CN101348513A - Ganoderic acid extraction method and preparation of soft capsule of ganoderic acid - Google Patents
Ganoderic acid extraction method and preparation of soft capsule of ganoderic acid Download PDFInfo
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- CN101348513A CN101348513A CNA2007101386682A CN200710138668A CN101348513A CN 101348513 A CN101348513 A CN 101348513A CN A2007101386682 A CNA2007101386682 A CN A2007101386682A CN 200710138668 A CN200710138668 A CN 200710138668A CN 101348513 A CN101348513 A CN 101348513A
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- 238000000605 extraction Methods 0.000 title claims abstract description 31
- 239000007901 soft capsule Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 229930182735 Ganoderic acid Natural products 0.000 title abstract 8
- RDMQPKIDHAFXKA-JNORPAGFSA-N Ganoderic Acid Am1 Chemical compound C([C@@]12C)C[C@H](O)C(C)(C)[C@@H]1CC(=O)C1=C2C(=O)C[C@]2(C)[C@@H]([C@@H](CC(=O)CC(C)C(O)=O)C)CC(=O)[C@]21C RDMQPKIDHAFXKA-JNORPAGFSA-N 0.000 title abstract 7
- 239000000284 extract Substances 0.000 claims abstract description 38
- 241000222336 Ganoderma Species 0.000 claims abstract description 27
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 230000001351 cycling effect Effects 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 210000000582 semen Anatomy 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 abstract 3
- 238000009833 condensation Methods 0.000 abstract 2
- 230000005494 condensation Effects 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 2
- 238000010979 pH adjustment Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- LWPLEHFGBRFRKI-CQKTXKLZSA-N Ganoderic acid B Natural products C[C@H](CC(=O)C[C@H](C)C(=O)O)[C@H]1CC(=O)[C@@]2(C)C3=C(C(=O)C[C@]12C)[C@@]4(C)CC[C@H](O)C(C)(C)[C@H]4C[C@@H]3O LWPLEHFGBRFRKI-CQKTXKLZSA-N 0.000 description 1
- LWPLEHFGBRFRKI-NBCWKOIPSA-N Ganoderic acid B Chemical compound C([C@@]12C)C[C@H](O)C(C)(C)[C@@H]1C[C@H](O)C1=C2C(=O)C[C@]2(C)[C@@H]([C@@H](CC(=O)C[C@@H](C)C(O)=O)C)CC(=O)[C@]21C LWPLEHFGBRFRKI-NBCWKOIPSA-N 0.000 description 1
- IEDDICKFTXIWIP-UHFFFAOYSA-N Ganoderic acid D Natural products CC(CC(=O)CCC1CC(=O)C2(C)C3=C(C(=O)CC12C)C4(C)CCC(=O)C(C)(C)C4CC3O)C(=O)O IEDDICKFTXIWIP-UHFFFAOYSA-N 0.000 description 1
- 240000008397 Ganoderma lucidum Species 0.000 description 1
- 235000001637 Ganoderma lucidum Nutrition 0.000 description 1
- AKWNYHCILPEENZ-GESKOEBASA-N Ganosporeric acid A Chemical compound C([C@@]12C)CC(=O)C(C)(C)C1CC(=O)C1=C2C(=O)C(=O)[C@]2(C)[C@@H]([C@@H](CC(=O)C[C@@H](C)C(O)=O)C)CC(=O)[C@]21C AKWNYHCILPEENZ-GESKOEBASA-N 0.000 description 1
- AKWNYHCILPEENZ-UHFFFAOYSA-N Ganosporeric acid A Natural products CC12CCC(=O)C(C)(C)C1CC(=O)C1=C2C(=O)C(=O)C2(C)C(C(CC(=O)CC(C)C(O)=O)C)CC(=O)C21C AKWNYHCILPEENZ-UHFFFAOYSA-N 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 231100000215 acute (single dose) toxicity testing Toxicity 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000011047 acute toxicity test Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- VVXZWUASDACSNQ-UHFFFAOYSA-N ganoderic acid C Natural products CC12CCC(O)C(C)(C)C1CC(O)C1=C2C(=O)CC2(C)C(C(CC(=O)CC(C)C(O)=O)C)CC(O)C21 VVXZWUASDACSNQ-UHFFFAOYSA-N 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 229960001340 histamine Drugs 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 231100001252 long-term toxicity Toxicity 0.000 description 1
- VZYPWBVGOUSGOD-KEUIGMMSSA-N lucidenic acid A Natural products COC(=O)CC[C@@H](C)[C@H]1CC[C@@]2(C)C3=C(C(=O)C[C@]12C)[C@@]4(C)CCC(=O)C(C)(C)[C@@H]4C[C@@H]3O VZYPWBVGOUSGOD-KEUIGMMSSA-N 0.000 description 1
- INIPQDKLXQHEAJ-RGGGUVNYSA-N lucidenic acid a Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@H]1C[C@H](O)C1=C2C(=O)C[C@]2(C)[C@@H]([C@@H](CCC(O)=O)C)CC(=O)[C@]21C INIPQDKLXQHEAJ-RGGGUVNYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003716 rejuvenation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 235000015961 tonic Nutrition 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 229960000716 tonics Drugs 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000820 toxicity test Toxicity 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting ganoderic acid and a method preparing soft capsules of the ganoderic acid. The method for extracting the ganoderic acid comprises the following steps that entities of ganoderic seeds are made into refined powder of ganoderma; the powder is extracted with absolute ethanol and subsequently extracted with ultrasound to obtain a material liquid; the material liquid is filtered and undergoes decompressed condensation to obtain a black concrete extract; the black concrete extract undergoes recycled extractions with ultrasound and then an alkali extraction ,to obtain a combined yellow extraction liquid which undergoes pH adjustment and cycles of extractions with chloroform/ultrasound; and then the chloroform layer undergoes decompressed condensation and drying to obtain a yellow solid powder which is the extract of the ganoderic acid, the extract is used for the preparation of the soft capsule of the ganoderic acid. The method for extracting ganoderic acids has the advantages of low cost and high efficiency.
Description
Technical field
The present invention relates to a kind of Ganodenic acid healthcare products, relate in particular to a kind of extraction and preparation of soft capsule method thereof of Ganodenic acid.
Background technology
Along with growth in the living standard, people's self health care and disease prevention consciousness are strengthened gradually, and various health-care products arise at the historic moment.Glossy ganoderma is as a kind of famous and precious herbal medicine, have strengthen the body resistance to consolidate the constitution, effect such as strengthening by means of tonics, can reducing blood-fat, hypoglycemic, protect the liver, anticancer and improve immunizing power, the exploitation that is used for healthcare products has very vast market prospect.
Glossy ganoderma contains the number of chemical composition, and wherein Ganodenic acid has the intensive pharmacologically active, has pain relieving, calmness, inhibition histamine to discharge, detoxify, protect the liver, kill functions such as tumour cell.In the Ganoderma sporophore total triterpenes content be about 1.5%, the market supply of Ganoderma sporophore is abundant, price is Ganoderma spore powder about one of eight parts, and do not need the special wall breaking technology of Ganoderma spore.Thereby, from Ganoderma sporophore, extract Ganodenic acid and be prepared into the soft capsule of easy absorption, have bigger market potential.
At present, there is the cost height in the extraction of Ganodenic acid, the defective that percentage allocation is low, then disclose a kind of utilization as Chinese patent ZL96116559.6 " the water extraction process method of a kind of high reactivity ganoderan and high-content Ganodenic acid " and under the decompression cold condition, carried out the poach extraction, carry out freeze thawing treatment after concentrating heating under the low pressure condition again, carry out concentrating for the second time under the low pressure condition method of under reduced pressure, drying, the method for extraction ganoderan and Ganodenic acid again.It is provenance that Chinese patent application CN1687438 " extracting method of high germanium glossy ganoderma polysaccharide and Ganodenic acid " then discloses a kind of glossy ganoderma, after glossy ganoderma separation, purification, rejuvenation, enlarged culturing, carries out inoculation culture, after treating that mycelia is covered with, add entry and pull an oar, filter, static cultivation, drying treatment.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of efficiently, the extracting method of Ganodenic acid cheaply.
The technical scheme that solves the problems of the technologies described above is as follows:
A kind of method of extraction of Ganodenic acid mainly may further comprise the steps:
(1) gets Ganoderma sporophore, carry out superfine grinding, cross 70～150 μ m aperture sieve, make the smart powder of glossy ganoderma;
(2) take by weighing the smart powder of Ganoderma sporophore, add dehydrated alcohol in ultrasonic circulating equipment, circulation limit, limit adds the smart powder of glossy ganoderma, and the ratio of amount is 1: 7～9 between smart powder (g) of glossy ganoderma and the dehydrated alcohol (mL), 28 ℃～32 ℃ of extraction temperatures, speed of circulation is 15～30r/s;
(3) step (2) is used the ultrasonic wave lixiviate after finishing, and ultrasonic power 700～1000W extracts, and obtains feed liquid;
(4) filter, feed liquid is evaporated to dried black medicinal extract;
(5) black medicinal extract is dissolved in chloroform, adds the equivalent saturated sodium bicarbonate solution again and carry out the ultrasonic wave cycling extraction;
(6) saturated sodium bicarbonate extracts 2-3 time, merges the yellow alkali extract that obtains, and regulates pH to 4.00 under cycling condition;
(7) acidizing fluid extracts 1-3 time with the chloroform ultrasonic circulating, and chloroform layer concentrating under reduced pressure, drying get faint yellow powdery solid and be the Ganodenic acid extract.
Be preferably: in the step (3), extraction conditions is 1-5s, and gap 0.5-1.5s, omnidistance extraction time are 25～40min.
In the step (5), speed of circulation is 15～30r/s, extraction 15min, 28 ℃～32 ℃, power 700～1000W, work 3s, gap 1s.
In the step (6), regulate pH with the cold hydrochloric acid of 6mol/L.
Another technical issues that need to address of the present invention are, will extract the method that further is prepared into the Ganodenic acid soft capsule behind the Ganodenic acid according to the said extracted method.
A kind of method for preparing the Ganodenic acid soft capsule, its step mainly is:
Extract Ganodenic acid according to the described extracting method of claim 1-4, the Ganodenic acid extract is crossed 70～150 μ m aperture sieve, Ganodenic acid extract after sieving and Semen Maydis oil are 1: 1～1.5 mixed by weight, grind well with colloidal mill, get content and prepare the Ganodenic acid soft capsule with pressing (compacting of rotation rolling capsule machine).
The present invention adopts the ultrasonic circulating combination technique to extract Ganodenic acid from Ganoderma sporophore, chmice acute toxicity test, mouse sperm deformity experiment, 30 days toxicity tests of rat show that the Ganodenic acid extract does not have toxicity, and the soft capsule of being made by the Ganodenic acid extract has safe and reliable, lower-cost characteristics.Be easy to get calmly, extract Ganodenic acid and make soft capsule in the Ganoderma sporophore with low cost, the extraction yield of total Ganodenic acid is about 80%, and total extraction time is about 3h, every heavy 0.5g of the Ganodenic acid soft capsule of preparation, and cost is about 2 yuan/.
Embodiment
Embodiment 1
Get dustless, as not have the first-class log cultivation of going mouldy Ganoderma sporophore 1000g, carry out superfine grinding, cross 120 μ m aperture sieve, make the smart powder of glossy ganoderma.Take by weighing the smart powder 300g of Ganoderma sporophore, add the 2300mL dehydrated alcohol in ultrasonic circulating equipment, circulation limit, limit adds the smart powder of Ganoderma sporophore, 30 ℃ of extraction temperatures, and speed of circulation is 30r/s.Feed intake and finish the back and use the ultrasonic wave lixiviate, ultrasonic power 800W, extraction 3s (second), gap 1s, omnidistance extraction time be 30min (minute).Filter, feed liquid is evaporated to dried black medicinal extract.Black medicinal extract is dissolved in chloroform, and the saturated sodium bicarbonate solution that adds equivalent again carries out ultrasonic wave circulation 30r/s, extraction 15min, 30 ℃, power 800W, work 3s, gap 1s.And then, merge yellow alkali extract three times with saturated sodium bicarbonate extraction 2 times, under cycling condition, transfer pH to 4.00 with the cold hydrochloric acid of 6mol/L.Then, acidizing fluid extracts 2 times with the chloroform ultrasonic circulating, and chloroform layer concentrating under reduced pressure, drying get faint yellow powdery solid and be the Ganodenic acid extract.
Identify and assay extract obtained, find that wherein red Ganoderma lucidum spore acid A (ganosporericacid A) is 0.11%, red sesame acid A (lucidenic acid A) is 0.13%, Ganodenic acid B (ganoderic acid B) is 0.43%, Ganodenic acid C (ganoderic acid C) is 0.16%.The Ganodenic acid extract is carried out acute, long term toxicity test, prove nontoxic.
Get above-mentioned Ganodenic acid extract and cross 100 μ m aperture sieve, with Semen Maydis oil by weight than the mixed that is 1: 1, with colloidal mill homogenize 30min, get content after the homogenize with rotation rolling capsule machine compacting soft capsule.Every heavy 0.5g, cost is about 2 yuan/.
Above-listed detailed description is at the specifying of one of the present invention possible embodiments, and this embodiment is not in order to limiting claim of the present invention, and the equivalence that all the present invention of disengaging do is implemented or change, all should be contained in the claim of this case.
Claims (5)
1. the method for the extraction of a Ganodenic acid is characterized in that, mainly may further comprise the steps:
(1) gets Ganoderma sporophore, carry out superfine grinding, cross 70～150 μ m aperture sieve, make the smart powder of glossy ganoderma;
(2) take by weighing the smart powder of glossy ganoderma, add dehydrated alcohol in ultrasonic circulating equipment, circulation limit, limit adds the smart powder of glossy ganoderma, and the ratio of amount is 1: 7～9 between smart powder (g) of glossy ganoderma and the dehydrated alcohol (mL), 28 ℃～32 ℃ of extraction temperatures, and speed of circulation is 15～30r/s;
(3) step (2) is used the ultrasonic wave lixiviate after finishing, and ultrasonic power 700～1000W extracts, and obtains feed liquid;
(4) filter and to be evaporated to dried black medicinal extract after the feed liquid;
(5) black medicinal extract is dissolved in chloroform, adds the equivalent saturated sodium bicarbonate solution again and carry out the ultrasonic wave cycling extraction;
(6) saturated sodium bicarbonate extracts 2-3 time, merges the yellow alkali extract that obtains, and regulates pH to 4.00 under cycling condition;
(7) acidizing fluid extracts 2-3 time with the chloroform ultrasonic circulating, and chloroform layer concentrating under reduced pressure, drying get faint yellow powdery solid and be the Ganodenic acid extract.
2. the method for the extraction of Ganodenic acid according to claim 1 is characterized in that,
In the step (3), extraction conditions is 1-5s, and gap 0.5-1.5s, omnidistance extraction time are 25～40min.
3. the method for the extraction of Ganodenic acid according to claim 1 is characterized in that,
In the step (5), speed of circulation is 15～30r/s, extraction 15min, 28 ℃～32 ℃, power 700～1000W, work 3s, gap 1s.
4. the method for the extraction of Ganodenic acid according to claim 1 is characterized in that,
In the step (6), regulate pH with the cold hydrochloric acid of 6mol/L.
5. one kind prepares Ganodenic acid preparation of soft capsule method, and its step mainly is:
(A) extract Ganodenic acid according to the described extracting method of claim 1-4;
(B) the Ganodenic acid extract that extracts in the step (A) is crossed 70～150 μ m aperture sieve, Ganodenic acid extract after sieving and Semen Maydis oil are 1: 1～1.5 mixed by weight, grind well with colloidal mill;
(C) content that grinds well in the step (B) is prepared the Ganodenic acid soft capsule with pressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101386682A CN101348513A (en) | 2007-07-18 | 2007-07-18 | Ganoderic acid extraction method and preparation of soft capsule of ganoderic acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101386682A CN101348513A (en) | 2007-07-18 | 2007-07-18 | Ganoderic acid extraction method and preparation of soft capsule of ganoderic acid |
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| CN101348513A true CN101348513A (en) | 2009-01-21 |
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| CNA2007101386682A Pending CN101348513A (en) | 2007-07-18 | 2007-07-18 | Ganoderic acid extraction method and preparation of soft capsule of ganoderic acid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101623502B (en) * | 2009-05-08 | 2011-06-08 | 华东理工大学 | Preparation method of Ganodenic acid monomer Me cyclodextrin inclusion compound and of oral solid preparation |
| CN103550264A (en) * | 2013-11-01 | 2014-02-05 | 王颖 | Method for extracting Ganoderma lucidum essences |
| CN103724389A (en) * | 2013-12-23 | 2014-04-16 | 福建仙芝楼生物科技有限公司 | Method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F |
| CN104324057A (en) * | 2014-10-20 | 2015-02-04 | 三生源生物科技（天津）有限公司 | Method for extracting triterpenoids |
| CN104805170A (en) * | 2015-02-03 | 2015-07-29 | 安发（福建）生物科技有限公司 | Submerged fermentation and extraction process method for ganoderma triterpene acid |
| CN108003211A (en) * | 2017-12-22 | 2018-05-08 | 福建农大菌草技术开发公司 | A kind of method of quick separating ganoderic acid in accessory substance from ganoderma lucidum |
-
2007
- 2007-07-18 CN CNA2007101386682A patent/CN101348513A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101623502B (en) * | 2009-05-08 | 2011-06-08 | 华东理工大学 | Preparation method of Ganodenic acid monomer Me cyclodextrin inclusion compound and of oral solid preparation |
| CN103550264A (en) * | 2013-11-01 | 2014-02-05 | 王颖 | Method for extracting Ganoderma lucidum essences |
| CN103550264B (en) * | 2013-11-01 | 2015-07-22 | 王颖 | Method for extracting Ganoderma lucidum essences |
| CN103724389A (en) * | 2013-12-23 | 2014-04-16 | 福建仙芝楼生物科技有限公司 | Method for separating and preparing anti-tumor components ganoderic acid C1 and ganoderic acid F |
| CN103724389B (en) * | 2013-12-23 | 2015-09-02 | 福建仙芝楼生物科技有限公司 | The method of antineoplastic component ganoderic acid C 1 and Ganodenic acid F is prepared in a kind of separation |
| CN104324057A (en) * | 2014-10-20 | 2015-02-04 | 三生源生物科技（天津）有限公司 | Method for extracting triterpenoids |
| CN104805170A (en) * | 2015-02-03 | 2015-07-29 | 安发（福建）生物科技有限公司 | Submerged fermentation and extraction process method for ganoderma triterpene acid |
| CN104805170B (en) * | 2015-02-03 | 2018-06-01 | 安发（福建）生物科技有限公司 | Ganodenic acid acid submerged fermentation process for extracting |
| CN108003211A (en) * | 2017-12-22 | 2018-05-08 | 福建农大菌草技术开发公司 | A kind of method of quick separating ganoderic acid in accessory substance from ganoderma lucidum |
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