CN1424303A - Refinery pyrethrin preparation - Google Patents
Refinery pyrethrin preparation Download PDFInfo
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- CN1424303A CN1424303A CN 02134162 CN02134162A CN1424303A CN 1424303 A CN1424303 A CN 1424303A CN 02134162 CN02134162 CN 02134162 CN 02134162 A CN02134162 A CN 02134162A CN 1424303 A CN1424303 A CN 1424303A
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Abstract
A process for refining pyrethrin includes such steps as collecting dried flower of pyrethrum, extracting with organic solvent (petroleum ether or n-hexane) or subcritical propane, butane or CO2 liquid, recovering solvent to obtain extract, mixing with mixed solvent A, removing insoluble substance, low-temp freezing, filtering, dewaxing, decolouring, vacuum concentrating filtrate, dissolving in mixed solvent B, filtering, removing insoluble substance, recovering solvent and concentrating.
Description
Technical field: the invention belongs to natural biological sterilant preparation method, relate in particular to a kind of refinery pyrethrin preparation.
Technical background: natural pyrethrin is the insect killing optimal medicine of effectively preserving the ecological environment; a large amount of at present miehailin aerosols that use, electric mosquito repellent etc. all belong to synthetic Cypermethrin, d-allethrin etc.; because synthetic plan chrysanthemum ester class bionic pesticide is the product about 40%, the seriously polluted health risk that contained a large amount of impurity cause.Resemble the disastrous cotton boll insect pest in cotton region and will control, removing Bt and viral coupling sterilant is an aspect, will be one of the strongest means with the multiple full agricultural chemicals of natural pyrethrin preparation.Cause very big demand like this to natural chrysanthemum ester, also supply falls short of demand to natural pyrethrin on the market, from dry pyrethrum flower, extract the natural pyrethrin method and just become a focus, the technology of extracting at present pyrethrin in the world can be divided three classes, the continuous solvent method that adopts as Australian CIG pyrethrum company, this method production cost is lower, but facility investment is relatively large, other method equipment cost is very high, be difficult to popularization and application, as the normal hexane extraction method etc., exist the operational path complexity, pollute bigger shortcoming.
Summary of the invention: the objective of the invention is to making with extra care and a kind of modified version novel process of design at organic solvent (sherwood oil, normal hexane etc.) and subcritical (propane, butane, carbon dioxide liquid) extraction natural pyrethrin medicinal extract.Pyrethrum medicinal extract by the aforesaid method extraction is black, and mainly by the 20-35% pyrethrin, 65-80% impurity is formed, and impurity mainly is made up of saturated fatty acid, unsaturated fatty acids and resin natural gum, pigment etc.To achieve these goals, the invention provides following technical scheme:
Refinery pyrethrin preparation, getting dry pyrethrum flower extracts with organic solvent (sherwood oil, normal hexane etc.) or with subcritical (propane, butane, carbonic acid gas etc.), reclaim solvent or spe medium and get medicinal extract, extract medicinal extract, remove insolubles at stirring at normal temperature mixed solvent A; Lysate filters dewaxing, decolouring in cryogenic freezing; Filtrate concentrates under vacuum, gets concentrated extract; Medicinal extract dissolves with mixed solvent B; Remove by filter mixed solvent B insolubles, concentrate and reclaim solvent, promptly get purified product.
Above-mentioned process for purification, medicinal extract add 4-10 amount (w/w) mixed solvent A, in 30 degree stirring and dissolving, remove insolubles, filter lysate; Lysate is cooled to throw out and fully separates out under 0 to-30 ℃ of condition, leach the low temperature insolubles, filtrate is mixed by a certain percentage via activated carbon and aluminum oxide and is formed decolouring absorption stationary phase material, and the mixed solvent A that mix to form with different ratios is as the elutriant wash-out, be eluted to colourless repeatedly with mixed liquor A, merge elutriant, low temperature reclaims mixed solution and gets raw oil; Add then 4-10 doubly (w/w) amount mixed solvent B normal temperature stir moltenly, get lysate and freezingly down be placed to solution and place clarification at 0 to-30 ℃, remove by filter insolubles, low temperature reclaims mixed solvent and must make with extra care the pyrethrin oil production under vacuum.
Above-mentioned process for purification mixed solvent A chooses: be the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, ethyl acetate, acetone, ether, acetonitrile, in the Nitromethane 99Min. equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
Above-mentioned process for purification mixed solvent B chooses: be the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, in ethyl acetate, acetone, ether, the acetonitrile equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
More specifically method is chosen medicinal extract and is added 4-10 amount (w/w) mixed solvent A, stirs moltenly at 30 degree, removes insolubles, filter lysate; Lysate is cooled to throw out and fully separates out under 0 to-30 ℃ of condition, leach the low temperature insolubles, filtrate was mixed composition decolouring absorption stationary phase material via activated carbon and aluminum oxide between 1: 9 to 9: 1, and be the oil ethers with mixed solvent A, hexanaphthene, normal hexane, methyl alcohol, ethanol, propyl alcohol, low-carbon alcohol such as Virahol (carbon number is less than 6), ethyl acetate, acetone, ether, acetonitrile, the mixed solution that certain two or three solvent in the Nitromethane 99Min. equal solvent is formed by a certain percentage is eluted to colourless repeatedly, merge elutriant, low temperature reclaims mixed solution and gets raw oil; Adding 4-10 times (w/w) amount mixed solvent B then is the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, the mixed solution normal temperature that certain two or three solvent is formed by a certain percentage in ethyl acetate, acetone, ether, the acetonitrile equal solvent stirs molten, get lysate freezing solution that is placed under 0 to-30 ℃ and place clarification, remove by filter insolubles, low temperature reclaims mixed solvent and must make with extra care the pyrethrin oil production under vacuum.
Description of drawings:
Fig. 1 is a refinery pyrethrin preparation schema of the present invention.
Embodiment:
Further essentiality content of the present invention is described below in conjunction with embodiment, but content of the present invention is not limited thereto.
Embodiment 1:
1, processing parameter is chosen:
Mixed solvent A:
Be low-carbon alcohol (carbon number is less than 6) such as oil ethers, hexanaphthene, normal hexane, methyl alcohol, ethanol, propyl alcohol, Virahol, ethyl acetate, acetone, ether, acetonitrile, in the Nitromethane 99Min. equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
Mixed solvent B:
Be low-carbon alcohol (carbon number is less than 6) such as oil ethers, hexanaphthene, normal hexane, methyl alcohol, ethanol, propyl alcohol, Virahol, in ethyl acetate, acetone, ether, the acetonitrile equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
Dewaxing, decolorizing and absorbing material: activated carbon and aluminum oxide (or diatomite) are formed by a certain percentage, and compositing range is between 1: 9 to 9: 1
2, operation steps:
2-1, medicinal extract stirring and dissolving are removed impurity: get a certain amount of medicinal extract and add 4-10 amount (w/w) mixed solvent A,
Stir moltenly at 30 degree, remove insolubles, filter lysate.
2-2, dewaxing, decolouring: 2-1 processing gained lysate is cooled to heavy earnest fully separates out under 0 to-30 ℃ of condition, leach the low temperature insolubles, filtrate is mixed by a certain percentage via activated carbon and aluminum oxide and is formed decolouring absorption stationary phase material, and the mixed solvent A that mix to form with different ratios is as the elutriant wash-out, be eluted to colourless repeatedly with mixed liquor A, merge elutriant, low temperature reclaims mixed solution and gets raw oil.
2-3,2-2 gained raw oil add 4-10 doubly (w/w) amount mixed solvent B normal temperature stir molten, get lysate freezing solution that is placed under 0 to-30 ℃ and place clarification, remove by filter insolubles, low temperature reclaims mixed solvent and must make with extra care the pyrethrin oil production under vacuum, and wherein the content of insecticidal active ingredient pyrethrin is more than 70%.
3, the refinement treatment of 1021.5 gram pyrethrum subcritical abstraction things:
| Sample number into spectrum | 20020615 | Sample source | The subcritical abstraction thing |
| Sample characteristics of for example | The black fluid thing | Solvent | Mixed solvent A, mixed solvent B |
3-1,1021.5 gram medicinal extract add 7L mixed solvent A 30 ℃ of stirring and dissolving, mixed solution is put in 0 ℃ to-30 ℃ scope, being cooled to throw out fully separates out, filter, remove insoluble substance, filtrate gets deep green liquid through decolorizing column (stationary phase by activated carbon: aluminum oxide mixes by a certain percentage and forms) wash-out, be eluted to colourless repeatedly with mixed solution, merge elutriant, concentrating under reduced pressure gets 429.60 gram oily matter, is raw product.
3-2,1) the thick product that obtains 429.60 gram oily matter abundant stirring and dissolving in 3L mixed solvent B, the dissolving mixing solutions is through cryogenic freezing in 0 ℃ to-30 ℃ scope, the insolubles precipitation is separated out fully, remove by filter sedimentable matter, filtrate is through concentrating under reduced pressure, concentrate to such an extent that purified product 365.20 restrains, insolubles remnants are 64.40 grams.
The 3-3 product quality analysis
| The sample title | Amount of analysis (g) | Chrysanthemum ester content % | Get ester rate % |
| Medicinal extract | ????0.217 | ????30.14 | ??????- |
| Thick oil | ????0.117 | ????64.50 | ????89.99 |
| Treated oil | ????0.114 | ????72.08 | ????95.00 |
Embodiment 2:
932.5 the refinement treatment of gram pyrethrum petroleum ether extract
| Sample number into spectrum | 20020616 | Sample source | Petroleum ether extract |
| Sample characteristics of for example | The black fluid thing | Solvent | Mixed solvent A, mixed solvent B |
[treatment process]
1,932.5 gram medicinal extract add 6L mixed solvent A 30 ℃ of stirring and dissolving, mixed solution is placed in 0 ℃ to-30 ℃ scope, being cooled to throw out fully separates out, filter, remove insoluble substance, filtrate gets deep green liquid through decolorizing column (stationary phase is by activated carbon: the aluminum oxide certain proportion mixes and forms) wash-out, is eluted to colourless repeatedly with mixed solution, merge the elutriant concentrating under reduced pressure and get 364.32 gram oily matter, be raw product.
2,1) the thick product that obtains 364.32 gram oily matter abundant stirring and dissolving in 2.5L mixed solvent B, lysate is through low temperature in 0 ℃ to-30 ℃ scope, the freezing insoluble substance precipitation that makes is separated out fully, after solution filters, filtrate gets purified product product 293.97 grams through concentrating under reduced pressure, gets residual insoluble substance 70.35 grams.
[product quality analysis]
| The sample title | Amount of analysis (g) | Chrysanthemum ester content % | Get ester rate % |
| Medicinal extract | ????0.112 | ????28.00 | ??????- |
| Thick oil | ????0.117 | ????63.02 | ????87.93 |
| Treated oil | ????0.114 | ????70.29 | ????94.99 |
Embodiment 3:
The refinement treatment of 3000 gram pyrethrum N-hexane extracts
| Sample number into spectrum | ??20020617 | Sample source | N-hexane extract |
| Sample characteristics of for example | The black fluid thing | Solvent | Mixed solvent A, mixed solvent B |
[treatment process]
1,3000 gram medicinal extract add 15L mixed solvent A 30 ℃ of stirring and dissolving, mixed solution is placed in 0 ℃ to-30 ℃ scope, being cooled to throw out fully separates out, filter, remove insoluble substance, filtrate gets deep green liquid through decolorizing column (stationary phase by activated carbon: aluminum oxide mixes by a certain percentage and forms) wash-out, be eluted to colourless repeatedly with mixed solution, merge elutriant, concentrating under reduced pressure gets 1790 gram oily matter, is raw product.
2,1) the thick product that obtains 1790 gram oily matter abundant stirring and dissolving in 8L mixed solvent B, lysate is freezing in 0 ℃ to-30 ℃ scope of low temperature, the insoluble substance precipitation is separated out fully, behind the filtering solution, concentrating filter liquor gets purified product 1260 grams, gets residual insolubles material 521.23 grams.
[product quality analysis]
| The sample title | Amount of analysis (g) | Chrysanthemum ester content % | Get ester rate % |
| Medicinal extract | ????0.217 | ????30.40 | ??????- |
| Thick oil | ????0.117 | ????63.50 | ????89.99 |
| Treated oil | ????0.114 | ????71.21 | ????90.01 |
Embodiment 4:
The refinement treatment of 4000 gram pyrethrum subcritical abstraction things
| Sample number into spectrum | ??20020618 | Sample source | The subcritical abstraction thing |
| Sample characteristics of for example | The black fluid thing | Solvent | Mixed solvent A, mixed solvent B |
[treatment process]
1,4000 gram medicinal extract add 20L mixed solvent A and stir molten at 30 ℃, mixed solution is placed in 0 ℃ to-30 ℃ scope, being cooled to throw out fully separates out, remove by filter insolubles, filtrate gets deep green liquid through decolorizing column (stationary phase by activated carbon: the diatomite fine powder mixes by a certain percentage and forms) wash-out, is eluted to colourlessly repeatedly with mixed solution, merges elutriant, concentrating under reduced pressure gets 1827.69 gram oily matter, is raw product.
2,1) the thick product that obtains 1827.69 gram oily matter abundant stirring and dissolving in 10L mixed solvent B, lysate is freezing in 0 ℃ to-30 ℃ scope of low temperature, the insoluble substance precipitation is separated out fully, filtering solution, filtrate gets purified product 1542.01 grams through concentrating under reduced pressure, gets residual insoluble substance 285.68 grams.
[product quality analysis]
| The sample title | Amount of analysis (g) | Chrysanthemum ester content % | Get ester rate % |
| Medicinal extract | ????0.117 | ????33.00 | ?????- |
| Thick oil | ????0.106 | ????65.00 | ????89.99 |
| Treated oil | ????0.114 | ????73.19 | ????95.00 |
It is as follows to draw the excellent beneficial effect that the refining method of Dalmatian chrysanthemum of the present invention compared with prior art reaches from above experimental result:
1, can find out from above experimental result: the patent of invention that the present invention and the applicant declare " the refined raw production. art of high-purity pyrethrin " (application number: 97118710.X; Publication number: CN1176246A) relatively, done larger improvement, the refined raw production. art has been simplified step greatly, be reduced to three key steps, and the pyrethrins content in yield and the product is improved all.
2, one of characteristics of the present invention are kept away water for whole method flow, distribute without aqueous solvent; Step with simple several dissolvings, filtration, the physical process such as concentrated, just pyrethrum dried flower extract purification can be become highly purified pyrethrins product (the chrysanthemum ester content surpasses 70%), product color is shallow, transparent, evenly, product quality is highly stable, and output and quality reaches the requirement of company standard and international market fully.
3, another characteristics of the present invention are to utilize by activated carbon: aluminium oxide (or diatomite) mixes the fixedly phase that forms by a certain percentage, and as the committed step of dewaxing, decolouring, this is never used in technique in the past.
4, in the inventive method step, behind mixed solvent B dissolving semifinished product chrysanthemum ester oil, lysate freezing placement in 0 ℃ to-30 ℃ scope of low temperature is separated out the insoluble matter precipitation fully, place transparent supernatant solution and pour out, reduced pressure concentration also can get purified product. Needn't refilter, operate simplyr, and the yield of purified product also can be controlled at about 95%. Thereby method flow is easy to operate, and production cost is low, and day output increases.
5, the content analysis of pyrethrins adopts the GC analytic approach of AOAC, with the definite content with respect to peak area of interior mark, as external standard, calculates the absolute content of pyrethrins with internationally recognized standard items. Thereby the content of the pyrethrins of each duplicate samples is all comparatively accurate, and mutually relatively or the pyrethrins content for preparing sample with in the past process for refining relatively, all be quite reliably quite accurately.
Claims (5)
1, refinery pyrethrin preparation, it is characterized in that getting dry pyrethrum flower extracts with organic solvent (sherwood oil, normal hexane etc.) or with subcritical (propane, butane, carbonic acid gas etc.), reclaim solvent or spe medium and get medicinal extract, extract medicinal extract, remove insolubles at stirring at normal temperature mixed solvent A; Lysate filters dewaxing, decolouring in cryogenic freezing; Filtrate concentrates under vacuum, gets concentrated extract; Medicinal extract dissolves with mixed solvent B; Remove by filter mixed solvent B insolubles, concentrate and reclaim solvent, promptly get purified product.
2, process for purification according to claim 1 is characterized in that medicinal extract adds 4-10 amount (w/w) mixed solvent A, stirs moltenly at 30 degree, removes insolubles, filter lysate; Lysate is cooled to throw out and fully separates out under 0 to-30 ℃ of condition, leach the low temperature insolubles, filtrate is mixed by a certain percentage via activated carbon and aluminum oxide and is formed decolouring absorption stationary phase material, and the mixed solvent A that mix to form with different ratios is as the elutriant wash-out, be eluted to colourless repeatedly with mixed liquor A, merge elutriant, low temperature reclaims mixed solution and gets raw oil; Add then 4-10 doubly (w/w) amount mixed solvent B normal temperature stir moltenly, get lysate and freezingly down be placed to solution and place clarification at 0 to-30 ℃, remove by filter insolubles, low temperature reclaims mixed solvent and must make with extra care the pyrethrin oil production under vacuum.
3, process for purification according to claim 1 and 2, it is characterized in that mixed solvent A chooses: be the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, ethyl acetate, acetone, ether, acetonitrile, in the Nitromethane 99Min. equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
4, process for purification according to claim 1 and 2, it is characterized in that mixed solvent B chooses: be the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, in ethyl acetate, acetone, ether, the second cyanogen equal solvent, the mixed solution that certain two or three solvent is formed by a certain percentage.
5, process for purification according to claim 1 is characterized in that medicinal extract adds 4-10 amount (w/w) mixed solvent A, in 30 degree stirring and dissolving, removes insolubles, filter lysate; Lysate is cooled to throw out and fully separates out under 0 to-30 ℃ of condition, leach the low temperature insolubles, filtrate was mixed composition decolouring absorption stationary phase material via activated carbon and aluminum oxide between 1: 9 to 9: 1, and be the oil ethers with mixed solvent A, hexanaphthene, normal hexane, methyl alcohol, ethanol, propyl alcohol, low-carbon alcohol such as Virahol (carbon number is less than 6), ethyl acetate, acetone, ether, acetonitrile, the mixed solution that certain two or three solvent in the Nitromethane 99Min. equal solvent is formed by a certain percentage is eluted to colourless repeatedly, merge elutriant, low temperature reclaims mixed solution and gets raw oil; Adding 4-10 times (w/w) amount mixed solvent B then is the oil ethers, hexanaphthene, normal hexane, low-carbon alcohol (carbon number is less than 6) such as methyl alcohol, ethanol, propyl alcohol, Virahol, the mixed solution normal temperature that certain two or three solvent is formed by a certain percentage in ethyl acetate, acetone, ether, the acetonitrile equal solvent stirs molten, get lysate freezing solution that is placed under 0 to-30 ℃ and place clarification, remove by filter insolubles, low temperature reclaims mixed solvent and must make with extra care the pyrethrin oil production under vacuum.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02134162 CN1424303A (en) | 2002-11-21 | 2002-11-21 | Refinery pyrethrin preparation |
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|---|---|---|---|
| CN 02134162 CN1424303A (en) | 2002-11-21 | 2002-11-21 | Refinery pyrethrin preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735643A (en) * | 2009-11-26 | 2010-06-16 | 晨光生物科技集团股份有限公司 | Method for removing peculiar smell of red cabbage |
| CN102675108A (en) * | 2012-04-25 | 2012-09-19 | 华南理工大学 | Refining method of pyrethrin crude extract |
| CN107365622A (en) * | 2017-06-20 | 2017-11-21 | 云南汉木森生物科技有限责任公司 | A kind of extracting method of hemp wax |
| CN107445924A (en) * | 2017-07-31 | 2017-12-08 | 梅跃进 | A kind of method of subcritical abstraction pyrethrins |
-
2002
- 2002-11-21 CN CN 02134162 patent/CN1424303A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735643A (en) * | 2009-11-26 | 2010-06-16 | 晨光生物科技集团股份有限公司 | Method for removing peculiar smell of red cabbage |
| CN101735643B (en) * | 2009-11-26 | 2012-12-05 | 晨光生物科技集团股份有限公司 | Method for removing peculiar smell of red cabbage |
| CN102675108A (en) * | 2012-04-25 | 2012-09-19 | 华南理工大学 | Refining method of pyrethrin crude extract |
| CN102675108B (en) * | 2012-04-25 | 2014-05-07 | 华南理工大学 | Refining method of pyrethrin crude extract |
| CN107365622A (en) * | 2017-06-20 | 2017-11-21 | 云南汉木森生物科技有限责任公司 | A kind of extracting method of hemp wax |
| CN107445924A (en) * | 2017-07-31 | 2017-12-08 | 梅跃进 | A kind of method of subcritical abstraction pyrethrins |
| CN107445924B (en) * | 2017-07-31 | 2020-05-08 | 梅跃进 | Subcritical pyrethrin extraction method |
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