CN110407894A - The extracting method of effective component in a kind of two capillus of Yi nationality's medicine - Google Patents
The extracting method of effective component in a kind of two capillus of Yi nationality's medicine Download PDFInfo
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- CN110407894A CN110407894A CN201910627215.9A CN201910627215A CN110407894A CN 110407894 A CN110407894 A CN 110407894A CN 201910627215 A CN201910627215 A CN 201910627215A CN 110407894 A CN110407894 A CN 110407894A
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- capillus
- nationality
- effective component
- alcoholic solution
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- 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)
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The present invention discloses a kind of extracting method of effective component in two capillus of Yi nationality's medicine, including takes two capillus plant, cleans and the pre-treatment step of natural air drying or low temperature drying;Two capillus plant of dried and clean are crushed, sieving obtains the pulverising step of two capillus powder;Alcoholic solution is added in two capillus powder and grinds 25~35min, obtain extraction material adds alcohol grinding steps;Said extracted is subjected to refluxing extraction by alcoholic solution with material in 25 ~ 50 DEG C of ultrasound environments, the reflux that crude extract is obtained after collection extracting solution concentration slightly proposes step;Crude extract is separated with macroreticular resin, obtains the separating step of essence extract;Essence extract is dried, the drying steps of gentiamarin monomer are obtained.The present invention has the characteristics that easy to operate, extraction efficiency is high, yield of effective components and purity is high.
Description
Technical field
The invention belongs to natural drug purification technique fields, and in particular to it is a kind of it is easy to operate, extraction efficiency is high, effectively at
It is divided to the extracting method of effective component in two capillus of Yi nationality's medicine of recovery rate and purity is high.
Background technique
Two capillus (Incarvillea arguta, Yi nationality's medicine name: watt cloth friend) and it is the perennial tool stem draft of Bignoniaceae Incarvillea AJuss
Plant, also known as: suona horn flower firecracker flower, closestool flower, Yan Hongdou, is passed through towards day, hepatitis grass etc., has medical value, herb can enter
Medicine, at present not yet by artificial introducing and planting.It is grown on 1400~2700(-3400 of height above sea level) meter area, the Lancang River, Drainage Area of Jinsha River
Dry-hot valley area, in roadside, shrubbery.Produce Northeast Yunnan, China, east, in west, northwest, distribution Southeast Sichuan, WESTERN GUIZHOU and
The northwestward, Gansu, Tibet.India and Himalayas various countries also have.
Yi nationality, distributed over Yunnan, Sichuan and Guizhou's drug is the summary of experience and wisdom crystallization that the Yi nationality, distributed over Yunnan, Sichuan and Guizhou people struggle with disease for a long time, is Chinese medicine greatness
An important component in treasure-house." watt cloth friend " is traditional Yi nationality doctor's Generally used, with dispelling wind and eliminating dampness and activating microcirculation and removing stasis medicinal
Effect is mainly used for treating hepatopathy (hepatitis, hepatomegaly, hepatodynia etc.), diarrhea (bacillary dysentery, enteritis etc.), toothache (including lymph junction
Core, parotitis, acute toothache, periodontitis etc.), carbuncle swells (including cream pain, furunculosis, nameless sores or boils), Fracture Hematoma, rheumatism internal lesion caused by overexertion etc.
Disease.Existing research shows that two capillus have good effect in treatment liver's illness and dysentery, preparation is used for clinical treatment acute bacillary dysentery
And virus hepatitis, cure rate are higher than the control group with western medicine.The B prime (ursolic acid) and D prime (enol therefrom isolated
Compound B a pair of copper compound) be respectively have the effects that reduce serum glutamic pyruvic transminase, cooling, antibacterial, calmness it is effective at
Point.
Two capillus contain a variety of chemical components, at present from its rhizome or the isolated monoterpene of aerial part, iridoid, times
The compounds such as hemiterpene, triterpene, steroidal, alkaloid, flavones, amide, Phenylpropanoid Glycosides.Wherein gentiamarin mainly having as two capillus
Ingredient is imitated, certain concern has been obtained, but the extraction of two capillus principle active component gentiamarins in the prior art is generally existing
The problem of extraction efficiency is low, yield and purity are low, trivial operations, so that the resource utilization of two capillus of natural plant is lower.
Summary of the invention
The purpose of the present invention is to provide it is a kind of it is easy to operate, extraction efficiency is high, the Yi nationality of effective component yield and purity is high
The extracting method of effective component in two capillus of medicine.
The object of the present invention is achieved like this: slightly mentioning, separates, dries including pretreatment, crushing plus alcohol grinding, reflux
Step, the specific steps are as follows:
A, it pre-processes: taking two capillus plant, clean simultaneously natural air drying or low temperature drying;
B, it crushes: two capillus plant of dried and clean is crushed, sieving obtains two capillus powder;
C, plus alcohol is ground: alcoholic solution being added in two capillus powder and grinds 25~35min, obtains extraction material;
D, reflux slightly mentions: said extracted being carried out refluxing extraction by alcoholic solution with material in 25 ~ 50 DEG C of ultrasound environments, is received
Crude extract is obtained after collection extracting solution concentration;
E, it separates: crude extract being separated with macroreticular resin, obtains essence extract;
F, drying: essence extract is dried, and obtains gentiamarin monomer.
The invention has the benefit that
1, the present invention is aided with separation by cleverly limiting the parameter areas such as the thick temperature raising degree of reflux and milling time and cooperating
And drying process, so as to guarantee the yield and purity of final gentiamarin monomer, significantly improve while simplifying operation
The medical values of two capillus.
2, the present invention is ground by the way that alcoholic solution is added with two capillus powder, prevents the effect of rough gentian hardship enzyme in plant
Issue unboiled water solution;It is especially additionally added cellulase, can be to the full extent crushed the cell wall of two capillus plant, so that interior
The active principle in portion dissolves out, and so during subsequent alcohol extracting, can also more preferably extract these effective components.
3, slightly to mention alcoholic solution in step to the dissolution of effective component carried out in ultrasound environments for present invention reflux, using super
Sound effect accelerates the dissolution of effective component in a solvent, improves the recovery rate of effective component.
4, after the present invention passes through alcoholic solution refluxing extraction, using the isolated crude extract of macroreticular resin, so that final
Gentiamarin monomer yield and purity are higher, and are separated using alcoholic solution refluxing extraction and macroreticular resin, and alcoholic solution can return
Receipts are recycled, and can avoid the pollution to environment, while reduce cost.
Therefore, the present invention has the characteristics that easy to operate, extraction efficiency is high, effective component yield and purity is high.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but the present invention is limited in any way,
Any changes and modifications based on technical field, all belong to the scope of protection of the present invention.
The present invention includes pretreatment, crushes, adds alcohol grinding, reflux slightly mention, separate, drying steps, the specific steps are as follows:
A, it pre-processes: taking two capillus plant, clean simultaneously natural air drying or low temperature drying;
B, it crushes: two capillus plant of dried and clean is crushed, sieving obtains two capillus powder;
C, plus alcohol is ground: alcoholic solution being added in two capillus powder and grinds 25~35min, obtains extraction material;
D, reflux slightly mentions: said extracted being carried out refluxing extraction by alcoholic solution with material in 25 ~ 50 DEG C of ultrasound environments, is received
Crude extract is obtained after collection extracting solution concentration;
E, it separates: crude extract being separated with macroreticular resin, obtains essence extract;
F, drying: essence extract is dried, and obtains gentiamarin monomer.
Two capillus plant smashed it through 1,2 or No. 3 standard medicine sieve in the step B.
The feed liquid mass ratio of two capillus powder and alcoholic solution is 1:2~4 in the step C, is also added in the step C
Cellulase.
Alcoholic solution in the step C before the milling total amount of adding 40~60%, remaining part divides 1 during the grinding process
~5 additions.
Alcoholic solution in the step C is the ethanol solution that volume fraction is 60~80%, the alcoholic solution in the D step
The ethanol solution for being 30~50% for volume fraction.
Extraction passes through alcoholic solution refluxing extraction 3 times in 25~50 DEG C of ultrasound environments with material in the D step.
The feed liquid mass ratio of extraction material and alcoholic solution is 1:6~12, returns for each time in each secondary refluxing extraction of D step
The time of stream is 30~60min.
It is ground under normal pressure state in the step C.
Isolated essence extract is freeze-dried in the F-step, obtains gentiamarin monomer.
Embodiment 1
S1: taking two capillus plant, cleans simultaneously natural air drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes (No. 2 standard medicine sieves, similarly hereinafter), are obtained two capillus powder
End.
S3: the ethanol solution that volume fraction is 70% is added by feed liquid mass ratio 1:3 in two capillus powder, then normal
30min is ground under pressure condition, obtains extraction material.
S4: the ethanol solution that said extracted material volume fraction is 30% is flowed back in 25 DEG C of ultrasound environments and is mentioned
It takes 3 times, obtains crude extract after extracting solution concentration;Wherein this 3 times reflux feed liquid mass ratioes and the time be respectively as follows: (1:12,
60min), (1:9,45min), (1:6,30min).
S5: crude extract is separated by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, obtain gentiamarin monomer.
Embodiment 2
S1: taking two capillus plant, cleans simultaneously low temperature drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes, are obtained two capillus powder.
S3: the ethanol solution that the volume fraction of total amount 50% is 70% is added by solid-liquid ratio 1:4 in two capillus powder, is then existed
35min is ground under normal pressure state, is divided the alcoholic solution of 5 addition residues 50% during the grinding process, is obtained extraction material.
S4: will be above-mentioned that extraction through-put volume score returns in 25 DEG C of ultrasound environments for 50% ethanol solution
Stream No. 3 times obtains crude extract after extracting solution concentration;Wherein this 3 times reflux feed liquid mass ratioes and the time be respectively as follows: (1:12,
60min), (1:9,45min), (1:6,30min).
S5: crude extract is separated by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, obtain gentiamarin monomer.
Embodiment 3
S1: taking two capillus plant, cleans simultaneously natural air drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes, are obtained two capillus powder.
S3: the ethanol solution that the volume fraction of total amount 40% is 70% is added by solid-liquid ratio 1:2 in two capillus powder, in normal pressure
25min is ground under state, is divided the alcoholic solution of 3 addition residues 60% during the grinding process, is obtained extraction material.
S4: above-mentioned extraction is flowed back 3 with the ethanol solution that through-put volume score is 30% in 50 DEG C of ultrasound environments
It is secondary, crude extract is obtained after extracting solution concentration;Wherein this 3 times reflux feed liquid mass ratioes and the time be respectively as follows: (1:12,60min),
(1:9,45min), (1:6,30min).
S5: decolorization is carried out to crude extract by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, obtain gentiamarin monomer.
Embodiment 4
S1: taking two capillus plant, cleans simultaneously natural air drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes, are obtained two capillus powder.
S3: the ethanol solution that the volume fraction of total amount 60% is 70% is added by solid-liquid ratio 1:3 in two capillus powder, in normal pressure
30min is ground under state, is divided the alcoholic solution of 4 addition residues 40% during the grinding process, is obtained extraction material.
S4: said extracted is flowed back 3 with the ethanol solution that through-put volume score is 50% in 40 DEG C of ultrasound environments
It is secondary, crude extract is obtained after extracting solution concentration;Wherein this 3 times reflux feed liquid mass ratioes and the time be respectively as follows: (1:12,60min),
(1:9,45min), (1:6,30min).
S5: crude extract is separated by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, obtain gentiamarin monomer.
Embodiment 5
S1: taking two capillus plant, cleans simultaneously natural air drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes, are obtained two capillus powder.
S3: being added the ethanol solution that the volume fraction of total amount 50% is 70% by feed liquid mass ratio 1:3.5 for two capillus powder,
30min is ground under normal pressure state, the alcoholic solution of residue 50% is added again after grinding 15min, obtains extraction material.
S4: it is 40% ethanol solution by said extracted through-put volume score, while cellulase is added, at 30 DEG C
It flows back 3 times in ultrasound environments, obtains crude extract after extracting solution concentration;Wherein the feed liquid mass ratio of this 3 times reflux and time difference
Are as follows: (1:12,60min), (1:9,45min), (1:6,30min).
S5: crude extract is separated by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, obtain gentiamarin monomer.
Embodiment 6
S1: taking two capillus plant, cleans simultaneously low temperature drying.
S2: two capillus plant of dried and clean are crushed, and are crossed 24 meshes, are obtained two capillus powder.
S3: the ethanol solution that the volume fraction of total amount 60% is 70% is added by solid-liquid ratio 1:2.5 in two capillus powder, normal
35min is ground under pressure condition, is divided the alcoholic solution of 2 addition residues 40% during the grinding process, is obtained extraction material.
S4: it is 50% ethanol solution by said extracted through-put volume score, while cellulase is added, at 45 DEG C
It flows back 3 times in ultrasound environments, obtains crude extract after extracting solution concentration;Wherein the feed liquid mass ratio of this 3 times reflux and time difference
Are as follows: (1:12,60min), (1:9,45min), (1:6,30min).
S5: separating treatment is carried out to crude extract by macroreticular resin partition method, obtains essence extract.
S6: essence extract is freeze-dried, and obtains gentiamarin monomer.
Record the yield such as table 1 of gentiamarin in embodiment 1 to 6.
The yield of gentiamarin in each embodiment of table 1
Claims (9)
1. the extracting method of effective component in a kind of two capillus of Yi nationality's medicine, it is characterised in that ground including pretreatment, crushing plus alcohol,
Reflux slightly mention, separate, drying steps, the specific steps are as follows:
A, it pre-processes: taking two capillus plant, clean simultaneously natural air drying or low temperature drying;
B, it crushes: two capillus plant of dried and clean is crushed, sieving obtains two capillus powder;
C, plus alcohol is ground: alcoholic solution being added in two capillus powder and grinds 25~35min, obtains extraction material;
D, reflux slightly mentions: said extracted being carried out refluxing extraction by alcoholic solution with material in 25 ~ 50 DEG C of ultrasound environments, is received
Crude extract is obtained after collection extracting solution concentration;
E, it separates: crude extract being separated with macroreticular resin, obtains essence extract;
F, drying: essence extract is dried, and obtains gentiamarin monomer.
2. according to claim 1 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that two in the step B
Capillus plant smashes it through 1,2 or No. 3 standard medicine sieve.
3. according to claim 1 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that two in the step C
The feed liquid mass ratio of capillus powder and alcoholic solution is 1:2~4, is also added with cellulase in the step C.
4. according to claim 3 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that in the step C
Alcoholic solution before the milling total amount of adding 40~60%, remaining part divide during the grinding process 1~5 time addition.
5. according to claim 1 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that in the step C
Alcoholic solution is the ethanol solution that volume fraction is 60~80%, and it is 30~50% that the alcoholic solution in the D step, which is volume fraction,
Ethanol solution.
6. according to claim 1 into two capillus of Yi nationality's medicine described in 5 any one effective component extracting method, it is characterised in that institute
It states extraction material in D step and passes through alcoholic solution refluxing extraction 3 times in 25~50 DEG C of ultrasound environments.
7. according to claim 6 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that each time of the D step
The feed liquid mass ratio of extraction material and alcoholic solution is 1:6~12 in refluxing extraction, each time flowed back is 30~60min.
8. according to claim 6 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that in the step C
It is ground under normal pressure state.
9. according to claim 6 in two capillus of Yi nationality's medicine effective component extracting method, it is characterised in that in the F-step will
Isolated essence extract is freeze-dried, and gentiamarin monomer is obtained.
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