CN109200101A - A kind of preparation method of Boschniakia rossica Extract - Google Patents
A kind of preparation method of Boschniakia rossica Extract Download PDFInfo
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- CN109200101A CN109200101A CN201811335545.2A CN201811335545A CN109200101A CN 109200101 A CN109200101 A CN 109200101A CN 201811335545 A CN201811335545 A CN 201811335545A CN 109200101 A CN109200101 A CN 109200101A
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- 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)
- A61K36/64—Orobanchaceae (Broom-rape family)
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- 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
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- 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, decoction
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- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- 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
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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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Abstract
The invention discloses a kind of preparation methods of Boschniakia rossica Extract, this method is first to pulverize broomrape raw material, then broken wall, subcritical water technology is recycled to extract, it extracts feed liquid and uses purification with macroreticular resin after being centrifuged, being concentrated, obtain Boschniakia rossica Extract product finally by concentration and spray drying.Advantages of the present invention includes two aspects: 1, being destroyed using the micro-nano wall breaking technology of low temperature to broomrape cell wall, can significantly improve the release of broomrape general glycoside.2, using Subcritical water chromotagraphy technology, Extraction solvent is the water under subcritical state, rather than other organic solvents, can improve extraction efficiency, in turn avoid the waste of resource, not can cause environmental pollution also.
Description
Technical field
The invention belongs to field of natural organic chemistry, are related to a kind of side that Boschniakia rossica Extract is prepared using broomrape as raw material
Method.It is prepared using cell wall breaking technology and Subcritical water chromotagraphy technology using broomrape general glycoside as chief active more particularly to a kind of
The method of the Boschniakia rossica Extract of ingredient.
Background technique
Broomrape is the herb of Orobanchaceae Orobanche plant broomrape, with all herbal medicine.Spring excavation, dries dissection.It is main
It is distributed in Changbai Mountain in China area and Region of The Northern Part of Daxinganling mountain area, NORTHERN KOREA mountain area, Japanese Fuji, Russian west
Berli subregion is also distributed.Broomrape nature and flavor are sweet, sour, wet, cure mainly impotence due to the kidney deficiency, waist and knee crymodynia, the drip of urine something lost, metrorrhagia and metrostaxis band
Under, the diseases such as dry constipation of intestines, cystitis, there is the effect of tonifying kidney and strengthening yang, relax bowel and defecation, cooperation other drugs can treat nocturnal emission, woman
A variety of diseases such as the infertile equal genital system diseases of female, senility habitual constipation, cystitis, blood urine, also have rheumatic arthritis
Certain curative effect.
The broomrape herb deoxidation vomiting nut of table containing 8- glucoside acid (8-epideoxyloganic acid), broomrape cinnamyl alcohol
Glucoside (rossicaside) B, C, D, broomrape cinnamyl alcohol glucoside A, broomrape glucoside (boschnaside), boschniakine glucoside
(boschnaloside), pinoresinol-β-D- glucopyanoside (pinoresinol- β-D-glucopyranoside), p-
Coumaric acid (p-coumaric acid), p-coumaric acid methyl esters (methyl p-coumarate), cupreol (β-sitos-
Terol), the chemical components such as oleanolic acid (oleanolic acid), 3-Epioleanolic Acid (3-epioleanolic acid).
Glucoside substance in broomrape is the natural active matter that a kind of pair of human health has significant health-care effect, has been caused
The spectrum of international community is all over pass column.Domestic at present is mainly that organic solvent extracts to the extracting method of glucoside substance in broomrape,
Have using supercritical carbon dioxide extraction.The present invention uses Subcritical water chromotagraphy technology to the glucoside object in broomrape for the first time
Matter extracts.
Summary of the invention
The purpose of the present invention is to provide a kind of using broomrape general glycoside as the system of the Boschniakia rossica Extract of main active
Preparation Method.The present invention first pulverizes broomrape, then broken wall, recycles Subcritical water chromotagraphy technology to extract, finally
Boschniakia rossica Extract product is obtained using purification with macroreticular resin.
The technical proposal of the invention is realized in this way, it the following steps are included:
(1) it pulverizes raw material broomrape to obtain powder；
(2) powder obtained in step (1) is subjected to breaking-wall cell processing；
(3) powder after broken wall treatment in step (2) is extracted and is centrifuged using Subcritical water chromotagraphy technology, collected respectively
Material residue and centrifugate, material residue carry out second and extract, and extracting parameter is the same as the first time.The centrifugate extracted twice merges；
(4) centrifugate obtained in step (3) is concentrated, obtains concentrate A；
(5) concentrate A obtained in step (4) is used into purification with macroreticular resin, collects ethanol eluate；
(6) ethanol eluate collected in step (5) is concentrated, obtains concentrate B；
(7) concentrate B obtained in step (6) is spray-dried, obtains Boschniakia rossica Extract powder.
The preferable technical solution of the present invention is: in the step (1), after broomrape pulverizes, the mesh number of powder exists
It is more than 300 mesh.
The preferable technical solution of the present invention is: in the step (2), the method for breaking-wall cell processing is that low temperature is micro-nano
Wall breaking technology, ultra-micro powder is placed under -170 DEG C of low temperature environment makes its freezing, and then room temperature melts again, and repeatedly 4~7
It is secondary, so that cell wall is broken.
The preferable technical solution of the present invention is: broken to broomrape using Subcritical water chromotagraphy technology in the step (3)
Wall powder extracts, and pressure limit is 15~20MPa, and Extracting temperature is 330~350 DEG C, broomrape broken wall powder: water=1:5
~8(m/m), extraction time is 20~30min.
The preferable technical solution of the present invention is: in the step (3), extracting feed liquid and is centrifuged using tube centrifuge
Separation, the revolving speed of centrifuge are 10000~16000r/min.
The preferable technical solution of the present invention is: in the step (4), using reduced pressure, and vacuum degree is -0.07~-
0.08Mpa, thickening temperature is at 80~90 DEG C.It is concentrated into concentrate A: broomrape broken wall powder=1:0.8~1.2(m/m) until.
The preferable technical solution of the present invention is: in the step (5), on macroporous absorbent resin selection D101, concentrate A
Column flow rate is 1.5BV/h, and washing flow velocity is 2BV/h, and the ethanol solution that eluting solvent is 70%, elution flow rate 2BV/h washes
De- agent dosage is 6BV.
The preferable technical solution of the present invention is: in the step (6), using reduced pressure, and vacuum degree is -0.05~-
0.07Mpa, thickening temperature is at 55~65 DEG C.The content of solid content in concentrate B is concentrated between 20~30%.
The invention has the following advantages that
1, the present invention destroys broomrape cell wall using the micro-nano wall breaking technology of low temperature, and it is total can to significantly improve broomrape
The release of glucoside.
2, the present invention uses Subcritical water chromotagraphy technology, and Extraction solvent is the water under subcritical state, rather than other have
Solvent can improve extraction efficiency, in turn avoid the waste of resource, not can cause environmental pollution also.
Specific embodiment
Embodiment 1
Broomrape herb 1kg is taken to be crushed to 300 mesh with micronizer, then by ultra-micro powder superfreeze to -170 DEG C,
Room temperature is melted again, repeated freezing, thawing step 4 times.The purified water stirring that 8kg is added in treated powder is equal
It is even, 20min is extracted under conditions of pressure 15Mpa, temperature are 330 DEG C.Feed liquid is carried out with tube centrifuge after the completion of extraction
Centrifugation, centrifuge speed 13000r/min collect centrifugate into storage tank, and material residue carries out the 2nd time and extracts and be centrifuged, and merge 2
Secondary centrifugate.Centrifugate is using being concentrated under reduced pressure, and vacuum degree -0.07Mpa, 90 DEG C of temperature, the weight for obtaining concentrate A is
1.03kg.Concentrate A is purified with D101 type macroporous absorbent resin, column flow rate is 1.5BV/h, water lotion on concentrate A
Flow velocity is 2BV/h, and the water lotion of punching to outflow is colourless, then continues to elute with 70% ethanol solution, elution flow rate 2BV/
H, 70% ethanol solution dosage are 6BV, collect ethanol elution solvent portions.The ethanol elution solution of collection is used again and is subtracted
Pressure concentration, vacuum degree -0.05Mpa, 65 DEG C of temperature, the weight for obtaining concentrate B is 261.7g.Then concentrate B is sprayed
Mist is dry, obtains the Boschniakia rossica Extract powder 56.5g that broomrape general glycoside purity is 42.17%.
Embodiment 2
Broomrape herb 1kg is taken to be crushed to 300 mesh with micronizer, then by ultra-micro powder superfreeze to -170 DEG C,
Room temperature is melted again, repeated freezing, thawing step 5 times.The purified water stirring that 7kg is added in treated powder is equal
It is even, 25min is extracted under conditions of pressure 18Mpa, temperature are 340 DEG C.Feed liquid is carried out with tube centrifuge after the completion of extraction
Centrifugation, centrifuge speed 15000r/min collect centrifugate into storage tank, and material residue carries out the 2nd time and extracts and be centrifuged, and merge 2
Secondary centrifugate.Centrifugate is using being concentrated under reduced pressure, and vacuum degree -0.08Mpa, 85 DEG C of temperature, the weight for obtaining concentrate A is
0.97kg.Concentrate A is purified with D101 type macroporous absorbent resin, column flow rate is 1.5BV/h, water lotion on concentrate A
Flow velocity is 2BV/h, and the water lotion of punching to outflow is colourless, then continues to elute with 70% ethanol solution, elution flow rate 2BV/
H, 70% ethanol solution dosage are 6BV, collect ethanol elution solvent portions.The ethanol elution solution of collection is used again and is subtracted
Pressure concentration, vacuum degree -0.06Mpa, temperature 60 C, the weight for obtaining concentrate B is 247.8g.Then concentrate B is sprayed
Mist is dry, obtains the Boschniakia rossica Extract powder 54.8g that broomrape general glycoside purity is 43.66%.
Embodiment 3
Broomrape herb 1kg is taken to be crushed to 300 mesh with micronizer, then by ultra-micro powder superfreeze to -170 DEG C,
Room temperature is melted again, repeated freezing, thawing step 6 times.The purified water stirring that 6kg is added in treated powder is equal
It is even, 30min is extracted under conditions of pressure 20Mpa, temperature are 350 DEG C.Feed liquid is carried out with tube centrifuge after the completion of extraction
Centrifugation, centrifuge speed 16000r/min collect centrifugate into storage tank, and material residue carries out the 2nd time and extracts and be centrifuged, and merge 2
Secondary centrifugate.Centrifugate is using being concentrated under reduced pressure, and vacuum degree -0.08Mpa, 80 DEG C of temperature, the weight for obtaining concentrate A is
1.06kg.Concentrate A is purified with D101 type macroporous absorbent resin, column flow rate is 1.5BV/h, water lotion on concentrate A
Flow velocity is 2BV/h, and the water lotion of punching to outflow is colourless, then continues to elute with 70% ethanol solution, elution flow rate 2BV/
H, 70% ethanol solution dosage are 6BV, collect ethanol elution solvent portions.The ethanol elution solution of collection is used again and is subtracted
Pressure concentration, vacuum degree -0.07Mpa, 55 DEG C of temperature, the weight for obtaining concentrate B is 233.2g.Then concentrate B is sprayed
Mist is dry, obtains the Boschniakia rossica Extract powder 55.1g that broomrape general glycoside purity is 43.39%.
Above-described embodiment is technical conception and technical characteristics to illustrate the invention, can not limit the present invention with this
Protection scope.The equivalent transformation or modification that all essence according to the present invention is done, should all cover in protection model of the invention
Within enclosing.
Claims (11)
1. a kind of preparation method of Boschniakia rossica Extract, which is characterized in that including the following steps:
(1) it pulverizes raw material broomrape to obtain powder；
(2) powder obtained in step (1) is subjected to breaking-wall cell processing；
(3) powder after broken wall treatment in step (2) is extracted and is centrifuged using Subcritical water chromotagraphy technology, collected respectively
Material residue and centrifugate, material residue carry out second and extract, and extracting parameter is the same as the first time.
2. the centrifugate extracted twice merges；
(4) centrifugate obtained in step (3) is concentrated, obtains concentrate A；
(5) concentrate A obtained in step (4) is used into purification with macroreticular resin, collects ethanol eluate；
(6) ethanol eluate collected in step (5) is concentrated, obtains concentrate B；
(7) concentrate B obtained in step (6) is spray-dried, obtains Boschniakia rossica Extract powder.
3. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (1)
In, after broomrape pulverizes, the mesh number of powder is more than 300 mesh.
4. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (2)
In, the method for breaking-wall cell processing is the micro-nano wall breaking technology of low temperature, ultra-micro powder is placed under -170 DEG C of low temperature environment
Make its freezing, then room temperature melts again, and 4~7 times repeatedly, so that cell wall is broken.
5. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (3)
In, broomrape broken wall powder is extracted using Subcritical water chromotagraphy technology, pressure limit is 15~20MPa, Extracting temperature
It is 330~350 DEG C, broomrape broken wall powder: water=1:5~8(m/m), extraction time is 20~30min.
6. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (3)
In, it extracts feed liquid and is centrifuged using tube centrifuge, the revolving speed of centrifuge is 10000~16000r/min.
7. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (4)
In, using reduced pressure, vacuum degree is -0.07~-0.08Mpa, and thickening temperature is at 80~90 DEG C.
8. being concentrated into concentrate A: broomrape broken wall powder=1:0.8~1.2(m/m) until.
9. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (5)
In, macroporous absorbent resin selects D101, and column flow rate is 1.5BV/h on concentrate A, and washing flow velocity is 2BV/h, and eluting solvent is
70% ethanol solution, elution flow rate 2BV/h, eluting agent 6BV.
10. a kind of preparation method of Boschniakia rossica Extract according to claim 1, it is characterised in that: the step (6)
In, using reduced pressure, vacuum degree is -0.05~-0.07Mpa, and thickening temperature is at 55~65 DEG C.
11. being concentrated into the content of solid content in concentrate B between 20~30%.
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| CN201811335545.2A CN109200101A (en) | 2018-11-13 | 2018-11-13 | A kind of preparation method of Boschniakia rossica Extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109893608A (en) * | 2019-04-03 | 2019-06-18 | 吉林省精鑫药业集团有限公司 | A kind of preparation method of Chinese patent drug gastrodia capsule content |
| CN109985018A (en) * | 2019-04-08 | 2019-07-09 | 吉林省精鑫药业集团有限公司 | A kind of preparation method of Chinese materia medica preparation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044504A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting boschniakia rossica glucoside form boschniakia rossica |
-
2018
- 2018-11-13 CN CN201811335545.2A patent/CN109200101A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044504A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting boschniakia rossica glucoside form boschniakia rossica |
Non-Patent Citations (1)
| Title |
|---|
| 郑光耀等: "亚临界水萃取技术在植物提取物领域的应用研究进展", 《林产化学与工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109893608A (en) * | 2019-04-03 | 2019-06-18 | 吉林省精鑫药业集团有限公司 | A kind of preparation method of Chinese patent drug gastrodia capsule content |
| CN109985018A (en) * | 2019-04-08 | 2019-07-09 | 吉林省精鑫药业集团有限公司 | A kind of preparation method of Chinese materia medica preparation |
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