CN104274503A - Preparation method and application of helleborus volatile oil - Google Patents
Preparation method and application of helleborus volatile oil Download PDFInfo
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- CN104274503A CN104274503A CN201410550598.1A CN201410550598A CN104274503A CN 104274503 A CN104274503 A CN 104274503A CN 201410550598 A CN201410550598 A CN 201410550598A CN 104274503 A CN104274503 A CN 104274503A
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- Prior art keywords
- volatile oil
- preparation
- chimonanthi praecocis
- radix chimonanthi
- extract
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
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- Pharmacology & Pharmacy (AREA)
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a preparation method and an application of helleborus volatile oil. The preparation method comprises: crushing the medicinal material helleborus, sieving and fermenting for 3-5 days by using biological enzyme; adding the fermented raw material into a supercritical extraction kettle, performing supercritical extraction by using ethanol as an entrainer to obtain an extract; and extracting the extract through an organic solvent to obtain the helleborus volatile oil. Pharmacological experiments show that the obtained helleborus volatile oil has significant antibacterial activity, and can be used in such fields as daily chemicals, medicine and the like.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of Radix Chimonanthi praecocis volatile oil.
Background technology
Miao Ethnomedicine Radix Chimonanthi praecocis is the dry root of Calycanthaceae Chimonanthus praecox (L.) Link. platymiscium Chimonanthus praecox (L.) Link., and its chemical composition is mainly based on volatile oil, alkaloid and coumarin kind compound.Pharmacological research shows, it has the effects such as good easing pain and diminishing inflammation and scavenging free radicals, is the parts of generic medicinal plants of do treatment rheumatic arthralgia among the people.
Volatile oil is the effective constituents in Chinese medicine, widely distributed in plant kingdom, and has multiple pharmacologically active and purposes widely.Be mainly used in varieties of food items, cosmetics of everyday use, making essence to use, to the not yet systematic expansion of the functional study of volatile oil.Now to the research of Radix Chimonanthi praecocis volatile oil more be the antioxidation of volatile oil and the activity of easing pain and diminishing inflammation, and relatively less to its antibacterial activity research.Therefore, to the research of the antibacterial action of Radix Chimonanthi praecocis volatile oil, contribute to the deep development to Radix Chimonanthi praecocis volatile oil, as anticorrosion in food antiseptic, cosmetics of everyday use etc.
By literature search, identical with the present invention open source literature report is had no.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application of Radix Chimonanthi praecocis volatile oil, this volatile oil quality better, purity are high, and antibacterial effect is obvious.
The present invention completes by following technical solution:
A. medical material Radix Chimonanthi praecocis is pulverized, cross 40 mesh sieves, add the cellulase of raw materials quality 1 ~ 3%, spray the acetic acid/sodium acetate buffer of raw materials quality 0.5 ~ 1 times, film wrapped, in 40 ~ 50 DEG C of fermentations 3 ~ 5 days;
B. the raw material after fermentation is joined in supercritical extraction reactor, extracting pressure be 15 ~ 25MPa, extraction temperature is 35 ~ 45 DEG C, CO
2flow be 20 ~ 30kg/h, concentration be 80% ethanol be under the condition of entrainer extract 2 ~ 3h, collect extract;
C. gained extract is again through steps such as organic solvent extraction 2 ~ 3 times, anhydrous sodium sulfate drying, concentrating under reduced pressure, can obtain Radix Chimonanthi praecocis volatile oil.
The activity of the cellulase described in step a is 30 ~ 60U/mg.
Organic solvent described in step c is any one in petroleum ether or ether.
Gained Radix Chimonanthi praecocis volatile oil of the present invention has the application in the medicine of antibacterial, bactericidal action in preparation
Tool of the present invention has the following advantages and effect:
(1) the technology of the present invention route simple possible, mild condition, suitability for industrialized is produced;
(2) leaching process of the present invention carries out in closed system, and operative temperature is low, and therefore volatile ingredient not easily loses, and thermally labile component and oxidizable composition also can not be damaged.
Further illustrate the present invention below in conjunction with detailed description of the invention, but the scope of protection of present invention is not limited to following embodiments.
detailed description of the invention:
Embodiment 1:
Medical material Radix Chimonanthi praecocis is pulverized, crosses 40 mesh sieves, get raw material 5kg, add the cellulase (active is 30U/mg) of raw materials quality 1%, spray the acetic acid/sodium acetate buffer of raw materials quality 0.5 times, film wrapped, in 40 DEG C of fermentations 3 days; Raw material after fermentation is joined in supercritical extraction reactor, extracting pressure be 15MPa, extraction temperature is 40 DEG C, CO
2flow be 25kg/h, concentration be 80% ethanol be extract 2h under the condition of entrainer, collect extract; Gained extract is again through petroleum ether extraction 2 times, and anhydrous sodium sulfate drying, concentrating under reduced pressure recycling design, can obtain lurid Radix Chimonanthi praecocis volatile oil 130mL.
Embodiment 2:
Medical material Radix Chimonanthi praecocis is pulverized, crosses 40 mesh sieves, get raw material 5kg, add the cellulase (active is 60U/mg) of raw materials quality 3%, spray the acetic acid/sodium acetate buffer of raw materials quality 1 times, film wrapped, in 45 DEG C of fermentations 5 days; Raw material after fermentation is joined in supercritical extraction reactor, extracting pressure be 20MPa, extraction temperature is 35 DEG C, CO
2flow be 20kg/h, concentration be 80% ethanol be extract 3h under the condition of entrainer, collect extract; Gained extract is again through extracted with diethyl ether 3 times, and anhydrous sodium sulfate drying, concentrating under reduced pressure recycling design, can obtain lurid Radix Chimonanthi praecocis volatile oil 149mL.
Embodiment 3:
Medical material Radix Chimonanthi praecocis is pulverized, crosses 40 mesh sieves, get raw material 5kg, add the cellulase (active is 50U/mg) of raw materials quality 2%, spray the acetic acid/sodium acetate buffer of raw materials quality 1 times, film wrapped, in 50 DEG C of fermentations 4 days; Raw material after fermentation is joined in supercritical extraction reactor, extracting pressure be 25MPa, extraction temperature is 45 DEG C, CO
2flow be 30kg/h, concentration be 80% ethanol be extract 2.5h under the condition of entrainer, collect extract; Gained extract is again through petroleum ether extraction 2 times, and anhydrous sodium sulfate drying, concentrating under reduced pressure recycling design, can obtain lurid Radix Chimonanthi praecocis volatile oil 138mL.
Embodiment 4: the fungistatic effect of Radix Chimonanthi praecocis volatile oil
1 material
1.1 strain staphylococcus aureuses, escherichia coli, bacillus subtilis and bacillus pyocyaneus.
The agar that 1.2 culture medium M-H broth bouillons add 0.3% makes semisolid culturemedium.
Radix Chimonanthi praecocis volatile oil prepared by 1.3 test product said methods.
2 methods and result
The mensuration of 2.1 MIC adopts micro-agar dilution to measure MIC.Above-mentioned prepared Radix Chimonanthi praecocis volatile oil is done the multiple proportions water dilution of 1:2 ~ 256, get 20 μ L and add in culture hole, then add each bacterium liquid (10 with bouillon agar dilution respectively
7) 200 μ L, mixing, cultivate 24h in 37 DEG C, repeated trials once, the results are shown in Table 1.
The Minimal inhibitory concentration result of table 1 Radix Chimonanthi praecocis volatile oil
Note :-without bacterial growth ,+there is bacterial growth.
3 conclusions
Test shows, after Radix Chimonanthi praecocis volatile oil 8 times dilution, all has significant antibacterial action to staphylococcus aureus, escherichia coli, bacillus subtilis and bacillus pyocyaneus; After 16 times of dilutions, significant antibacterial action is still had to staphylococcus aureus, bacillus subtilis, bacillus pyocyaneus, and stronger than 1% berberine.
Claims (4)
1. a preparation method for Radix Chimonanthi praecocis volatile oil, is characterized in that, comprises the steps:
A. medical material Radix Chimonanthi praecocis is pulverized, cross 40 mesh sieves, add the cellulase of raw materials quality 1 ~ 3%, spray the acetic acid/sodium acetate buffer of raw materials quality 0.5 ~ 1 times, film wrapped, in 40 ~ 50 DEG C of fermentations 3 ~ 5 days;
B. the raw material after fermentation is joined in supercritical extraction reactor, extracting pressure be 15 ~ 25MPa, extraction temperature is 35 ~ 45 DEG C, CO
2flow be 20 ~ 30kg/h, concentration be 80% ethanol be under the condition of entrainer extract 2 ~ 3h, collect extract;
C. gained extract is again through steps such as organic solvent extraction 2 ~ 3 times, anhydrous sodium sulfate drying, concentrating under reduced pressure, can obtain Radix Chimonanthi praecocis volatile oil.
2. the preparation method of a kind of Radix Chimonanthi praecocis volatile oil according to claim 1, is characterized in that, the activity of the cellulase described in step a is 30 ~ 60U/mg.
3. the preparation method of a kind of Radix Chimonanthi praecocis volatile oil according to claim 1, is characterized in that, the organic solvent described in step c is any one in petroleum ether or ether.
4. the Radix Chimonanthi praecocis volatile oil prepared according to method described in claim 1 ~ 3 has the application in the medicine of antibacterial, bactericidal action in preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550598.1A CN104274503A (en) | 2014-10-17 | 2014-10-17 | Preparation method and application of helleborus volatile oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550598.1A CN104274503A (en) | 2014-10-17 | 2014-10-17 | Preparation method and application of helleborus volatile oil |
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| Publication Number | Publication Date |
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| CN104274503A true CN104274503A (en) | 2015-01-14 |
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| CN201410550598.1A Pending CN104274503A (en) | 2014-10-17 | 2014-10-17 | Preparation method and application of helleborus volatile oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105695101A (en) * | 2016-03-17 | 2016-06-22 | 西双版纳版纳药业有限责任公司 | Zingiber purpureum Rosc. volatile oil extracted through supercritical carbon dioxide and preparation method and application of Zingiber purpureum Rosc. volatile oil |
| CN106190579A (en) * | 2016-08-22 | 2016-12-07 | 鹰潭华宝香精香料有限公司 | The method extracting Herba Schizonepetae spice |
| CN107853670A (en) * | 2017-10-30 | 2018-03-30 | 潍坊友容实业有限公司 | A kind of Suaeda salsa biogenic salt extracting method |
| CN110946164A (en) * | 2018-09-26 | 2020-04-03 | 贵州省烟草公司铜仁市公司 | Morus tinctorius disease prevention liquid and application method thereof |
-
2014
- 2014-10-17 CN CN201410550598.1A patent/CN104274503A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105695101A (en) * | 2016-03-17 | 2016-06-22 | 西双版纳版纳药业有限责任公司 | Zingiber purpureum Rosc. volatile oil extracted through supercritical carbon dioxide and preparation method and application of Zingiber purpureum Rosc. volatile oil |
| CN106190579A (en) * | 2016-08-22 | 2016-12-07 | 鹰潭华宝香精香料有限公司 | The method extracting Herba Schizonepetae spice |
| CN107853670A (en) * | 2017-10-30 | 2018-03-30 | 潍坊友容实业有限公司 | A kind of Suaeda salsa biogenic salt extracting method |
| CN110946164A (en) * | 2018-09-26 | 2020-04-03 | 贵州省烟草公司铜仁市公司 | Morus tinctorius disease prevention liquid and application method thereof |
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Application publication date: 20150114 |
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| WD01 | Invention patent application deemed withdrawn after publication |