CN106349038A - Method for preparing musk ketone efficiently and mildly - Google Patents
Method for preparing musk ketone efficiently and mildly Download PDFInfo
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- CN106349038A CN106349038A CN201610001972.1A CN201610001972A CN106349038A CN 106349038 A CN106349038 A CN 106349038A CN 201610001972 A CN201610001972 A CN 201610001972A CN 106349038 A CN106349038 A CN 106349038A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract
The invention discloses a method for preparing musk ketone efficiently and mildly. The method comprises the following steps: crushing musk, sieving musk, soaking musk by using ethanol, performing reflux extraction by using ethanol, and performing reflux extraction by using water to obtain a filtrate; soaking a filter residue by using hot water, and performing hot-pressing distillation extraction to obtain a hot-pressed extract; concentrating the hot-pressed extract and the filtrate, centrifuging, washing, and dissolving in distilled water to obtain a dissolved solution; adjusting the pH of the dissolved solution, filtering by using a ceramic membrane, circularly washing, adding pure water for dissolving, decolorizing, filtering, and performing spray drying to obtain the musk ketone. By the method, the purity of the musk ketone can be increased, and reaches above 99%; the preparation process is simple, and easy to operate; a treatment condition is mild, so that the musk ketone is not affected; the extracting effect is good, more than 99% of the musk ketone in the musk can be extracted; the method has the advantages of high efficiency, rapidness, achievement of high purity, and the like.
Description
Technical field
The present invention relates to pharmaceutical technology field, specifically a kind of method efficiently gently preparing muscone.
Background technology
Moschus is that secretions in the male glandular sac of animal in deer family Moschus moschiferouss are dried and form, and is a kind of fine perfumery, if putting a wee bit indoors, will houseful delicate fragrance, abnormal smells from the patient is totally different.Moschus is not only fragrant pleasant, and lasting fragrance.Moschus uses in China, with a long history.The Tang Dynasty poet Tu Fu meets in " Flos Caryophylli " poem: " in the blue Moschus moschiferouss of evening pendant ".Moschus is the important source material preparing senior essence.Ancient times scholar, poet, artist add a little Moschus in first-class Moschus moschiferouss material, make " Moschus moschiferouss ink " and write, draw a picture, fragrance is quiet and beautiful, if calligraphy and painting is sealed appropriate, can preserve for a long time, anti-corrosion mothproof.Moschus is warm in nature, nontoxic, bitter in the mouth.Enter the heart, spleen, Liver Channel, have and have one's ideas straightened out, ward off dirty, dredging collateral, scattered silt function.Cure mainly apoplexy, syncope due to accumulation of phlegm, infantile convulsion, middle evil unhappiness, trusted subordinate sudden and violent pain, traumatic injury, swollen ulcer drug.Many clinical materials show, during patients with coronary heart disease angina pectoris attacks, or when being in faintness shock, take the Soviet Union with Moschus as main component and close ball, the state of an illness can be eased.Moschus mainly contains moisture 23.56%, ash 3.62% (wherein containing potassium, sodium, calcium, magnesium, ferrum, chlorine, sulfate radical, phosphate anion etc.), oxygenatedchemicalss (wherein contain ammonium carbonate 1.15%, the ammonia 1.89% in ammonium salt, carbamide 0.40%, amino acid nitrogen 1.07%, total nitrogen 9.15%), cholesterol 2.19%, crude fibre 0.59%, fatty acid 6.15%Muscone2.2%.Moschus principle active component is muscone, and muscone, as the active component of Moschus, is the aromatic odor main source of Moschus.The process extracting muscone from Moschus is excessively simple, and extraction effect is poor, and purity is low, causes certain loss.
Content of the invention
It is an object of the invention to provide a kind of method efficiently gently preparing muscone that extraction effect is good, quick, purity is high, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the following technical scheme of present invention offer:
A kind of method efficiently gently preparing muscone, comprises the following steps:
1) Moschus is crushed, cross 60-100 mesh sieve, then use 40-50 DEG C of 75-95v% ethanol to soak 3-5 hour, then with 8-15 times of weight 75-95v% alcohol reflux 3-4 time, flow back 3-4h every time, and filtration takes filtering residue, filtrate standby；
2) by filtering residue water reflux, extract, 2-3 time of 8-15 times of weight, extract 3-4h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby；
3) by step 2) in filtering residue with 50-55 DEG C of hot-water soak 4-8 hour, then with the water for injection hot pressing distillation extraction 4-6 hour of 6-9 times of quality, hot pressing is extracted and is needed control container pressure in 0.3-0.5mpa, temperature at 90-125 DEG C, prepared hot pressing extracting solution；
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.05-1.35, addition ethanol, it is centrifuged and must precipitate, wherein centrifugal rotational speed is 11000-14000r/min, and centrifugation time is 30-40min, and centrifugation number of times is 1-3 time；
5) precipitation is washed respectively with the dehydrated alcohol of 3-5 times of weight, acetone successively, the precipitation after washing is distilled water dissolution with 3-5 times, prepared lysate；
6) lysate is adjusted ph for after 4.8-5.5, filtered with the ceramic membrane that membrane aperture is 0.01 μm -2 μm, then the acidic aqueous solution circulation washing ceramic membrane being 4.5-5.5 with ph, abandon filtrate, the alkaline aqueous solution circulation washing ceramic membrane being 7.9-8.6 with ph again, plus pure water is dissolved, obtain aqueous solution；
7) aqueous solution obtaining in step 6) addition decolorising agent is decoloured, temperature during desolventing technology is 42-48 DEG C, bleaching time is 0.8-1.2 hour, decolouring finishes and obtains destaining solution after filtering；
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 120-130 DEG C, and outlet temperature is 105-110 DEG C, obtains final product muscone.
As the further scheme of the present invention: the Moschus after broken in step 1) is soaked 4 hours with 45 DEG C of 95v% ethanol.
As the further scheme of the present invention: in step 1) during alcohol reflux, using 12 times of weight 95v% ethanol.
As the further scheme of the present invention: step 2) in the filtering residue water reflux, extract, of 12 times of weight.
As the further scheme of the present invention: in step 3), hot pressing is extracted needs control container pressure in 0.4mpa, and temperature is at 110 DEG C.
As the further scheme of the present invention: in step 6), acidic aqueous solution adopts hydrochloric acid solution, alkaline aqueous solution adopts sodium hydroxide solution.
As the further scheme of the present invention: in step 7), decolorising agent is activated carbon.
Compared with prior art, the invention has the beneficial effects as follows:
The purity of muscone can be improved by the preparation method of the present invention, reach more than 99%, and preparation process is simple, easy to operate, treatment conditions are gentle, muscone will not be impacted, extraction effect is good, can extract in Moschus more than 99% muscone, has the advantages that efficient, quick, purity is high.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, broadly fall into the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of method efficiently gently preparing muscone, comprise the following steps:
1) Moschus is crushed, cross 60 mesh sieves, then use 40 DEG C of 75v% ethanol to soak 3 hours, then use 8 times of weight 75v% alcohol reflux 3 times, every time backflow 3h, filtration, take filtering residue, filtrate standby.
2) by the filtering residue water reflux, extract, 2 times of 8 times of weight, extract 3h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby.
3) by step 2) in filtering residue with 50 DEG C of hot-water soak 4 hours, then with the water for injection hot pressing distillation extraction 4 hours of 6 times of quality, hot pressing is extracted and is needed control container pressure in 0.3mpa, temperature at 90 DEG C, prepared hot pressing extracting solution.
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.05, add ethanol, be centrifuged and must precipitate, wherein centrifugal rotational speed is 11000r/min, centrifugation time is 30min, centrifugation number of times is 1 time.
5) precipitation is washed respectively with the dehydrated alcohol of 3 times of weight, acetone successively, by the precipitation after washing 3 times of distillation water dissolutioies, prepared lysate.
6) after lysate regulation ph being 4.8, filtered with the ceramic membrane that membrane aperture is 0.01 μm, the acidic aqueous solution circulation washing ceramic membrane being then 4.5 with ph, abandon filtrate, ceramic membrane is washed in the alkaline aqueous solution circulation being 7.9 with ph again, plus pure water is dissolved, and obtains aqueous solution.
7) aqueous solution obtaining in step 6) addition activated carbon is decoloured, temperature during desolventing technology is 42 DEG C, bleaching time is 0.8 hour, and decolouring finishes and obtains destaining solution after filtering.
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 120 DEG C, and outlet temperature is 105 DEG C, obtains final product muscone.
Embodiment 2
In the embodiment of the present invention, a kind of method efficiently gently preparing muscone, comprise the following steps:
1) Moschus is crushed, cross 100 mesh sieves, then use 50 DEG C of 95v% ethanol to soak 5 hours, then use 15 times of weight 95v% alcohol reflux 4 times, every time backflow 4h, filtration, take filtering residue, filtrate standby.
2) by the filtering residue water reflux, extract, 3 times of 15 times of weight, extract 4h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby.
3) by step 2) in filtering residue with 55 DEG C of hot-water soak 8 hours, then with the water for injection hot pressing distillation extraction 6 hours of 9 times of quality, hot pressing is extracted and is needed control container pressure in 0.5mpa, temperature at 125 DEG C, prepared hot pressing extracting solution.
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.35, add ethanol, be centrifuged and must precipitate, wherein centrifugal rotational speed is 14000r/min, centrifugation time is 40min, centrifugation number of times is 3 times.
5) precipitation is washed respectively with the dehydrated alcohol of 5 times of weight, acetone successively, by the precipitation after washing 5 times of distillation water dissolutioies, prepared lysate.
6) after lysate regulation ph being 5.5, filtered with the ceramic membrane that membrane aperture is 2 μm, the acidic aqueous solution circulation washing ceramic membrane being then 5.5 with ph, abandon filtrate, ceramic membrane is washed in the alkaline aqueous solution circulation being 8.6 with ph again, plus pure water is dissolved, and obtains aqueous solution.
7) aqueous solution obtaining in step 6) addition activated carbon is decoloured, temperature during desolventing technology is 48 DEG C, bleaching time is 1.2 hours, and decolouring finishes and obtains destaining solution after filtering.
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 130 DEG C, and outlet temperature is 110 DEG C, obtains final product muscone.
Embodiment 3
In the embodiment of the present invention, a kind of method efficiently gently preparing muscone, comprise the following steps:
1) Moschus is crushed, cross 80 mesh sieves, then use 45 DEG C of 95v% ethanol to soak 4 hours, then use 12 times of weight 95v% alcohol reflux 3 times, every time backflow 3.5h, filtration, take filtering residue, filtrate standby.
2) by the filtering residue water reflux, extract, 2 times of 12 times of weight, extract 3.5h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby.
3) by step 2) in filtering residue with 52 DEG C of hot-water soak 6 hours, then with the water for injection hot pressing distillation extraction 5 hours of 7.5 times of quality, hot pressing is extracted and is needed control container pressure in 0.4mpa, temperature at 110 DEG C, prepared hot pressing extracting solution.
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.2, add ethanol, be centrifuged and must precipitate, wherein centrifugal rotational speed is 13000r/min, centrifugation time is 35min, centrifugation number of times is 2 times.
5) precipitation is washed respectively with the dehydrated alcohol of 4 times of weight, acetone successively, by the precipitation after washing 4 times of distillation water dissolutioies, prepared lysate.
6) after lysate regulation ph being 5.1, filtered with the ceramic membrane that membrane aperture is 0.5 μm, the hydrochloric acid solution circulation washing ceramic membrane being then 5 with ph, abandon filtrate, ceramic membrane is washed in the sodium hydroxide solution circulation being 8.2 with ph again, plus pure water is dissolved, and obtains aqueous solution.
7) aqueous solution obtaining in step 6) addition activated carbon is decoloured, temperature during desolventing technology is 46 DEG C, bleaching time is 1 hour, and decolouring finishes and obtains destaining solution after filtering.
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 125 DEG C, and outlet temperature is 108 DEG C, obtains final product muscone.
Embodiment 4
In the embodiment of the present invention, a kind of method efficiently gently preparing muscone, comprise the following steps:
1) Moschus is crushed, cross 70 mesh sieves, then use 48 DEG C of 85v% ethanol to soak 3.5 hours, then use 10 times of weight 85v% alcohol reflux 4 times, every time backflow 3.8h, filtration, take filtering residue, filtrate standby.
2) by the filtering residue water reflux, extract, 3 times of 10 times of weight, extract 3-4h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby.
3) by step 2) in filtering residue with 54 DEG C of hot-water soak 7 hours, then with the water for injection hot pressing distillation extraction 4.5 hours of 8 times of quality, hot pressing is extracted and is needed control container pressure in 0.5mpa, temperature at 100 DEG C, prepared hot pressing extracting solution.
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.15, add ethanol, be centrifuged and must precipitate, wherein centrifugal rotational speed is 12000r/min, centrifugation time is 38min, centrifugation number of times is 3 times.
5) precipitation is washed respectively with the dehydrated alcohol of 5 times of weight, acetone successively, by the precipitation after washing 4.5 times of distillation water dissolutioies, prepared lysate.
6) after lysate regulation ph being 5.3, filtered with the ceramic membrane that membrane aperture is 1.5 μm, the hydrochloric acid solution circulation washing ceramic membrane being then 5.3 with ph, abandon filtrate, ceramic membrane is washed in the sodium hydroxide solution circulation being 8.4 with ph again, plus pure water is dissolved, and obtains aqueous solution.
7) aqueous solution obtaining in step 6) addition activated carbon is decoloured, temperature during desolventing technology is 44 DEG C, bleaching time is 0.9 hour, and decolouring finishes and obtains destaining solution after filtering.
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 128 DEG C, and outlet temperature is 109 DEG C, obtains final product muscone.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and without departing from the spirit or essential characteristics of the present invention, the present invention can be realized in other specific forms.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is limited by claims rather than described above, it is intended that all changes in the implication and scope of the equivalency of claim that fall are included in the present invention.
In addition, it should be understood that, although this specification is been described by according to embodiment, but not each embodiment only comprises an independent technical scheme, this narrating mode of description is only for clarity, those skilled in the art should using description as an entirety, the technical scheme in each embodiment can also through appropriately combined, formed it will be appreciated by those skilled in the art that other embodiment.
Claims (7)
1. a kind of method efficiently gently preparing muscone is it is characterised in that comprise the following steps:
1) Moschus is crushed, cross 60-100 mesh sieve, then use 40-50 DEG C of 75-95v% ethanol to soak 3-5 hour, then with 8-15 times of weight 75-95v% alcohol reflux 3-4 time, flow back 3-4h every time, and filtration takes filtering residue, filtrate standby；
2) by filtering residue water reflux, extract, 2-3 time of 8-15 times of weight, extract 3-4h every time, filter, collect filtering residue, filtrate is merged with the filtrate in step 1) standby；
3) by step 2) in filtering residue with 50-55 DEG C of hot-water soak 4-8 hour, then with the water for injection hot pressing distillation extraction 4-6 hour of 6-9 times of quality, hot pressing is extracted and is needed control container pressure in 0.3-0.5mpa, temperature at 90-125 DEG C, prepared hot pressing extracting solution；
4) by hot pressing extracting solution and step 2) in merges after filtrate merge, be concentrated into the extractum that relative density at 60 DEG C is 1.05-1.35, addition ethanol, it is centrifuged and must precipitate, wherein centrifugal rotational speed is 11000-14000r/min, and centrifugation time is 30-40min, and centrifugation number of times is 1-3 time；
5) precipitation is washed respectively with the dehydrated alcohol of 3-5 times of weight, acetone successively, the precipitation after washing is distilled water dissolution with 3-5 times, prepared lysate；
6) lysate is adjusted ph for after 4.8-5.5, filtered with the ceramic membrane that membrane aperture is 0.01 μm -2 μm, then the acidic aqueous solution circulation washing ceramic membrane being 4.5-5.5 with ph, abandon filtrate, the alkaline aqueous solution circulation washing ceramic membrane being 7.9-8.6 with ph again, plus pure water is dissolved, obtain aqueous solution；
7) aqueous solution obtaining in step 6) addition decolorising agent is decoloured, temperature during desolventing technology is 42-48 DEG C, bleaching time is 0.8-1.2 hour, decolouring finishes and obtains destaining solution after filtering；
8) destaining solution is taken to be spray-dried, the inlet temperature of spray drying is 120-130 DEG C, and outlet temperature is 105-110 DEG C, obtains final product muscone.
2. the method efficiently gently preparing muscone according to claim 1 is it is characterised in that the Moschus after broken in step 1) is soaked 4 hours with 45 DEG C of 95v% ethanol.
3. the method efficiently gently preparing muscone according to claim 1 is it is characterised in that in step 1) during alcohol reflux, using 12 times of weight 95v% ethanol.
4. the method efficiently gently preparing muscone according to claim 1 is it is characterised in that step 2) in the filtering residue water reflux, extract, of 12 times of weight.
5. the method efficiently gently preparing muscone according to claim 1 it is characterised in that in step 3) hot pressing extract need control container pressure in 0.4mpa, temperature is at 110 DEG C.
6. the method efficiently gently preparing muscone according to claim 1 it is characterised in that in step 6) acidic aqueous solution adopt hydrochloric acid solution, alkaline aqueous solution adopts sodium hydroxide solution.
7. the method efficiently gently preparing muscone according to claim 1 it is characterised in that in step 7) decolorising agent be activated carbon.
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| CN201610001972.1A CN106349038B (en) | 2016-01-06 | 2016-01-06 | A method of preparing muskone |
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Cited By (4)
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| CN110818549A (en) * | 2019-11-13 | 2020-02-21 | 冯桂侠 | Method for preparing muscone |
| CN111557442A (en) * | 2020-05-09 | 2020-08-21 | 邢玉娇 | Proanthocyanidins lycium ruthenicum freeze-dried powder and preparation method thereof |
| CN112624913A (en) * | 2021-01-21 | 2021-04-09 | 彭邯峰 | Method for extracting muscone from musk |
| CN114621071A (en) * | 2022-04-18 | 2022-06-14 | 濮阳市欧亚化工科技有限公司 | Method for continuously decoloring musk ketone by using activated carbon fibers |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114621071A (en) * | 2022-04-18 | 2022-06-14 | 濮阳市欧亚化工科技有限公司 | Method for continuously decoloring musk ketone by using activated carbon fibers |
| CN114621071B (en) * | 2022-04-18 | 2022-12-02 | 濮阳市欧亚化工科技有限公司 | Method for continuously decoloring musk ketone by using activated carbon fibers |
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