and filtrate is then collected by filtration, and filtrate will merge twice, and obtain 2.5L Pseudo-ginseng extract solution；

(b) by pseudo-ginseng extract solution with blade diameter length ratio 1:10 macroreticular resin AB-8 chromatographic columns, then with the 60% of 2 times of column volumes Alcohol flushing, remove not adsorbent, then 70% ethanol rinse with 3 times of column volumes, active ingredient desorb, receipts Collect eluent 500mL；

Then, the eluent being collected into carries out heating concentration, and thickening temperature is 65 DEG C, and is concentrated into concentrated solution density and is 1.06kg/m³, obtain concentrate 100mL；

(c) concentrate adds the ethyl acetate of 5 times of volumes, stirs 10min under the conditions of rotating speed is 50~60rpm, stands 30min, upper lower leaf, aqueous phase and organic phase is collected respectively；

Aqueous phase the same terms reextraction, merges organic phase twice, obtains 500mL ethyl acetate solutions；

(d) pseudo-ginseng crude extract is added into crystallization bottle, adds 3 times of purified waters, 80 DEG C of heating stirrings are filtered off except filter to complete molten Slag, filtrate are cooled to 6 DEG C, crystallization 40h, filter off except mother liquor obtains arasaponin crystal；

(e) under nitrogen part, 50 DEG C of dry 24h, 5g crystal is obtained, 40 mesh sieves is crossed after then crystal is crushed, that is, are obtained The Notogineng Extract of 2.5g content of the total saponins in radix notoginseng >=80%.

Embodiment 2

A kind of preparation method of Notogineng Extract, the preparation method comprise the following steps：

(a) after 200kg pseudo-ginseng being ground into 100~200 mesh fine powders, 10 times of volume purified waters and 2% lemon are added Acid is heated to 80 DEG C, extracts 45min, collects filter residue and filtrate respectively；

Filter residue carries out secondary extraction according to as above condition, and filtrate is then collected by filtration, and filtrate will merge twice, and obtain 2500L pseudo-ginseng extract solutions；

Aqueous phase the same terms reextraction, merges organic phase twice, obtains 5000L ethyl acetate solutions；

(e) under nitrogen part, 50 DEG C of dry 24h, 51kg crystal is obtained, 40 mesh sieves is crossed after then crystal is crushed, are produced To the Notogineng Extract of 50kg content of the total saponins in radix notoginseng >=80%.

Comparative example 1

For this comparative example in addition to step (a) heats and is added without citric acid in leaching process, remaining is same as Example 1.

Effect assessment

In summary, from embodiment 1 and the experimental result of embodiment 2, the preparation method of Notogineng Extract of the present invention The preparation of small-scale Notogineng Extract is applicable not only to, while also can be used in a kilogram extraction for level pseudo-ginseng, and even if is carried out The amplification test of kilogram level, remains able to obtain higher recovery rate, and can obtain the pseudo-ginseng of high content of the total saponins in radix notoginseng Extract.

Meanwhile contrasted from embodiment 1 and the product of comparative example 1, the addition of citric acid can effectively reduce the total soap of pseudo-ginseng The probability that glycosides is oxidized in extraction process, so as to improve the content of arasaponin in product Notogineng Extract.

Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology The scope of scheme.

Claims (10)

1. a kind of preparation method of Notogineng Extract, it is characterised in that the preparation method comprises the following steps：

(a) after pseudo-ginseng being ground into 100~200 mesh fine powders, add water and citric acid to heat extraction, filtering, collect filter residue respectively And filtrate, filter residue add water and citric acid to heat extraction, are filtrated to get filtrate, secondary filtrate is merged again, obtain pseudo-ginseng extraction Liquid；

(b) pseudo-ginseng extract solution is adsorbed with resin, then by elution, concentration, obtains concentrate；

(c) concentrate adds ethyl acetate to extract, then collected organic layer and water layer respectively；Water layer adds ethyl acetate extraction again Take, collected organic layer；Then the organic layer collected twice is merged, obtains extract；Then, extract is concentrated and dried, obtained To pseudo-ginseng crude extract；

(d) by pseudo-ginseng crude extract add water dissolve by heating after cooling crystallization, obtain crystal；

(e) under the conditions of gas shield, crystal is dried, it is fine powder then to crush, that is, obtains content of the total saponins in radix notoginseng >=80% Notogineng Extract.

2. the preparation method of Notogineng Extract according to claim 1, it is characterised in that step

(a) in, the dosage of citric acid by addition water quality 2%~3%.

3. the preparation method of Notogineng Extract according to claim 1, it is characterised in that step

(b) in, the resin is AB-8, LX-8 or HPD826 resin.

4. the preparation method of Notogineng Extract according to claim 1, it is characterised in that step

(b) in, the eluent of the elution is ethanol.

5. the preparation method of Notogineng Extract according to claim 1, it is characterised in that step

(b) in, the concentration is heating concentration.

6. the preparation method of Notogineng Extract according to claim 5, it is characterised in that it is described heating concentration temperature be 60~70 DEG C.

7. the preparation method of Notogineng Extract according to claim 1, it is characterised in that in step (c), ethyl acetate Volumetric usage is 3~5 times of the volume of concentrate.

8. the preparation method of Notogineng Extract according to claim 1, it is characterised in that in step (c), the extract It is concentrated and dried and is：Extract heating evaporation is concentrated, dried to gained solid product；

Or the extract is concentrated and dried and is：First extract is concentrated, then by gained extraction concentrate spray drying.

9. the preparation method of Notogineng Extract according to claim 1, it is characterised in that in step (d), the heating Temperature is 70~80 DEG C；

Preferably, the temperature of the cooling crystallization is 4~6 DEG C, and the time is 36~48h.

10. the preparation method of Notogineng Extract according to claim 1, it is characterised in that in step (e), the hole of screen cloth Footpath is 30~70 mesh.

CN201711209777.9A 2017-11-27 2017-11-27 The preparation method of Notogineng Extract Pending CN107693559A (en)

Priority Applications (1)

Application Number	Priority Date	Filing Date	Title
CN201711209777.9A CN107693559A (en)	2017-11-27	2017-11-27	The preparation method of Notogineng Extract

Applications Claiming Priority (1)

Application Number	Priority Date	Filing Date	Title
CN201711209777.9A CN107693559A (en)	2017-11-27	2017-11-27	The preparation method of Notogineng Extract

Publications (1)

Publication Number	Publication Date
CN107693559A true CN107693559A (en)	2018-02-16

Family

ID=61185990

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
CN201711209777.9A Pending CN107693559A (en)	2017-11-27	2017-11-27	The preparation method of Notogineng Extract