CN1321638C - Ligustilide oil and its preparation - Google Patents
Ligustilide oil and its preparation Download PDFInfo
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- CN1321638C CN1321638C CNB200510105552XA CN200510105552A CN1321638C CN 1321638 C CN1321638 C CN 1321638C CN B200510105552X A CNB200510105552X A CN B200510105552XA CN 200510105552 A CN200510105552 A CN 200510105552A CN 1321638 C CN1321638 C CN 1321638C
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- Prior art keywords
- ligustilide
- oil
- petroleum ether
- rhizoma chuanxiong
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- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical compound C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 title claims abstract description 100
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000003921 oil Substances 0.000 claims abstract description 78
- 239000003208 petroleum Substances 0.000 claims abstract description 45
- 239000007901 soft capsule Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 239000007902 hard capsule Substances 0.000 claims abstract description 8
- 239000003480 eluent Substances 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 235000019198 oils Nutrition 0.000 claims description 74
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 19
- 238000000194 supercritical-fluid extraction Methods 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 7
- 240000008415 Lactuca sativa Species 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 235000012045 salad Nutrition 0.000 claims description 6
- 235000019482 Palm oil Nutrition 0.000 claims description 5
- 239000008273 gelatin Substances 0.000 claims description 5
- 229920000159 gelatin Polymers 0.000 claims description 5
- 239000002540 palm oil Substances 0.000 claims description 5
- 239000000546 pharmaceutical excipient Substances 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims description 3
- 239000002775 capsule Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000010779 crude oil Substances 0.000 abstract 7
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 239000013558 reference substance Substances 0.000 description 8
- 229960001866 silicon dioxide Drugs 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 201000006474 Brain Ischemia Diseases 0.000 description 4
- 206010008120 Cerebral ischaemia Diseases 0.000 description 4
- 206010008118 cerebral infarction Diseases 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UIAGMCDKSXEBJQ-IBGZPJMESA-N 3-o-(2-methoxyethyl) 5-o-propan-2-yl (4s)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate Chemical compound COCCOC(=O)C1=C(C)NC(C)=C(C(=O)OC(C)C)[C@H]1C1=CC=CC([N+]([O-])=O)=C1 UIAGMCDKSXEBJQ-IBGZPJMESA-N 0.000 description 3
- 241000699670 Mus sp. Species 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 229960000715 nimodipine Drugs 0.000 description 3
- 150000003904 phospholipids Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000029058 respiratory gaseous exchange Effects 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 238000006424 Flood reaction Methods 0.000 description 1
- 238000012449 Kunming mouse Methods 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000003727 cerebral blood flow Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007912 intraperitoneal administration Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The present invention discloses ligustilide oil, wherein the content of ligustilide in the oil is from 50 to 60%. The ligustilide oil is obtained by the following technology: firstly, crude oil of Chuanxiong rhizome is prepared; secondly, petroleum ether with a boiling range of 30 to 60 DEG C or 60 to 90 DEG C is added to the crude oil, and a petroleum ether solution is obtained, wherein the content of the petroleum ether is five times of that of the crude oil; thirdly, silica gel with 80 to 200 meshes is added to the crude oil, and is loaded into a short column for treating the petroleum ether solution, wherein the content of the silica gel is 1.6 to tiwce of that of the crude oil, and the proportion of the diameter to the height of the short column is 1:1.3 to 1:1.5; fourthly, after the petroleum ether solution depletes in the column, petroleum ether is used for washing the column, wherein the content of the petroleum ether is once or twice of that of the crude oil; fifthly, the column is washed by petroleum ether with the content of 12 to 16 times of that of the crude oil, and eluent is collected. The eluent is concentrated to the exhaust of the petroleum ether, and the ligustilide oil is obtained. The present invention can be used for preparing soft capsule preparations and liquid hard capsule preparations. The present invention has the advantages of high ligustilide content, low energy consumption, recycled solvents and silica gel, low cost, high ligustilide yield, convenient technological operation and simple required equipment. The present invention is suitable for industrialized mass production.
Description
The application is for dividing an application, and the application number of original application is 03153586.0, and the applying date is on August 18th, 2003.
Technical field
The present invention relates to a kind of ligustilide oil and preparation thereof, refer to especially a kind ofly from Rhizoma Chuanxiong, to extract, technology system, the ligustilide oil after the enrichment and the preparation thereof of enrichment ligustilide, belong to modern Chinese traditional medicine field.
Background technology
Ligustilide is one of main effective ingredient in the Rhizoma Chuanxiong, has anti-cerebral ischemia and improves cerebral blood flow, is used for the treatment of the various symptoms that caused by cerebral ischemia.
Because the pure product of ligustilide are unstable, all use at present with the form of Rhizoma Chuanxiong oil, the method of Rhizoma Chuanxiong oil available water steam distillation obtains, ligustilide content can reach more than 50% in the Rhizoma Chuanxiong oil that obtains from Rhizoma Chuanxiong, but because production process needs long Steam Heating (reaching several days) energy resource consumption very big, gained Rhizoma Chuanxiong oil collecting amount is very low, and the yield of ligustilide is lower.The also available CO of Rhizoma Chuanxiong oil
2Supercritical extraction method extracts, but ligustilide content in the gained Rhizoma Chuanxiong oil is used the HPLC internal mark method determination with ligustilide reference substance (purity reaches more than 98%), and its content has only 5～9%, and slightly oily with the Rhizoma Chuanxiong of 85% ethanol room temperature dipping gained, its ligustilide content only is 14%～18%.Therefore, study a kind of simplely, the process of enriching that can make ligustilide content reach the ligustilide oil more than 50% has Practical significance.
Summary of the invention
The purpose of this invention is to provide a kind of technology of enrichment ligustilide and the ligustilide oil that obtains.
Another object of the present invention provides the Rhizoma Ligustici pharmaceutical preparation of being rich in ligustilide.
For achieving the above object, the present invention is by the following technical solutions:
A kind of ligustilide oil, the content of ligustilide is 50～60% in the oil, is obtained by following prepared:
(1) the preparation Rhizoma Chuanxiong is slightly oily;
(2) overstriking oil 5 times of amounts, boiling ranges are the petroleum ether of 30～60 ℃ or 60 ℃～90 ℃, must petroleum ether solution;
(3) with 80～200 purpose silica gel of～2 times of amounts of thick oily 1.6 times of amounts, dress up short column, diameter and aspect ratio are 1: 1.3～1: the 1.5 above-mentioned petroleum ether solution of processing;
(4) after petroleum ether solution flows to end, wash post with the petroleum ether of 1～2 times of amount of thick oil in post;
(5) wash post with the petroleum ether of thick oily 12～16 times of amounts, collect eluent, be concentrated into petroleum ether to the greatest extent, promptly get ligustilide oil.
The described method of the thick oil of Rhizoma Chuanxiong for preparing of step (1) is for flooding Rhizoma Chuanxiong or CO with 85% ethanol room temperature
2Supercritical extraction obtains slightly oil of Rhizoma Chuanxiong.
Described 85% ethanol room temperature dipping is meant that the raw material that will contain ligustilide floods 3 times through four times of amount 85% ethanol room temperatures, obtains slightly oil of Rhizoma Chuanxiong.
Described CO
2Supercritical extraction is meant and will contains the raw material of ligustilide through CO
2Supercritical extraction, extraction conditions is: pressure 34.5MPa, 60 ℃ of temperature, modifier ethanol 0.3ml, 3 hours extraction time, the Rhizoma Chuanxiong oil that obtains.
This method is utilized following principle enrichment ligustilide: silica gel adsorption, the applied sample amount of overload.With common upper column quantity down can not the eluting ligustilide low polarity solvent, can separate eliminating than the more weak impurity of ligustilide absorption, the eluting ligustilide, but can not adsorb stronger impurity than ligustilide by eluting, thus reach the purpose of purification enrichment ligustilide.
With the ligustilide oil 25%～50% (its ligustilide content 50%～60%) of enrichment processing back gained, Petiolus Trachycarpi oil 3%～6%, hydrogenated palm oil 3%～6%, phosphatidase 12 %～4% and salad oil 42%～59%.Being mixed with soft capsule content, is rubber with glycerol-gelatin, is pressed into soft capsule, and every soft capsule contains ligustilide and is not less than 25mg and every soft capsule and contains ligustilide and be not less than 50mg.
With the ligustilide oil 20～80% (its ligustilide content 50%～60%) of enrichment processing back gained, fat-soluble excipient such as salad oil 80～20%, fill becomes liquid hard capsule, and every hard capsule contains ligustilide and is not less than 50mg.
The test of pesticide effectiveness shows that this product has anti-cerebral ischemia, is used for the treatment of the various symptoms that caused by cerebral ischemia.
Advantage of the present invention is: the ligustilide oil of back gained is handled in enrichment, and through being standard with the ligustilide reference substance, HPLC measures, and the content of ligustilide reaches 50～60% in the ligustilide oil.Energy low consumption, all technical process except that enrichment process, all is at room temperature to operate; Solvent for use and silica gel can be recycled, and cost is low; Ligustilide yield height; Technological operation is simple; Equipment needed thereby is simple, is suitable for industrialized great production.
Be described further below in conjunction with the preferable specific embodiment.
The specific embodiment
Embodiment 1, be the technology of raw material enrichment ligustilide with the Rhizoma Chuanxiong
One, material and method
1, material:
Rhizoma Chuanxiong: purchase in Tianjin medical material company
Ethanol: purchase in Tianjin Alcohol Plant
Silica gel: purchase in Haiyang Chemical Plant, Qingdao
Petroleum ether: purchase in Tianjin Milky Way chemical reagent work
The ligustilide reference substance: Rhizoma Chuanxiong by silicagel column, obtains grease through alcohol extraction, reaches ligustilide reference substance more than 98% obtaining content on the preparation HPLC, meets the requirement of reference substance.
2, method:
(1) Rhizoma Chuanxiong is flooded 3 times through four times of amount 85% ethanol room temperatures, obtain slightly oil of Rhizoma Chuanxiong;
(2) overstriking oil 5 times of amounts, boiling ranges are 60～90 ℃ petroleum ether, get petroleum ether solution;
(3) with 100～200 purpose silica gel of thick oily 1.8 times of amounts, dress up short column, diameter and aspect ratio are 1: 1.3 above-mentioned petroleum ether solution of processing;
(4) after petroleum ether solution flows to end, wash post with the petroleum ether of 1.5 times of amounts of thick oil in post;
(5) wash post with the petroleum ether of thick oily 12 times of amounts, collect eluent, be concentrated into petroleum ether to the greatest extent, promptly get ligustilide oil.
Two, detection and result:
Through being standard with the ligustilide reference substance, HPLC measures, C
1NPost; Mobile phase is 64% methanol-1% glacial acetic acid; The detection wavelength is 272nm.The content of ligustilide reaches 15～17% in the thick oil of Rhizoma Chuanxiong, ligustilide yield 90～95%; The content of ligustilide reaches 50～60% in the ligustilide oil, ligustilide yield 85%.
Embodiment 2, be the technology of raw material enrichment ligustilide with the Rhizoma Chuanxiong
One, material and method
1, material: with embodiment 1.
2, method:
(1) Rhizoma Chuanxiong is flooded 3 times through four times of amount 85% ethanol room temperatures, obtain slightly oil of Rhizoma Chuanxiong;
(2) overstriking oil 5 times of amounts, boiling ranges are 30～60 ℃ petroleum ether, get petroleum ether solution;
(3) with 80～100 purpose silica gel of thick oily 2 times of amounts, dress up short column, diameter and aspect ratio are 1: 1.5 above-mentioned petroleum ether solution of processing;
(4) after petroleum ether solution flows to end, wash post with the petroleum ether of 2 times of amounts of thick oil in post;
(5) wash post with the petroleum ether of thick oily 16 times of amounts, collect eluent, be concentrated into petroleum ether to the greatest extent, promptly get ligustilide oil.
Two, detection and result:
Through being standard with the ligustilide reference substance, HPLC measures, and the content of ligustilide reaches 17% in the thick oil of Rhizoma Chuanxiong, ligustilide yield 90～95%; The content of ligustilide reaches 50～55% in the ligustilide oil, ligustilide yield 85%.
Embodiment 3, with CO
2The thick oil of the Rhizoma Chuanxiong of supercritical extraction method gained is the technology of raw material enrichment ligustilide
One, material and method
1, material: with embodiment 1.
2, method
(1) with Rhizoma Chuanxiong CO
2Supercritical extraction, CO
2The supercritical extraction condition is: pressure 34.5MPa, and 60 ℃ of temperature, modifier ethanol 0.3ml, 3 hours extraction time, the Rhizoma Chuanxiong that obtains is oil slightly;
(2) overstriking oil 5 times of amounts, boiling ranges are 60～90 ℃ of petroleum ether, get petroleum ether solution;
(3) with 100～200 purpose silica gel of thick oily 1.8 times of amounts, dress up short column, diameter and aspect ratio are 1: 1.4 above-mentioned petroleum ether solution of processing;
(4) after petroleum ether solution flows to end, wash post with the petroleum ether of 2 times of amounts of thick oil in post;
(5) wash post with the petroleum ether of thick oily 14 times of amounts, collect eluent, be concentrated into petroleum ether to the greatest extent, promptly get ligustilide oil.
Two, detection and result:
Through being standard with the ligustilide reference substance, HPLC measures, and the content of ligustilide reaches 8.8% in the thick oil of Rhizoma Chuanxiong; The content of ligustilide reaches 58% in the ligustilide oil, ligustilide yield 80%.
Embodiment 4, be rich in the preparation of ligustilide
One, prescription: ligustilide oil 50%, Petiolus Trachycarpi oil 3%, hydrogenated palm oil 3%, phosphatidase 12 % phospholipid and salad oil 42%.
Two, preparation method:
Being mixed with soft capsule content with formulation, is rubber with glycerol-gelatin, is pressed into soft capsule, and specification is every dress 0.2g content, and every soft capsule contains ligustilide and is not less than 50mg.
Consumption and usage: every day 2 times, each l grain.(fixing tentatively)
Embodiment 5, be rich in the preparation of ligustilide
One, prescription: ligustilide oil 25%, Petiolus Trachycarpi oil 6%, hydrogenated palm oil 6%, phosphatidase 14 % phospholipid and salad oil 59%.
Two, preparation method:
Being mixed with soft capsule content with formulation, is rubber with glycerol-gelatin, is pressed into soft capsule, and specification is every dress 0.2g content, and every soft capsule contains ligustilide and is not less than 25mg.
Consumption and usage: every day 2 times, each 1.(fixing tentatively)
Embodiment 6, be rich in the preparation of ligustilide
One, prescription: ligustilide oil 25%, Petiolus Trachycarpi oil 6%, hydrogenated palm oil 6%, phosphatidase 14 % phospholipid and salad oil 59%.
Two, preparation method:
Being mixed with soft capsule content with formulation, is rubber with glycerol-gelatin, is pressed into soft capsule, and specification is every dress 0.4g content.Every soft capsule contains ligustilide and is not less than 50mg.
Embodiment 7, be rich in the preparation of ligustilide
One, prescription: ligustilide oil 40%, excipient 60%.
Two, preparation method:
With ligustilide oil and fat-soluble excipient mix homogeneously, fill is in hard capsule case.And the employing joint filling material (
5%, PVA1%, ethanol 34%, water 60%) the capsule shells suit place is carried out once or secondary seals, be prepared into liquid hard capsule, every hard capsule contains ligustilide and is not less than 50mg.
Embodiment 8, pharmacodynamic experiment
One, material and method:
1, animal: choose 51 of 22～27g kunming mices, male and female have concurrently, are divided into 5 groups at random, are respectively normal
Matched group, nimodipine matched group, ligustilide line of oils.
2, method: nimodipine is selected intraperitoneal administration, each dosage group selection gastric infusion of ligustilide, and blank group gives the water with volume.Each is organized the mice administration and breaks end fast at the ear rear portion with shear after 1 hour, and clocks immediately.Continue the time of breathing of dehiscing behind the record mice broken end.
Two, result: can obviously prolong after nimodipine contrast, each dosage group mice administration of ligustilide and continue the time of breathing of dehiscing.
Claims (9)
1, a kind of ligustilide oil, the content of ligustilide is 50～60% in the oil, is obtained by following prepared:
(1) the preparation Rhizoma Chuanxiong is slightly oily;
(2) overstriking oil 5 times of amounts, boiling ranges are the petroleum ether of 30～60 ℃ or 60～90 ℃, must petroleum ether solution;
(3) with 80～200 purpose silica gel of～2 times of amounts of thick oily 1.6 times of amounts, dress up short column, diameter and aspect ratio are 1: 1.3～1: the 1.5 above-mentioned petroleum ether solution of processing;
(4) after petroleum ether solution flows to end, wash post with the petroleum ether of 1～2 times of amount of thick oil in post;
(5) wash post with the petroleum ether of thick oily 12～16 times of amounts, collect eluent, be concentrated into petroleum ether to the greatest extent, promptly get ligustilide oil;
Except that enrichment process, all operations at room temperature.
2, a kind of ligustilide oil according to claim 1 is characterized in that: described step (1) prepares the method for the thick oil of Rhizoma Chuanxiong for Rhizoma Chuanxiong is flooded or CO with 85% ethanol room temperature
2Supercritical extraction obtains slightly oil of Rhizoma Chuanxiong.
3, a kind of ligustilide oil according to claim 2 is characterized in that: described 85% ethanol room temperature dipping is meant Rhizoma Chuanxiong is flooded 3 times through four times of amount 85% ethanol room temperatures, obtains slightly oil of Rhizoma Chuanxiong.
4, a kind of ligustilide oil according to claim 2 is characterized in that: described CO
2Supercritical extraction is meant Rhizoma Chuanxiong through CO
2Supercritical extraction, extraction conditions is: pressure 34.5MPa, 60 ℃ of temperature, modifier ethanol 0.3ml, obtains Rhizoma Chuanxiong oil at 3 hours extraction time.
5, a kind of preparation that is rich in ligustilide, it is characterized in that: said preparation is a soft capsule, with glycerol-gelatin is rubber, this soft capsule content contains the ligustilide oil 25～50% after any one described enrichment among the claim 1-4, Petiolus Trachycarpi oil 3%～6%, hydrogenated palm oil 3%～6%, phosphatidase 12 %～4% and salad oil 42%～59%.
6, a kind of preparation that is rich in ligustilide is characterized in that: said preparation is a liquid hard capsule, and this capsule 's content contains the ligustilide oil 20～80% after any one described enrichment among the claim 1-4, fat-soluble excipient 80～20%.
7, preparation according to claim 5 is characterized in that: every of described soft capsule contains ligustilide and is not less than 25mg.
8, preparation according to claim 5 is characterized in that: every of described soft capsule contains ligustilide and is not less than 50mg.
9, preparation according to claim 6 is characterized in that: every of described liquid hard capsule contains ligustilide and is not less than 50mg.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03153586 CN1247564C (en) | 2003-08-18 | 2003-08-18 | Enrichment of ligusticum lactone and its preparations |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03153586 Division CN1247564C (en) | 2003-08-18 | 2003-08-18 | Enrichment of ligusticum lactone and its preparations |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1748676A CN1748676A (en) | 2006-03-22 |
| CN1321638C true CN1321638C (en) | 2007-06-20 |
Family
ID=34597770
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510105552XA Expired - Fee Related CN1321638C (en) | 2003-08-18 | 2003-08-18 | Ligustilide oil and its preparation |
| CN 03153586 Expired - Fee Related CN1247564C (en) | 2003-08-18 | 2003-08-18 | Enrichment of ligusticum lactone and its preparations |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03153586 Expired - Fee Related CN1247564C (en) | 2003-08-18 | 2003-08-18 | Enrichment of ligusticum lactone and its preparations |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN1321638C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321638C (en) * | 2003-08-18 | 2007-06-20 | 天津药物研究院 | Ligustilide oil and its preparation |
| CN102872175A (en) * | 2012-08-24 | 2013-01-16 | 天津中医药大学 | Ligusticum chuanxiong hort extract and preparation method and application thereof |
| CN105079059B (en) * | 2015-09-07 | 2020-03-31 | 宜诺(天津)医药工程有限公司 | Angelica sinensis extract and extraction method thereof |
| CN106138135B (en) * | 2016-08-18 | 2020-09-22 | 四川省中医药科学院 | Medicine for preventing and treating vascular cognitive disorder and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084851A (en) * | 1992-09-30 | 1994-04-06 | 兰州大学 | The synthetic method of Z-ligustilide |
| CN1311008A (en) * | 2000-03-01 | 2001-09-05 | 山东绿叶制药股份有限公司 | Chinese angelica root oil soft capsule and its preparing process |
| US20030165580A1 (en) * | 2002-03-04 | 2003-09-04 | Xinxian Zhao | Safe pharmaceutical composition for treatment and prevention of gynecological disease |
| JP2003289827A (en) * | 2002-04-02 | 2003-10-14 | Osaka Yakuhin Kenkyusho:Kk | Supplement containing japanese parsley extract |
| CN1552702A (en) * | 2003-06-03 | 2004-12-08 | 北京九龙制药厂 | Medicinal use and extraction of cis-ligusticum lactone |
| US20040247698A1 (en) * | 2003-06-04 | 2004-12-09 | Valenzuela Cortes Carmen Maria | Erectile Dysfunction Treatment |
| CN1583735A (en) * | 2003-08-18 | 2005-02-23 | 天津药物研究院 | Enrichment of ligusticum lactone and its preparations |
-
2003
- 2003-08-18 CN CNB200510105552XA patent/CN1321638C/en not_active Expired - Fee Related
- 2003-08-18 CN CN 03153586 patent/CN1247564C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084851A (en) * | 1992-09-30 | 1994-04-06 | 兰州大学 | The synthetic method of Z-ligustilide |
| CN1311008A (en) * | 2000-03-01 | 2001-09-05 | 山东绿叶制药股份有限公司 | Chinese angelica root oil soft capsule and its preparing process |
| US20030165580A1 (en) * | 2002-03-04 | 2003-09-04 | Xinxian Zhao | Safe pharmaceutical composition for treatment and prevention of gynecological disease |
| JP2003289827A (en) * | 2002-04-02 | 2003-10-14 | Osaka Yakuhin Kenkyusho:Kk | Supplement containing japanese parsley extract |
| CN1552702A (en) * | 2003-06-03 | 2004-12-08 | 北京九龙制药厂 | Medicinal use and extraction of cis-ligusticum lactone |
| US20040247698A1 (en) * | 2003-06-04 | 2004-12-09 | Valenzuela Cortes Carmen Maria | Erectile Dysfunction Treatment |
| CN1583735A (en) * | 2003-08-18 | 2005-02-23 | 天津药物研究院 | Enrichment of ligusticum lactone and its preparations |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1583735A (en) | 2005-02-23 |
| CN1247564C (en) | 2006-03-29 |
| CN1748676A (en) | 2006-03-22 |
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