CN104073344A - Extracting method for ganoderma lucidum spore oil - Google Patents
Extracting method for ganoderma lucidum spore oil Download PDFInfo
- Publication number
- CN104073344A CN104073344A CN201410338619.3A CN201410338619A CN104073344A CN 104073344 A CN104073344 A CN 104073344A CN 201410338619 A CN201410338619 A CN 201410338619A CN 104073344 A CN104073344 A CN 104073344A
- Authority
- CN
- China
- Prior art keywords
- ganoderma spore
- ganoderma lucidum
- extraction
- powder
- spore oil
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 30
- 240000008397 Ganoderma lucidum Species 0.000 title abstract description 21
- 235000001637 Ganoderma lucidum Nutrition 0.000 title abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 63
- 239000000843 powder Substances 0.000 claims abstract description 55
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims abstract description 40
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229940046009 vitamin E Drugs 0.000 claims abstract description 21
- 239000011709 vitamin E Substances 0.000 claims abstract description 21
- 229930003427 Vitamin E Natural products 0.000 claims abstract description 20
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000019165 vitamin E Nutrition 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 241000222336 Ganoderma Species 0.000 claims description 118
- 238000000926 separation method Methods 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000003963 antioxidant agent Substances 0.000 abstract description 5
- 235000006708 antioxidants Nutrition 0.000 abstract description 5
- 230000003078 antioxidant effect Effects 0.000 abstract description 4
- 230000000717 retained effect Effects 0.000 abstract description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 abstract 1
- 238000013021 overheating Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- -1 polyose Natural products 0.000 description 8
- 150000003648 triterpenes Chemical class 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 3
- RQOCXCFLRBRBCS-UHFFFAOYSA-N (22E)-cholesta-5,7,22-trien-3beta-ol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CCC(C)C)CCC33)C)C3=CC=C21 RQOCXCFLRBRBCS-UHFFFAOYSA-N 0.000 description 3
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 3
- DNVPQKQSNYMLRS-NXVQYWJNSA-N Ergosterol Natural products CC(C)[C@@H](C)C=C[C@H](C)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)CC[C@]4(C)[C@@H]3CC[C@]12C DNVPQKQSNYMLRS-NXVQYWJNSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- DNVPQKQSNYMLRS-SOWFXMKYSA-N ergosterol Chemical compound C1[C@@H](O)CC[C@]2(C)[C@H](CC[C@]3([C@H]([C@H](C)/C=C/[C@@H](C)C(C)C)CC[C@H]33)C)C3=CC=C21 DNVPQKQSNYMLRS-SOWFXMKYSA-N 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 2
- 230000000259 anti-tumor effect Effects 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010033557 Palpitations Diseases 0.000 description 1
- 241000222341 Polyporaceae Species 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 238000007908 dry granulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 208000013220 shortness of breath Diseases 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000037351 starvation Effects 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening 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
- 238000012546 transfer Methods 0.000 description 1
- 238000007601 warm air drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses an extraction method for ganoderma lucidum spore oil. The extraction method comprises the following steps: (1) cleansing ganoderma lucidum spores; (2) breaking the walls of the ganoderma lucidum spores to obtain ganoderma lucidum spore powder; (3) preparing the wall-broken ganoderma lucidum spore powder into particles through a granulator by adopting a dry pressing method; (4) putting the particles into a supercritical CO2 extraction kettle for extraction; (5) isolating coarse ganoderma lucidum spore oil; (6) rectifying and separating to obtain the ganoderma lucidum spore oil. According to the invention, absolute ethyl alcohol-acetone is adopted as an entrainer, so that the polarity range of the extraction agents is expanded, and the extraction efficiency is effectively improved; when the walls of ganoderma lucidum spore powder are broken, natural antioxidant vitamin E is added, so that the effective constituents of the ganoderma lucidum spore powder can be effectively prevented from being oxidized and rancidified; the superfine nanometer technology is adopted, so that the local overheating phenomenon can be avoided in the smashing process and the effective active constituents in the ganoderma lucidum spore powder can be greatly retained; the coarse ganoderma lucidum spore oil is rectified and separated in nitrogen, so that the effective constituents in the ganoderma lucidum spore oil can be effectively protected from being oxidized and rancidified.
Description
Technical field
The present invention relates to the extracting method of Ganoderma spore oil, particularly a kind of employing supercritical CO
2extraction and separation technology extracts the method for Ganoderma spore oil.
Background technology
Glossy ganoderma, is called again auspicious grass, Ganoderma lucidum seu Japonicum, be China traditional strengthen the body resistance to consolidate the constitution, the Chinese medicine of strengthening by means of tonics, in successive dynasties medical book, it is classified as to top grade in Chinese medicine.Glossy ganoderma is On Polyporaceae, have " celestial grass " good reputation, and it has invigorating QI and tranquilization, relieving cough and asthma effect, for dizzy egersis, and shortness of breath and palpitation, consumptive disease is coughed and is breathed heavily, and in having the moving plant and biology of medicine food of antitumous effect, is listed in first-selection.Ganoderma spore is the glossy ganoderma growth and maturity phase to produce the seed discharging, sexual cell for glossy ganoderma, the whole hereditary active substance with glossy ganoderma, it is the elite of glossy ganoderma, and the compositions such as the triterpenes in Ganoderma spore, fatty acid, sterols, polyose, alkaloids and ucleosides in Ganoderma spore oil, have been comprised, be the aggregate of Ganoderma spore effective constituent, there is multiple physiologically active.Wherein, Ganoderma lucidum triterpenes components is the main effective constituent of glossy ganoderma, because of the diversity of its chemical structure, make ganoderma lucidum triterpene compounds have antitumor, anti-oxidant, suppress cholesterol biosynthesis, anticoagulant, protect the liver, the physiologically active more widely such as analgesia.Glossy ganoderma medicine in the market, healthcare products are of a great variety, and a lot of ganoderma lucidum prods are with total triterpene property functional component as a token of.Ganoderma lucidum triterpene compounds is not only the focus of current glossy ganoderma chemistry and pharmacological research, and has good prospects for commercial application.In recent years, Ganoderma spore oil production has become the treasure in high-grade healthcare products, has very important medical value and economic worth.
The traditional extracting method of Ganoderma spore oil generally adopts methyl alcohol or the lixiviate of ethanol equal solvent, but the method exists, extraction efficiency is low, extraction time is many, energy consumption is high, the shortcomings such as solvent load is large, dissolvent residual.Supercritical CO
2abstraction technique is the technology of emerging extraction, separation and a purifying of foodstuffs industry, compare with traditional solvent extration, have no solvent residue, pollution-free, avoid extract thermo-cracking at high temperature, be conducive to the extraction of lipid-soluble substance and heat-sensitive substance, and technique is simple, energy consumption is low, and extraction agent is nontoxic, the advantages such as easy recovery, have been widely used in the extraction of medicinal herb components and spices.
In prior art, adopt supercritical CO
2the patent report of Ganoderma Lucidum Spores Oil Extracted is more, and it is that to take the Ganoderma spore of broken wall be raw material that patent CN1239100C discloses its method of preparing Ganoderma spore oil, the aqueous ethanolic solution that is 5%～95% by volume fraction granulate dry after, use supercritical CO
2extraction, but adopt ethanolic soln to granulate, and warm air drying, ethanol is inflammable, and there is certain potential safety hazard in this scheme.In patent CN1194079C, Ganoderma spore powder is expanded through bulking machine, granulation, has changed raw material bulk density, can improve mass transfer effect, increase oil yield, but adopt puffing technique temperature higher, can accelerate oxidation and the process of becoming sour of lipid in spore powder, oily quality is brought to disadvantageous effect.Patent CN102041163A discloses the multistage supercritical CO of a kind of many bodies
2the method of Ganoderma Lucidum Spores Oil Extracted, it,, by having three grades of separated extraction kettles by putting into after Ganoderma spore powder dry granulation, take aqueous ethanolic solution as entrainment agent, by the method for classification decrease temperature and pressure, Ganoderma spore oil is separated.
To sum up, existing supercritical CO
2abstraction technique has the following disadvantages: 1) supercritical CO
2in extraction process, CO
2polarity a little less than, it only can extract nonpolar state composition and the very little composition of polarity, not good to the composition effect of extracting that polarity is larger, and triterpene compound chemical structure complexity in Ganoderma spore is various, polarity wide ranges, need higher extraction conditions just can extract, although exist in prior art by adopting aqueous ethanolic solution to carry out the scheme of auxiliary extraction as entrainment agent, but water is extremely low to the solubleness of triterpene compound, ethanol is also general to the solubleness of triterpene compound, and in extraction process, use aqueous ethanolic solution to do after entrainment agent, in gained Ganoderma spore oil, contain micro-shipwreck to remove completely, thereby affected oily quality, 2) when usining Ganoderma spore powder while extracting as raw material, after it is by broken wall, the Ganoderma spore powder of broken wall is not done to any sfgd., this make the lipid on Ganoderma spore powder surface of broken wall and triterpene compound very easily oxidized and become sour, thereby reduced the quality of oil yield and the gained Ganoderma spore oil of a part of Ganoderma spore powder.
Summary of the invention
For the deficiencies in the prior art part; the invention provides a kind of extracting method of Ganoderma spore oil; be intended to widen polarity scope, the raising extraction efficiency of extraction agent; and by adding antioxidant vitamin E when the broken wall, protect the effective constituent of Ganoderma spore powder avoid oxidized and become sour, improved the quality of oil yield and the oil of Ganoderma spore powder.
Technical scheme of the present invention is summarized as follows:
An extracting method for Ganoderma spore oil, comprises the following steps:
Step 1) Ganoderma spore processed at 50 ℃ dry 4 hours only;
Step 2) Ganoderma spore is put into ultra micro nano grinder broken wall, obtained Ganoderma spore powder;
Step 3) Ganoderma spore powder of broken wall is used dry pressing to make 10～30 object particles through nodulizer;
Step 4) Ganoderma spore powder particles is put into supercritical CO
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 10～100g, carries out subsequently supercritical CO
2extraction, extracting pressure is 20～30MPa, and extraction temperature is 30～50 ℃, and extraction time is 1～3 hour;
Step 5) from separation reactor I and separation reactor I I, obtain respectively the thick Ganoderma spore oil of different solubilities;
Step 6) the thick Ganoderma spore oil obtaining is carried out to rectifying separation under nitrogen environment, obtain Ganoderma spore oil.
Preferably, the extracting method of described Ganoderma spore oil, in described dehydrated alcohol-acetone mixed solution, the mass ratio of dehydrated alcohol and acetone is 8: 2～9: 1.
Preferably, the extracting method of described Ganoderma spore oil, in step 2) in, Ganoderma spore is carried out before broken wall, in ultra micro nano grinder, add vitamin-E powder.
Preferably, the extracting method of described Ganoderma spore oil, the mass ratio of described Ganoderma spore and vitamin-E powder is 10: 1.
Preferably, the extracting method of described Ganoderma spore oil, step 6) in rectification temperature be 120～160 ℃.
The invention has the beneficial effects as follows: 1) this case adopts dehydrated alcohol-acetone as entrainment agent, has overcome CO
2the weakness that polarity is low, the polarity scope of having widened extraction agent, and dehydrated alcohol-acetone mixed solution solvability is good, and volatility is high, and boiling point is low, and the Ganoderma spore oil extracting is separated out smoothly after step-down heats up, and organic solvent dehydrated alcohol and acetone can be with CO
2together volatilize and enter next extraction cycle, noresidue, to human body and environmentally friendly, extraction efficiency effectively improves simultaneously; 2) by add natural antioxidants vitamin-E when to ganoderma lucidium spore powder wall breaking, effectively avoided in the Ganoderma spore powder after broken wall effective constituent oxidized and become sour, improve the oil yield of Ganoderma spore powder, and effectively guaranteed purity and the content of effective constituent in Ganoderma spore oil; 3) adopt ultra micro nanometer wall breaking technology, in crushing process, avoid local superheating phenomenon, retained to greatest extent effective active composition in Ganoderma spore powder; 4) the thick Ganoderma spore oil obtaining is carried out to rectifying separation under nitrogen environment, improve oily purity simultaneously effectively in protection Ganoderma spore oil effective constituent not oxidized and become sour.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to specification sheets word.
An extracting method for Ganoderma spore oil, comprises the following steps:
Step 1) only Ganoderma spore processed and at 50 ℃ dry 4 hours to remove moisture;
Step 2) Ganoderma spore and a small amount of vitamin-E powder are put into ultra micro nano grinder broken wall, obtain being mixed with the Ganoderma spore powder of a small amount of vitamin-E powder, wherein, the mass ratio of Ganoderma spore and vitamin-E powder is preferably 10: 1.Vitamin-E is a kind of natural antioxidant, and it can mix with the Ganoderma spore powder of broken wall, effectively protects the effective active composition in Ganoderma spore, and the more important thing is, vitamin-E itself also can be by supercritical CO
2extraction, this just makes the effective active composition whole process in being extracted process in Ganoderma spore powder all by vitamin-E, be protected, and has greatly increased the stability of these effective active compositions, has indirectly improved the quality of gained Ganoderma spore oil.If vitamin-E powder addition is too much, in material, the content of Ganoderma spore powder reduces relatively, thereby affects CO
2single extraction quantity, and finally affect the integrated oil discharging productive rate of Ganoderma spore powder; If vitamin-E powder addition is on the low side, cannot meet the requirement of effective active composition in protection Ganoderma spore powder.
Step 3) Ganoderma spore powder of broken wall is used dry pressing to make 10～30 object particles through nodulizer, uses dry pressing can effectively avoid the destruction of moisture to effective constituent in Ganoderma spore powder.
Step 4) Ganoderma spore powder particles is put into the critical CO of super I
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, in dehydrated alcohol-acetone mixed solution the mass ratio of dehydrated alcohol and acetone be preferably 8: 2～9: 1, in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 10～100g, carries out subsequently supercritical CO
2extraction, extracting pressure is 20～30MPa, and extraction temperature is 30～50 ℃, and extraction time is 1～3 hour;
Step 5) from separation reactor I and separation reactor I I, obtain respectively the thick Ganoderma spore oil of different solubilities; Adopt classification pressure and temperature varying technology first to collect the spore oil that purity is higher so that precipitate is segmented collection, after what collect is the spore oil that contains certain impurity component, oil and impurity are obtained immediately separated online, improved oily purity.In separation reactor I, make the fat-soluble and low polarity component such as spore oil that solubleness is little, carotenoid, triterpene along with extraction time successively separates out successively, in separation reactor I I, decompression heats up subsequently, now CO
2departed from supercritical state, the ability of dissolving spore oil progressively declines, and makes to be originally dissolved in CO
2the impurity such as the moisture that interior another part solubleness is larger and ester matter and spore oil are separated, realized the object that the spore oil of purifying is collected in segmentation classification, but in order to obtain the Ganoderma spore oil that purity is higher, often after collecting these spore oil, also must carry out rectifying separation to them.
Step 6) the thick Ganoderma spore oil obtaining is carried out to rectifying separation under nitrogen environment, rectification temperature is preferably 120～160 ℃, obtains refining Ganoderma spore oil.Under nitrogen atmosphere, completely cut off the destruction of oxygen to effective active composition in Ganoderma spore oil, and be beneficial to temporarily or for a long time storing of later stage, in the storage receptacle of Ganoderma spore oil, also must correspondingly be full of nitrogen, with abundant starvation, be beneficial to follow-up processing.In resulting refining Ganoderma spore oil, can contain micro-vitamin-E, but this does not have negative impact to Ganoderma spore oil, because Ganoderma spore oil generally all can be processed to anticancer drugs or healthcare products, the vitamin-E of sneaking into wherein has no side effect to pharmacology.
Embodiment 1
Step 1) only 10kg Ganoderma spore processed and at 50 ℃ dry 4 hours to remove moisture;
Step 2) 10kg Ganoderma spore and 1kg vitamin-E powder are put into ultra micro nano grinder broken wall, obtain the Ganoderma spore powder that is mixed with vitamin-E powder of sporoderm-broken rate > 97%.
Step 3) Ganoderma spore powder of above-mentioned broken wall is used dry pressing to make 10 object particles through nodulizer.
Step 4) Ganoderma spore powder particles is put into supercritical CO
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, the quality of dehydrated alcohol and acetone is respectively 88g and 22g, and in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 110g, carries out subsequently supercritical CO
2extraction, the pressure of separation reactor I is 30MPa, and extraction temperature is 30 ℃, and extraction time is 1 hour; The pressure of separation reactor I I is 20MPa, and extraction temperature is 50 ℃, and extraction time is 1 hour.
Step 5) the thick Ganoderma spore oil that obtains different solubilities from separation reactor I and separation reactor I I is respectively 0.9kg altogether, and oil yield is 9%.
Step 6) the thick Ganoderma spore oil of the 0.9kg obtaining is carried out to rectifying separation under nitrogen environment, rectification temperature is 120 ℃, obtain the refining Ganoderma spore oil of 0.78kg, total oil yield is 7.8%, in spore oil, unsaturated fatty acids consists of 65～85%, total triterpene contents > 7%, total Quantitative Determination of Ergosterol > 3mg/g, Ganodenic acid A content > 1.5mg/g, peroxide value < 5mmol/kg, acid value < 8mg KOH/g, freezing transparent test period was over 6 hours.
Embodiment 2
Step 1) only 10kg Ganoderma spore processed and at 50 ℃ dry 4 hours to remove moisture;
Step 2) 10kg Ganoderma spore and 1kg vitamin-E powder are put into ultra micro nano grinder broken wall, obtain the Ganoderma spore powder that is mixed with vitamin-E powder of sporoderm-broken rate > 99%.
Step 3) Ganoderma spore powder of above-mentioned broken wall is used dry pressing to make 30 object particles through nodulizer.
Step 4) Ganoderma spore powder particles is put into supercritical CO
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, the quality of dehydrated alcohol and acetone is respectively 99g and 11g, and in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 110g, carries out subsequently supercritical CO
2extraction, the pressure of separation reactor I is 30MPa, and extraction temperature is 30 ℃, and extraction time is 3 hours; The pressure of separation reactor I I is 20MPa, and extraction temperature is 50 ℃, and extraction time is 2 hours.
Step 5) the thick Ganoderma spore oil that obtains different solubilities from separation reactor I and separation reactor I I is respectively 1.5kg altogether, and oil yield is 15%.
Step 6) the thick Ganoderma spore oil of the 1.5kg obtaining is carried out to rectifying separation under nitrogen environment, rectification temperature is 160 ℃, obtain the refining Ganoderma spore oil of 1.33kg, total oil yield is 13.3%, in spore oil, unsaturated fatty acids consists of 65～85%, total triterpene contents > 7%, total Quantitative Determination of Ergosterol > 3mg/g, Ganodenic acid A content > 1.5mg/g, peroxide value < 5mmol/kg, acid value < 8mg KOH/g, freezing transparent test period was over 6 hours.
Embodiment 3
Step 1) only 10kg Ganoderma spore processed and at 50 ℃ dry 4 hours to remove moisture;
Step 2) 10kg Ganoderma spore is put into ultra micro nano grinder broken wall, obtained the Ganoderma spore powder of sporoderm-broken rate > 97%.
Step 3) Ganoderma spore powder of above-mentioned broken wall is used dry pressing to make 20 object particles through nodulizer.
Step 4) Ganoderma spore powder particles is put into supercritical CO
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, the quality of dehydrated alcohol and acetone is respectively 85g and 15g, and in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 100g, carries out subsequently supercritical CO
2extraction, the pressure of separation reactor I is 30MPa, and extraction temperature is 30 ℃, and extraction time is 2 hours; The pressure of separation reactor I I is 20MPa, and extraction temperature is 50 ℃, and extraction time is 2 hours.
Step 5) the thick Ganoderma spore oil that obtains different solubilities from separation reactor I and separation reactor I I is respectively 1.1kg altogether, and oil yield is 11%.
Step 6) the thick Ganoderma spore oil of the 1.1kg obtaining is carried out to rectifying separation under nitrogen environment, rectification temperature is 130 ℃, obtain the refining Ganoderma spore oil of 0.89kg, total oil yield is 8.9%, in spore oil, unsaturated fatty acids consists of 60～75%, total triterpene contents > 5%, total Quantitative Determination of Ergosterol > 2mg/g, Ganodenic acid A content > 1.0mg/g, peroxide value < 5mmol/kg, acid value < 10mg KOH/g, freezing transparent test period was over 4 hours.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details.
Claims (5)
1. an extracting method for Ganoderma spore oil, is characterized in that, comprises the following steps:
Step 1) Ganoderma spore processed at 50 ℃ dry 4 hours only;
Step 2) Ganoderma spore is put into ultra micro nano grinder broken wall, obtained Ganoderma spore powder;
Step 3) Ganoderma spore powder of broken wall is used dry pressing to make 10～30 object particles through nodulizer;
Step 4) Ganoderma spore powder particles is put into supercritical CO
2in extraction kettle, using dehydrated alcohol-acetone mixed solution as entrainment agent, in extraction kettle, every kilogram of material adds dehydrated alcohol-acetone mixed solution of 10～100g, carries out subsequently supercritical CO
2extraction, extracting pressure is 20～30MPa, and extraction temperature is 30～50 ℃, and extraction time is 1～3 hour;
Step 5) from separation reactor I and separation reactor I I, obtain respectively the thick Ganoderma spore oil of different solubilities;
Step 6) the thick Ganoderma spore oil obtaining is carried out to rectifying separation under nitrogen environment, obtain Ganoderma spore oil.
2. the extracting method of Ganoderma spore oil according to claim 1, is characterized in that, in described dehydrated alcohol-acetone mixed solution, the mass ratio of dehydrated alcohol and acetone is 8: 2～9: 1.
3. the extracting method of Ganoderma spore oil according to claim 1, is characterized in that, in step 2) in, Ganoderma spore is carried out before broken wall, in ultra micro nano grinder, add vitamin-E powder.
4. the extracting method of Ganoderma spore oil according to claim 3, is characterized in that, the mass ratio of described Ganoderma spore and vitamin-E powder is 10: 1.
5. the extracting method of Ganoderma spore oil according to claim 1, is characterized in that step 6) in rectification temperature be 120～160 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410338619.3A CN104073344B (en) | 2014-07-16 | 2014-07-16 | A kind of extracting method of Ganoderma spore oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410338619.3A CN104073344B (en) | 2014-07-16 | 2014-07-16 | A kind of extracting method of Ganoderma spore oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104073344A true CN104073344A (en) | 2014-10-01 |
| CN104073344B CN104073344B (en) | 2016-08-24 |
Family
ID=51594955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410338619.3A Active CN104073344B (en) | 2014-07-16 | 2014-07-16 | A kind of extracting method of Ganoderma spore oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104073344B (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946383A (en) * | 2015-04-30 | 2015-09-30 | 江苏江大源生态生物科技有限公司 | Method for preparing ganoderma lucidum spores oil through supercritical CO2 composite microwave-assisted extraction |
| CN105232584A (en) * | 2015-09-30 | 2016-01-13 | 河南行知专利服务有限公司 | Decoction-free extraction process for precious Chinese herbal medicines |
| CN105820873A (en) * | 2016-04-28 | 2016-08-03 | 合肥云峰信息科技有限公司 | Extraction method of ganoderma lucidum spore oil |
| CN106318616A (en) * | 2016-10-19 | 2017-01-11 | 南京希元生物医药科技有限公司 | Ganoderma lucidum spores oil |
| CN106318612A (en) * | 2016-09-19 | 2017-01-11 | 中山大学 | Method for supercritical extraction of ganoderma lucidum spore oil |
| CN106381220A (en) * | 2016-10-19 | 2017-02-08 | 南京希元生物医药科技有限公司 | Preparation process of ganoderma lucidum spores oil |
| CN106619746A (en) * | 2016-10-19 | 2017-05-10 | 南京希元生物医药科技有限公司 | Ganoderma spore powder granules |
| CN112760165A (en) * | 2020-12-29 | 2021-05-07 | 江苏滋补堂药业有限公司 | Method for removing acid value of ganoderma lucidum spore oil |
| CN112779086A (en) * | 2020-12-18 | 2021-05-11 | 江苏滋补堂药业有限公司 | Method for removing peroxide value of ganoderma lucidum spore oil |
| CN113876818A (en) * | 2021-10-15 | 2022-01-04 | 南京中科药业有限公司 | Compound ganoderma lucidum spore oil extract for preventing stroke and preparation method and application thereof |
| CN114672370A (en) * | 2022-03-15 | 2022-06-28 | 苏凤全 | Preparation method of ganoderma lucidum spore oil and skin care product containing ganoderma lucidum spore oil |
| CN114917261A (en) * | 2022-05-30 | 2022-08-19 | 安徽芝神堂药业有限公司 | Production process of ganoderma lucidum spore oil extract for adjuvant therapy of tumors |
| CN115125059A (en) * | 2022-06-15 | 2022-09-30 | 中科健康产业集团股份有限公司 | Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil |
| CN115137760A (en) * | 2022-08-13 | 2022-10-04 | 青海净草生物科技有限公司 | Blood pressure lowering ganoderma lucidum spore oil capsule and preparation method thereof |
| CN115177974A (en) * | 2022-07-07 | 2022-10-14 | 广州海文森特实业有限公司 | Method and equipment for extracting and concentrating high-purity ganoderma lucidum triterpenoids |
| CN115282171A (en) * | 2022-08-13 | 2022-11-04 | 青海净草生物科技有限公司 | Ganoderma lucidum spore oil with immunity improving function and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1468947A (en) * | 2003-06-20 | 2004-01-21 | 列 陈 | Glossy ganoderma spore oil extracting and refining process |
| CN101380340A (en) * | 2008-10-14 | 2009-03-11 | 广东南台药业有限公司 | Wall-broken glossy ganoderma spore powder antioxidation method |
| CN102041163A (en) * | 2011-01-05 | 2011-05-04 | 南昌同心紫巢生物工程有限公司 | Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil |
| CN102911790A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Extraction method of phlomis umbrosa turcz volatile oil |
| CN103146473A (en) * | 2013-03-21 | 2013-06-12 | 云南森源化工有限公司 | Method for simultaneously extracting Australian tea tree essential oil and flavonoid glycosides |
| CN103710264A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Auxiliary additive for wall breaking of Mythic Fungus spores |
-
2014
- 2014-07-16 CN CN201410338619.3A patent/CN104073344B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1468947A (en) * | 2003-06-20 | 2004-01-21 | 列 陈 | Glossy ganoderma spore oil extracting and refining process |
| CN101380340A (en) * | 2008-10-14 | 2009-03-11 | 广东南台药业有限公司 | Wall-broken glossy ganoderma spore powder antioxidation method |
| CN102041163A (en) * | 2011-01-05 | 2011-05-04 | 南昌同心紫巢生物工程有限公司 | Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil |
| CN102911790A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Extraction method of phlomis umbrosa turcz volatile oil |
| CN103146473A (en) * | 2013-03-21 | 2013-06-12 | 云南森源化工有限公司 | Method for simultaneously extracting Australian tea tree essential oil and flavonoid glycosides |
| CN103710264A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Auxiliary additive for wall breaking of Mythic Fungus spores |
Non-Patent Citations (1)
| Title |
|---|
| 刘晓庚等: "夹带剂及其对超临界CO2萃取效能的影响", 《食品科学》 * |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946383B (en) * | 2015-04-30 | 2018-07-03 | 江苏江大源生态生物科技有限公司 | A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil |
| CN104946383A (en) * | 2015-04-30 | 2015-09-30 | 江苏江大源生态生物科技有限公司 | Method for preparing ganoderma lucidum spores oil through supercritical CO2 composite microwave-assisted extraction |
| CN105232584A (en) * | 2015-09-30 | 2016-01-13 | 河南行知专利服务有限公司 | Decoction-free extraction process for precious Chinese herbal medicines |
| CN105820873A (en) * | 2016-04-28 | 2016-08-03 | 合肥云峰信息科技有限公司 | Extraction method of ganoderma lucidum spore oil |
| CN106318612A (en) * | 2016-09-19 | 2017-01-11 | 中山大学 | Method for supercritical extraction of ganoderma lucidum spore oil |
| CN106619746B (en) * | 2016-10-19 | 2020-09-11 | 南京希元生物医药科技有限公司 | Ganoderma lucidum spore powder particle |
| CN106619746A (en) * | 2016-10-19 | 2017-05-10 | 南京希元生物医药科技有限公司 | Ganoderma spore powder granules |
| CN106381220A (en) * | 2016-10-19 | 2017-02-08 | 南京希元生物医药科技有限公司 | Preparation process of ganoderma lucidum spores oil |
| CN106318616A (en) * | 2016-10-19 | 2017-01-11 | 南京希元生物医药科技有限公司 | Ganoderma lucidum spores oil |
| CN112779086A (en) * | 2020-12-18 | 2021-05-11 | 江苏滋补堂药业有限公司 | Method for removing peroxide value of ganoderma lucidum spore oil |
| CN112760165A (en) * | 2020-12-29 | 2021-05-07 | 江苏滋补堂药业有限公司 | Method for removing acid value of ganoderma lucidum spore oil |
| CN113876818A (en) * | 2021-10-15 | 2022-01-04 | 南京中科药业有限公司 | Compound ganoderma lucidum spore oil extract for preventing stroke and preparation method and application thereof |
| CN114672370A (en) * | 2022-03-15 | 2022-06-28 | 苏凤全 | Preparation method of ganoderma lucidum spore oil and skin care product containing ganoderma lucidum spore oil |
| CN114917261A (en) * | 2022-05-30 | 2022-08-19 | 安徽芝神堂药业有限公司 | Production process of ganoderma lucidum spore oil extract for adjuvant therapy of tumors |
| CN115125059A (en) * | 2022-06-15 | 2022-09-30 | 中科健康产业集团股份有限公司 | Method for removing fat-soluble harmful ingredients in ganoderma lucidum spore oil |
| CN115125059B (en) * | 2022-06-15 | 2024-03-26 | 南京中科药业有限公司 | Method for removing fat-soluble harmful components in ganoderma lucidum spore oil |
| CN115177974A (en) * | 2022-07-07 | 2022-10-14 | 广州海文森特实业有限公司 | Method and equipment for extracting and concentrating high-purity ganoderma lucidum triterpenoids |
| CN115137760A (en) * | 2022-08-13 | 2022-10-04 | 青海净草生物科技有限公司 | Blood pressure lowering ganoderma lucidum spore oil capsule and preparation method thereof |
| CN115282171A (en) * | 2022-08-13 | 2022-11-04 | 青海净草生物科技有限公司 | Ganoderma lucidum spore oil with immunity improving function and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104073344B (en) | 2016-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104073344A (en) | Extracting method for ganoderma lucidum spore oil | |
| CN102041163B (en) | Multi-body multi-stage supercritical CO2 method for extraction of ganoderma lucidum spore oil | |
| CN103351941B (en) | Supercritical CO2 variable-temperature variable-pressure extraction method of lucid ganoderma spore oil | |
| CN103976453B (en) | Chu chrysanthemum extract, solid beverage, lozenge and food additives and preparation method thereof | |
| CN101935586A (en) | Method for extracting ganoderma spore oil with supercritical CO2 | |
| CN102060728A (en) | Method for extracting capsorubin and capsaicin from chillies | |
| CN102295988A (en) | Supercritical carbon dioxide extraction method of gardenia whole fruit oil | |
| CN110840921A (en) | High-pressure supercritical CO2Ganoderma extract and its preparation method | |
| CN102850414A (en) | Method for continuously extracting flaxseed gum and lignan from flaxseed husks | |
| CN107573317A (en) | A kind of extracting method of blueberry anthocyanin | |
| CN100998613B (en) | Method for producing effective component of glossy ganoderma by using supercritical technology | |
| CN100425247C (en) | Refining ganoderam lucidum spore oil and method for preparing same | |
| CN101683362A (en) | Method for extracting ganoderma oil by supercritical carbon dioxide | |
| CN1328255C (en) | Method for extracting garlicin | |
| CN103146473A (en) | Method for simultaneously extracting Australian tea tree essential oil and flavonoid glycosides | |
| CN105820873A (en) | Extraction method of ganoderma lucidum spore oil | |
| CN101628857B (en) | Production technique for extracting resveratrol from giant knotweed | |
| CN109609263A (en) | A kind of preparation process and oat oil of oat oil | |
| CN103436354A (en) | Method for extracting Trichosanthes kirilowii Maxim seed oil | |
| CN104083556B (en) | A kind of method that konjak ceramide is extracted from konjaku | |
| CN102267855A (en) | Extraction method of lycopene | |
| CN101390975A (en) | Extraction method of citrus active ingredient | |
| CN103897800A (en) | Process for extracting wheat germ oil by adopting supercritical extraction method | |
| CN102206241B (en) | Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue | |
| CN1687052A (en) | Method for extracting coumarin substances from rhodiola root of natural plant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201224 Address after: 2 Nanjing middle road, Yangzi River International Chemical Industry Park, Suzhou, Jiangsu Province Patentee after: ZHANG JIA GANG VINSCE BIO-PHARM Co.,Ltd. Address before: Building D, No.7, Guangdong Road, free trade zone, Zhangjiagang City, Jiangsu Province Patentee before: JIANGSU SWELLXIN BIO-PHARM. Pty Ltd. |
|
| TR01 | Transfer of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A method for extracting ganoderma lucidum spore oil Effective date of registration: 20210930 Granted publication date: 20160824 Pledgee: Agricultural Bank of China Limited Zhangjiagang branch Pledgor: ZHANG JIA GANG VINSCE BIO-PHARM Co.,Ltd. Registration number: Y2021320010400 |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 2 Nanjing middle road, Yangzi River International Chemical Industry Park, Suzhou, Jiangsu Province Patentee after: Wison Biomedical (Suzhou) Co.,Ltd. Address before: 2 Nanjing middle road, Yangzi River International Chemical Industry Park, Suzhou, Jiangsu Province Patentee before: Weisheng Biomedical (Suzhou) Co.,Ltd. Address after: 2 Nanjing middle road, Yangzi River International Chemical Industry Park, Suzhou, Jiangsu Province Patentee after: Weisheng Biomedical (Suzhou) Co.,Ltd. Address before: 2 Nanjing middle road, Yangzi River International Chemical Industry Park, Suzhou, Jiangsu Province Patentee before: ZHANG JIA GANG VINSCE BIO-PHARM Co.,Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20221031 Granted publication date: 20160824 Pledgee: Agricultural Bank of China Limited Zhangjiagang branch Pledgor: ZHANG JIA GANG VINSCE BIO-PHARM Co.,Ltd. Registration number: Y2021320010400 |