CN102344417A - Extraction method for ligustrazine - Google Patents
Extraction method for ligustrazine Download PDFInfo
- Publication number
- CN102344417A CN102344417A CN2010102471171A CN201010247117A CN102344417A CN 102344417 A CN102344417 A CN 102344417A CN 2010102471171 A CN2010102471171 A CN 2010102471171A CN 201010247117 A CN201010247117 A CN 201010247117A CN 102344417 A CN102344417 A CN 102344417A
- Authority
- CN
- China
- Prior art keywords
- chloroform
- extraction
- adds
- carrying
- extracting
- Prior art date
- 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
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to an extraction method for ligustrazine. Process steps of the extraction comprise: adopting crude powder of ligusticum chuanxiong hort rhizome; adding ethanol to the crude powder to carry out reflux extraction; mixing the resulting extracting solutions; carrying out vacuum concentration until the volume of the resulting solution is 1 time the volume of the ligusticum chuanxiong hort; carrying out cold preservation and filtration; adding ether to the filtrate to carry out extraction; extracting the ether phase through sulfuric acid; adjusting the pH value of the water layer to 9-10; carrying out extraction through chloroform; recovering the solvent from the chloroform layer; adding sulfuric acid to carry out dissolution; carrying out filtration; adding the chloroform to the filtrate to carry out extraction, wherein the amount of the chloroform is the same as the amount of the filtrate; removing the chloroform layer, vacuum recovering the solvent; adding petroleum ether to the solvent to carry out dissolution; carrying out filtration, vacuum recovering the petroleum ether to obtain the extract; adding the extract to a alumina chromatography column; carrying out elution through a mixture comprising the petroleum ether and the chloroform, wherein a volume of the petroleum ether to the chloroform is 3:2; collecting the eluent; vacuum recovering the solvent, then drying to obtain the crude crystal; adding dehydrated alcohol to the crude crystal to carry out recrystallization; carrying out washing and drying to obtain the product. With adopting the method provided by the present invention to prepare the ligustrazine, the product purity is high, the operation is convenient, the pollution is low, and the equipment investment is less.
Description
Technical field
The present invention relates to a kind of process for extracting of Ligustrazine, especially a kind of method of utilizing alcohol extracting, extraction, chromatography to extract Ligustrazine.
Background technology
Ligustrazine
Formal name used at school: Tetramethylpyrazine
Molecular formula: C
8H
12N
2
Molecular weight: 136.20
Molecular structure:
Compositional classification: alkaloid
Physical properties: colourless needle crystal, fusing point 80-82 ° (micro-mensuration), 190 ℃ of boiling points.Have special foreign odor, water absorbability is arranged, be prone to distillation.Be soluble in hot water, sherwood oil, be dissolved in chloroform, dilute hydrochloric acid, be slightly soluble in ether, be insoluble to cold water.
Ligusticum wallichii is the dry rhizome of samphire Ligusticum wallichii Ligusticum chuanxiong Hort..Have blood-activating and qi-promoting, the effect of wind-expelling pain-stopping is used to pacify nerve, a wind headache just, abdominal mass stomachache, the shouting pain of the chest side of body, tumbling and swelling, headache, rheumatic arthralgia.
Ligustrazine (Ligustrazine) is a kind of effective constituent that contains in the Chinese medicine Ligusticum wallichii; Has antiplatelet aggregative activity; And vasodilation, coronary blood flow increasing, microcirculation improvement and the effect of cerebral blood flow increasing amount are arranged, the effect of protection vascular endothelial cell is still arranged in addition.The clinical treatment ischemic heart vascular disease that are applicable to are like coronary heart disease, cerebral blood supply insufficiency, cerebral thrombosis, cerebral embolism, vasculitis etc.
In the prior art, the process for extracting yield of Ligustrazine is low, purity is not high.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, Ligustrazine that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) alcohol extracting: get Ligusticum wallichii rhizome meal, add 3-8 and doubly measure the 50-90% alcohol reflux 1-3 time, each 1.5 hours, united extraction liquid was evaporated to 1 times of amount of medicinal material volume, refrigerates 8-16 hour, filters, and gets filtrating;
2) extraction: filtrating adds the equivalent extracted with diethyl ether, gets ether solution, adds the extraction of equivalent 2mol/L sulfuric acid; The water intaking layer adds basic solution and regulates PH9-10, adds the equal amounts of chloroform extraction; Get chloroform layer, the reclaim under reduced pressure chloroform is done near, adds the 2mol/L sulfuric acid dissolution; Filter, filtrating adds the equal amounts of chloroform extraction, gets chloroform layer; Decompression and solvent recovery is done near, adds petroleum ether dissolution, filters; The reclaim under reduced pressure sherwood oil gets medicinal extract;
3) chromatography: add alumina chromatographic column, use sherwood oil: chloroform (3: 2) wash-out, collect elutriant, decompression and solvent recovery is also dry, gets coarse crystallization, adds the dehydrated alcohol recrystallization, washs, is drying to obtain.
The said extracted method is characterized in that the parameter of said refluxing extraction is: add 6 times of amount 80% alcohol heating reflux 2 times, each 1.5 hours.
The said extracted method is characterized in that said basic solution can be a kind of in saturated limewater, saturated sodium bicarbonate, the soda ash solution.
The said extracted method, the time that it is characterized in that said refrigeration is 12 hours.
Adopt technique scheme to prepare Ligustrazine, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1
Get Ligusticum wallichii rhizome meal 100g, add 3 times of amount 50% alcohol reflux 1 time, each 1.5 hours; United extraction liquid is evaporated to 1 times of amount of medicinal material volume, refrigerates 8 hours; Filter, filtrating adds the equivalent extracted with diethyl ether, gets ether solution; Add the extraction of equivalent 2mol/L sulfuric acid, the water intaking layer adds saturated sodium bicarbonate and regulates PH9-10; Add the equal amounts of chloroform extraction, get chloroform layer, the reclaim under reduced pressure chloroform is done near; Add the 2mol/L sulfuric acid dissolution, filter, filtrating adds the equal amounts of chloroform extraction; Get chloroform layer, decompression and solvent recovery is done near, adds petroleum ether dissolution; Filter; The reclaim under reduced pressure sherwood oil adds alumina chromatographic column, uses sherwood oil: chloroform (3: 2) wash-out; Collect elutriant; Decompression and solvent recovery is also dry, gets coarse crystallization, adds the dehydrated alcohol recrystallization; Washing; Be drying to obtain 1.33g, it is 92.5% that HPLC detects purity.
Embodiment 2
Get Ligusticum wallichii rhizome meal 100g, add 8 times of amount 90% alcohol reflux 3 times, each 1.5 hours; United extraction liquid is evaporated to 1 times of amount of medicinal material volume, refrigerates 16 hours; Filter, filtrating adds the equivalent extracted with diethyl ether, gets ether solution; Add the extraction of equivalent 2mol/L sulfuric acid, the water intaking layer adds saturated limewater and regulates PH9-10; Add the equal amounts of chloroform extraction, get chloroform layer, the reclaim under reduced pressure chloroform is done near; Add the 2mol/L sulfuric acid dissolution, filter, filtrating adds the equal amounts of chloroform extraction; Get chloroform layer, decompression and solvent recovery is done near, adds petroleum ether dissolution; Filter; The reclaim under reduced pressure sherwood oil adds alumina chromatographic column, uses sherwood oil: chloroform (3: 2) wash-out; Collect elutriant; Decompression and solvent recovery is also dry, gets coarse crystallization, adds the dehydrated alcohol recrystallization; Washing; Be drying to obtain 3.46g, it is 91.3% that HPLC detects purity.
Embodiment 3
Get Ligusticum wallichii rhizome meal 100g; Add 6 times of amount 80% alcohol reflux 2 times, each 1.5 hours, united extraction liquid; Be evaporated to 1 times of amount of medicinal material volume; Refrigerate 12 hours, filter, filtrating adds the equivalent extracted with diethyl ether; Get ether solution; Add the extraction of equivalent 2mol/L sulfuric acid, the water intaking layer adds saturated NaHCO
3Regulate PH9-10; Add the equal amounts of chloroform extraction, get chloroform layer, the reclaim under reduced pressure chloroform is done near; Add the 2mol/L sulfuric acid dissolution; Filter, filtrating adds the equal amounts of chloroform extraction, gets chloroform layer; Decompression and solvent recovery is done near; Add petroleum ether dissolution, filter the reclaim under reduced pressure sherwood oil; Add alumina chromatographic column; Use sherwood oil: chloroform (3: 2) wash-out, collect elutriant, decompression and solvent recovery is also dry; Get coarse crystallization; Add the dehydrated alcohol recrystallization, wash, be drying to obtain 2.13g, it is 98.3% that HPLC detects purity.
Claims (4)
1. the process for extracting of a Ligustrazine is characterized in that described method comprises the following steps:
1) alcohol extracting: get Ligusticum wallichii rhizome meal, add 3-8 and doubly measure the 50-90% alcohol reflux 1-3 time, each 1.5 hours, united extraction liquid was evaporated to 1 times of amount of medicinal material volume, refrigerates 8-16 hour, filters, and gets filtrating;
2) extraction: filtrating adds the equivalent extracted with diethyl ether, gets ether solution, adds the extraction of equivalent 2mol/L sulfuric acid; The water intaking layer adds basic solution and regulates PH9-10, adds the equal amounts of chloroform extraction; Get chloroform layer, the reclaim under reduced pressure chloroform is done near, adds the 2mol/L sulfuric acid dissolution; Filter, filtrating adds the equal amounts of chloroform extraction, gets chloroform layer; Decompression and solvent recovery is done near, adds petroleum ether dissolution, filters; The reclaim under reduced pressure sherwood oil gets medicinal extract;
3) chromatography: add alumina chromatographic column, use sherwood oil: chloroform (3: 2) wash-out, collect elutriant, decompression and solvent recovery is also dry, gets coarse crystallization, adds the dehydrated alcohol recrystallization, washs, is drying to obtain.
2. according to the said process for extracting of claim 1, it is characterized in that the parameter of said refluxing extraction is: add 6 times of amount 80% alcohol heating reflux 2 times, each 1.5 hours.
3. according to the said process for extracting of claim 1, it is characterized in that said basic solution can be a kind of in saturated limewater, saturated sodium bicarbonate, the soda ash solution.
4. according to the said process for extracting of claim 1, the time that it is characterized in that said refrigeration is 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102471171A CN102344417A (en) | 2010-08-06 | 2010-08-06 | Extraction method for ligustrazine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102471171A CN102344417A (en) | 2010-08-06 | 2010-08-06 | Extraction method for ligustrazine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102344417A true CN102344417A (en) | 2012-02-08 |
Family
ID=45543530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102471171A Pending CN102344417A (en) | 2010-08-06 | 2010-08-06 | Extraction method for ligustrazine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102344417A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859642A (en) * | 2016-04-19 | 2016-08-17 | 齐鲁工业大学 | Tetramethylpyrazine extraction and purification method |
| CN106083744A (en) * | 2016-06-23 | 2016-11-09 | 黄增琼 | A kind of method from Semen Podocarpi Macrophylli seed high efficiency extraction separating high-purity ligustrazine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602735A (en) * | 2009-07-01 | 2009-12-16 | 南京泽朗医药科技有限公司 | A kind of preparation method of Ligustrazine |
-
2010
- 2010-08-06 CN CN2010102471171A patent/CN102344417A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602735A (en) * | 2009-07-01 | 2009-12-16 | 南京泽朗医药科技有限公司 | A kind of preparation method of Ligustrazine |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859642A (en) * | 2016-04-19 | 2016-08-17 | 齐鲁工业大学 | Tetramethylpyrazine extraction and purification method |
| CN105859642B (en) * | 2016-04-19 | 2018-07-31 | 齐鲁工业大学 | A kind of method for extraction and purification of Tetramethylpyrazine |
| CN106083744A (en) * | 2016-06-23 | 2016-11-09 | 黄增琼 | A kind of method from Semen Podocarpi Macrophylli seed high efficiency extraction separating high-purity ligustrazine |
| CN106083744B (en) * | 2016-06-23 | 2018-08-14 | 黄增琼 | A method of from podocarpus seed high efficiency extraction separating high-purity ligustrazine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101830849B (en) | Method for preparing simplified high-purity bulleyaconitine A | |
| CN104326981B (en) | A kind of high efficiency extraction separation method of bulleyaconitine A | |
| CN102093175B (en) | Method for extracting quebrachitol from sapindaceae plant lychee and longan | |
| CN106083871A (en) | The method for extraction and purification of hyoscine in a kind of datura flower | |
| CN104666427A (en) | Method for extracting main active components of folium mori | |
| CN107118219B (en) | The method of separating-purifying gelsevirine, koumidine, koumine, gelsemine and furans koumine from elegant jessamine | |
| CN102228515B (en) | Separation and enrichment method of total flavones and total alkaloids of Lotus Plumule | |
| CN102351659B (en) | Method for preparing high-purity magnolol and high-purity honokiol from magnolia officinalis | |
| CN104193758B (en) | A kind of preparation method who extracts wedelolactone class monomeric compound from eclipta | |
| CN101967124A (en) | Separation and purification method for lappaconitine | |
| CN102344417A (en) | Extraction method for ligustrazine | |
| CN103554209B (en) | Method for preparing ginsenoside Rg1 from pseudo-ginseng | |
| CN103694212B (en) | A kind of purification process of Tridemethylsciadopitysin | |
| CN102093345B (en) | Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography | |
| CN103524578B (en) | A kind of method of extraction and isolation paeoniflorin compound from tree peony stamen | |
| CN105111144A (en) | Method of extracting nuciferine from lotus leaves | |
| CN101602735A (en) | A kind of preparation method of Ligustrazine | |
| CN107722080A (en) | A kind of method that ursin is extracted in the leaf from purple bergenia herb | |
| CN108299298A (en) | A kind of method of norisoboldine high efficiency extraction | |
| CN103739648A (en) | Preparation method for mussaendoside U | |
| CN106905339A (en) | A kind of method that capsule of weeping forsythia aglycon is purified from Folium Forsythia | |
| CN104311615B (en) | Method for extracting and separating hyperoside and gossypetin-3-O-beta-D-galactoside from rhododendron przewalskii maxim. leaves | |
| CN102836280A (en) | Folium Lycii total flavone extract and preparation method thereof | |
| CN102603852A (en) | Preparation method of tripterine | |
| CN102631386B (en) | Bupleurum antipyretic and analgesic preparation and technology for preparing same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Suzhou Ruilanbo TCM Technology Development Co., Ltd. Document name: the First Notification of an Office Action |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120208 |