CN1583063B - Extraction of effective components from frankinscene and its preparation and use - Google Patents
Extraction of effective components from frankinscene and its preparation and use Download PDFInfo
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- CN1583063B CN1583063B CN 200410024253 CN200410024253A CN1583063B CN 1583063 B CN1583063 B CN 1583063B CN 200410024253 CN200410024253 CN 200410024253 CN 200410024253 A CN200410024253 A CN 200410024253A CN 1583063 B CN1583063 B CN 1583063B
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- olibanum
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000000605 extraction Methods 0.000 title claims description 29
- 241000717739 Boswellia sacra Species 0.000 claims abstract description 44
- 239000004863 Frankincense Substances 0.000 claims abstract description 44
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000284 extract Substances 0.000 claims abstract description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 9
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 230000003110 anti-inflammatory effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 22
- 239000003814 drug Substances 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000001953 recrystallisation Methods 0.000 claims description 5
- 208000006820 Arthralgia Diseases 0.000 claims description 3
- 208000025747 Rheumatic disease Diseases 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000000552 rheumatic effect Effects 0.000 claims description 3
- 235000003717 Boswellia sacra Nutrition 0.000 claims description 2
- 235000012035 Boswellia serrata Nutrition 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 208000002193 Pain Diseases 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 abstract 1
- 239000012043 crude product Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 210000002784 stomach Anatomy 0.000 description 4
- 241000700159 Rattus Species 0.000 description 3
- 239000006071 cream Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GUGOEEXESWIERI-UHFFFAOYSA-N Terfenadine Chemical compound C1=CC(C(C)(C)C)=CC=C1C(O)CCCN1CCC(C(O)(C=2C=CC=CC=2)C=2C=CC=CC=2)CC1 GUGOEEXESWIERI-UHFFFAOYSA-N 0.000 description 2
- 206010047700 Vomiting Diseases 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000001387 anti-histamine Effects 0.000 description 2
- 239000000739 antihistaminic agent Substances 0.000 description 2
- 230000037396 body weight Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 235000014347 soups Nutrition 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 230000008673 vomiting Effects 0.000 description 2
- 201000000736 Amenorrhea Diseases 0.000 description 1
- 206010001928 Amenorrhoea Diseases 0.000 description 1
- 235000019890 Amylum Nutrition 0.000 description 1
- 208000005171 Dysmenorrhea Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 241001057584 Myrrha Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 231100000540 amenorrhea Toxicity 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000002683 foot Anatomy 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 210000000548 hind-foot Anatomy 0.000 description 1
- 229960001340 histamine Drugs 0.000 description 1
- 230000002757 inflammatory effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 206010040872 skin infection Diseases 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000010254 subcutaneous injection Methods 0.000 description 1
- 239000007929 subcutaneous injection Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for extracting active component from olibanum, an extract preparation and use. The method comprises the following steps: taking the olibanum(including mix-fried olibanum) as raw material, firstly crushing the raw material into 40-60mesh, putting in an extract device, adding 60-95% of ethanol with the weight of 1-10time of the raw material crude powder, concentrating the leach liquor into an extract; adding 1-10% of sodium bicarbonate solution or 1-5% of sodium hydroxide into the extract, stirring and extracting for 1-5 times under a normal temperature and a normal pressure, each time for 0.5-3h, then allowing to stand for 1-10h, collecting precipitation layer and dissolving with ether; then respectively gradiently extracting by using 1-5% of sodium hydroxide and 1-10% of solidum bicarbonate solution, and adjusting pH of the alkaline water layer to 2-6 by using acid, then extracting for 1-3 times by using ether, reclaiming the ether, and obtaining active component extract crude product of the olibanum. The inventive extracted olibanum extract is used for anti-inflammatory and curing rheumatism impediment pain.
Description
Technical field
The present invention relates to a kind of Chinese herbal medicine extract, particularly a kind of from the Chinese medicine Olibanum method of effective component extracting; The invention still further relates to the purposes of this Olibanum extract and be suitable for the medicament of clinical use.
Background technology
The Chinese crude drug Olibanum has pharmacological action widely, and experiment proof Olibanum has promoting blood circulation and stopping pain, the effect of detumescence and promoting granulation.At present clinical how directly being used as medicine, cooperate other medicines treatment dysmenorrheas, amenorrhea, gastral cavity pain, rheumatic arthralgia, diseases such as traumatic injury and pain and ulcer sore pain with the fecula of Olibanum.Also often cooperating Myrrha to be used to treat the skin infection diabrosis does not close up for a long time.Weak point is to make stomach weak person produce untoward reaction such as vomiting, goes into the decoct soup and is prone to muddiness, is difficult to take.The Olibanum effective ingredient is carried out industrialization extract, be prepared into about can be used for clinical medicament with extract then, inquired into by the relevant expert for a long time.
Summary of the invention
One of the object of the invention provides a kind of method of the Olibanum effective ingredient being carried out the industrialization extraction; Two of the object of the invention provides the purposes of this Olibanum extract and is suitable for the medicament of clinical use.
One of the object of the invention can be realized through following technical measures:
The Olibanum extraction process of effective component is characterized in that:
A, elder generation are broken into coarser powder with frankincense powder, add the ethanol of 1～10 times of amount 60～95%, lixiviate 1～3 time, and lixiviating solution gets extractum after concentrating;
B, add 1～10% sodium bicarbonate solution or 1～5% to extractum sodium hydroxide solution in normal temperature and pressure with stir extraction down 1～5 time, each 0.5～3 hour, after left standstill 1～10 hour, the collecting precipitation layer also dissolves with ether;
C, more respectively with 1～5% sodium hydroxide solution, 1～10% sodium bicarbonate solution gradient extraction, with acid the aqueous alkali layer is transferred pH=2～6 then, ether is reclaimed in reuse ether extraction 1～3 time, Olibanum effective component extracts bullion.
One of the object of the invention also can be realized through following technical measures:
Olibanum effective component extracts bullion with dehydrated alcohol or acetone solvent recrystallization, is got Olibanum effective component extracts elaboration; Extraction temperature is 2～80 ℃, and each extraction time is 1～48 hour.
Two of the object of the invention can be realized through following technical measures:
The Olibanum extract that the present invention extracts is used for antiinflammatory, the treatment rheumatic arthralgia.Olibanum extract is added proper auxiliary materials, process said various preparations on the pharmaceutics, wherein said preparation is meant oral formulations and injection.
Zoopery: getting body weight is 30 of 150～250g rats, and the male and female dual-purpose is divided into 3 groups immediately, 10 every group.Experimental group is irritated stomach respectively and is given Olibanum extract 0.5g/kg and 1g/kg body weight, and the normal control group is irritated stomach and given the equivalent normal saline, every day twice, continuous 7 days.Survey every Mus left hind paw normal volume with drainage.1h after the last administration, the rear solid end subcutaneous injection 0.2% histamine 0.1ml that stands on tiptoe in the rat left and right sides behind each measuring jaw volume of 0.5h, 1h, 2h, 4h and 6h 1 time, calculates the suppression ratio of Mus pawl swelling degree and experimental group then respectively.Experimental result shows, Olibanum extract can be obviously pressed against swelling, had inflammatory effect due to the remarkable antihistamine rat foot due to the antihistamine.As shown in the table, its antiinflammatory action of 2～4h is the most obvious behind antiinflammatory.
Table:
Method of the present invention has solved that relevant technologies expert makes great efforts for a long time always and the problem about Chinese crude drug Olibanum extracts active ingredients that realization is not arranged, and this method can form industrial sectorization to the Olibanum extracts active ingredients.The present invention is the untoward reaction in capable of reducing using as the effective antiinflammatory medicine, avoids stomach weak person to be prone to cause vomiting, goes into the decoct soup and be prone to muddy and defective such as be difficult to take, for new way has been opened up in the utilization of Olibanum effective ingredient.
The specific embodiment
Embodiment 1:
1, feeds intake: get Olibanum 20kg, be ground into 60 order coarser powder;
2, alcohol extraction: add 70% ethanol 35L the first time, controls 2 ℃ of temperature mercerations and carry 8 hours, adds 70% ethanol 100L for the second time, controls 50 ℃ of temperature, lixiviate 40 hours, and twice lixiviating solution merges, and after concentrating recovery ethanol, gets lixiviate cream 4kg;
3, extraction: 8% sodium bicarbonate solution that in extractum, adds 3 times of weight portions of extractum in normal temperature and pressure with stir extraction down 5 times, each 1 hour, after left standstill collecting precipitation layer and 2 hours with the ether dissolution of 0.5 times of weight portion of the beds of precipitation; Add 2% sodium bicarbonate solution of 3 times of weight portions, the 5% sodium hydroxide solution gradient pH extract and separate that the back adds 0.5 times of weight portion more earlier; With hydrochloric acid aqueous alkali layer pH value is adjusted to 5; And then to the ether that wherein adds 1 times of weight portion; Extract repeatedly 3 times, reclaim ether, the gained extract is white or faint yellow deposition.
4, extract is used acetone recrystallization, get Olibanum effective component extracts 1.2Kg.
Embodiment 2:
1, feeds intake: get Olibanum 20kg, be ground into 40 order coarser powder;
2, alcohol extraction: add 90% ether 180L for the first time, control 70 ℃ of temperature lixiviates 4 hours, add 80% ethanol 100L for the second time; Control 40 ℃ of temperature, lixiviate 10 hours adds 70% ethanol 100L for the third time; Control 10 ℃ of temperature; Lixiviate 2 hours, three times lixiviating solution merges, and after concentrating recovery ethanol, gets lixiviate cream 4kg;
3, extraction: 4% sodium hydroxide solution that in extractum, adds 0.5 times of weight portion of extractum in normal temperature and pressure with stir extraction down 3 times, each 2.5 hours, after left standstill collecting precipitation layer and 9 hours with the ether dissolution of 3 times of weight portions of the beds of precipitation; Add 9% sodium bicarbonate solution of 0.5 times of weight portion, the 1% sodium hydroxide solution gradient pH extract and separate that the back adds 4 times of weight portions more earlier; With sulphuric acid aqueous alkali layer pH value is adjusted to 2; And then to the ether that wherein adds 3 times of weight portions; Ether is reclaimed in the extraction back, and the gained extract is white or faint yellow deposition.
4, extract is used the dehydrated alcohol recrystallization, get Olibanum effective component extracts 1.23Kg.
Embodiment 3:
1, feeds intake: get Olibanum 20kg, be ground into 50 order coarser powder;
2, alcohol extraction: add 90% petroleum ether 60L, control 70 ℃ of temperature lixiviates 4 hours, collect lixiviating solution, after concentrating recovery ethanol, get lixiviate cream 3.8kg;
3, extraction: 2% sodium hydroxide solution that in extractum, adds 2 times of weight portions of extractum in normal temperature and pressure with stir extraction down 1 time, each 1 hour, after left standstill collecting precipitation layer and 5 hours with the ether dissolution of 2 times of weight portions of the beds of precipitation; Add 9% sodium bicarbonate solution of 3 times of weight portions, the 3% sodium hydroxide solution gradient pH extract and separate that the back adds 3 times of weight portions more earlier; With sulphuric acid aqueous alkali layer pH value is adjusted to 3; And then to the ether that wherein adds 2 times of weight portions; Ether is reclaimed in the extraction back, and the gained extract is white or faint yellow deposition.
4, extract is used the dehydrated alcohol recrystallization, get Olibanum effective component extracts 1.2Kg.
Embodiment 4:
Get Olibanum effective component extracts 600g, add microcrystalline Cellulose 100g, amylum pregelatinisatum 100g, carboxymethyl starch sodium 24g, Pulvis Talci 8g, magnesium stearate 8g make binding agent with dehydrated alcohol, are prepared into granule by the equivalent incremental method, and tabletting gets the Olibanum tablet.
Claims (6)
1. Olibanum extraction process of effective component is characterized in that:
A, elder generation are broken into coarser powder with frankincense powder, add the ethanol of 1～10 times of amount 60～95%, lixiviate 1～3 time, and lixiviating solution gets extractum after concentrating;
B, add 1～10% sodium bicarbonate solution or 1～5% to extractum sodium hydroxide solution in normal temperature and pressure with stir extraction down 1～5 time, each 0.5～3 hour, after left standstill 1～10 hour, the collecting precipitation layer also dissolves with ether;
C, more respectively with 1～5% sodium hydroxide solution, 1～10% sodium bicarbonate solution gradient extraction, with acid the aqueous alkali layer is transferred pH=2～6 then, ether is reclaimed in reuse ether extraction 1～3 time, Olibanum effective component extracts bullion.
2. Olibanum extraction process of effective component according to claim 1 is characterized in that Olibanum effective component extracts bullion with dehydrated alcohol or acetone solvent recrystallization, Olibanum effective component extracts elaboration.
3. Olibanum extraction process of effective component according to claim 1 is characterized in that step a is divided into twice with the ethanol lixiviate, and extraction temperature is 2 ℃ for the first time, and extraction temperature is 50 ℃ for the second time, and each extraction time is 1～48 hour.
4. the purposes of Olibanum effective ingredient in the medicine of preparation antiinflammatory and treatment rheumatic arthralgia that makes according to arbitrary method in the claim 1～3.
5. the preparation that the Olibanum effective ingredient that makes according to arbitrary method in the claim 1～3 prepares is characterized in that described Olibanum effective ingredient is added proper auxiliary materials to be processed.
6. according to the said preparation of claim 5, it is characterized in that it being oral formulations or injection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410024253 CN1583063B (en) | 2004-06-10 | 2004-06-10 | Extraction of effective components from frankinscene and its preparation and use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410024253 CN1583063B (en) | 2004-06-10 | 2004-06-10 | Extraction of effective components from frankinscene and its preparation and use |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1583063A CN1583063A (en) | 2005-02-23 |
| CN1583063B true CN1583063B (en) | 2012-03-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410024253 Expired - Lifetime CN1583063B (en) | 2004-06-10 | 2004-06-10 | Extraction of effective components from frankinscene and its preparation and use |
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| Country | Link |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100569245C (en) * | 2005-06-02 | 2009-12-16 | 成都中医药大学 | The purposes of Olibanum in the medicine of preparation treatment gout |
| CN101775058B (en) * | 2009-01-08 | 2012-07-18 | 凌沛学 | Preparation and application of pharmaceutical preparation of 11-carbonyl-betal- acetyl mastic acid and derivatives thereof extracted from frankincense |
| MY173288A (en) * | 2010-03-15 | 2020-01-13 | Laila Nutraceuticals | Boswellia oil, its fractions and compositions for enhancing brain function |
| ITRM20120453A1 (en) * | 2012-09-21 | 2014-03-22 | Aboca Spa Societa Agricola | NEW INCENSE EXTRACTS AND THEIR USES. |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0755940A1 (en) * | 1995-04-13 | 1997-01-29 | Council of Scientific and Industrial Research | Boswellic acid compositions and preparation thereof |
-
2004
- 2004-06-10 CN CN 200410024253 patent/CN1583063B/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0755940A1 (en) * | 1995-04-13 | 1997-01-29 | Council of Scientific and Industrial Research | Boswellic acid compositions and preparation thereof |
Non-Patent Citations (2)
| Title |
|---|
| 崔锐等.乳香化学和药理的研究进展.《中国药学杂志》.2003,(第06期), * |
| 沈红等.乳香、没药提取工艺可行性研究.《南京中医药大学学报(自然科学版)》.2003,(第05期), * |
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