CN112336767A - Method for extracting effective components from sweet osmanthus - Google Patents
Method for extracting effective components from sweet osmanthus Download PDFInfo
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- CN112336767A CN112336767A CN202011371851.9A CN202011371851A CN112336767A CN 112336767 A CN112336767 A CN 112336767A CN 202011371851 A CN202011371851 A CN 202011371851A CN 112336767 A CN112336767 A CN 112336767A
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- 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)
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- 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
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- A—HUMAN NECESSITIES
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- 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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- 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
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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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Abstract
The invention provides a method for extracting effective components from osmanthus fragrans, and belongs to the technical field of plant component extraction. The method solves the technical problems of serious loss of effective component extraction components in the existing sweet osmanthus. The method for extracting the effective components in the osmanthus comprises the following steps: step a, grinding sweet osmanthus into uniform powder by liquid nitrogen; b, putting the powder in the step a into an extracting agent, and fully mixing the powder in the step a in an ultrasonic oscillation mode; then centrifuging the filtrate, precipitating, discarding the precipitate, and collecting the supernatant; and c, separating the supernatant obtained by centrifuging through high performance liquid chromatography. The invention improves the loss of volatile components in the osmanthus or active components in cells which are difficult to dissolve out to a great extent.
Description
Technical Field
The invention belongs to the technical field of plant component extraction processes, and relates to a method for extracting effective components from osmanthus fragrans.
Background
At present, the known extraction mode of sweet osmanthus flavone is mostly in the form of ether extraction, and changes and improvements are mostly made on the basis in order to maintain the bioactivity of sweet osmanthus flavone and ensure the yield of sweet osmanthus flavone; the extraction mode of polysaccharide substances in the sweet osmanthus leaves also adopts an ethanol reflux mode. Meanwhile, in the aspect of detection, only a gas chromatograph is used for detection. The extraction method and detection of the sweet osmanthus are still more traditional and single; thereby causing serious loss of various effective components in the osmanthus fragrans.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for extracting effective components from osmanthus fragrans, and the technical problems to be solved by the invention are as follows: how to effectively reduce the loss of effective components in the osmanthus fragrans.
The purpose of the invention can be realized by the following technical scheme:
a method for extracting effective components from sweet osmanthus is characterized by comprising the following steps:
step a, grinding sweet osmanthus into uniform powder by liquid nitrogen;
b, putting the powder in the step a into an extracting agent, and fully mixing the powder in the step a in an ultrasonic oscillation mode; then centrifuging the filtrate, precipitating, discarding the precipitate, and collecting the supernatant;
and c, separating the supernatant obtained by centrifuging through high performance liquid chromatography.
The working principle is as follows: the inventor of the present invention researches the loss situation of active ingredients caused by cell disruption in plant extraction by summarizing the limiting conditions in the extraction process of osmanthus fragrans, further explores the extraction method of the effective ingredients of osmanthus fragrans, and finally forms the extraction method of the effective ingredients in osmanthus fragrans; thoroughly crushing the floral tissue of the sweet osmanthus into uniform powder in a liquid nitrogen grinding mode, adding petroleum ether extract, fully mixing in an ultrasonic oscillation mode, and then obtaining the active ingredients through centrifugal separation. The analysis of test data proves that the loss of volatile components in the osmanthus fragrans or active components in cells which are difficult to dissolve out is greatly improved by adopting the technical scheme; can simultaneously extract various active substances in the sweet osmanthus, and greatly improves the available medicinal value of the sweet osmanthus.
In the above method for extracting the effective components from osmanthus fragrans, the extractant in step b is petroleum ether; specifically, the paint comprises 50% of ethanol, 25% of ethyl acetate and 25% of petroleum ether by volume percentage.
In the above method for extracting effective components from osmanthus fragrans, in the step b, the centrifugal rotation speed is 12000 r/min; the centrifugation time was 10 min.
In the above method for extracting effective components from osmanthus fragrans, in the step b, the centrifugal rotation speed is 12000 r/min; the centrifugation time was 10 min.
In the method for extracting the effective components from the sweet osmanthus, in the step b, the ultrasonic oscillation frequency is 20-80 KHz; the ultrasonic oscillation time is 8-12 min.
In the above method for extracting effective components from flos Osmanthi Fragrantis, preferably, the ultrasonic oscillation frequency is 60 KHz; the ultrasonic oscillation time is 10 min.
In the method for extracting the effective components from the osmanthus fragrans, in the step b, the material-liquid ratio of the osmanthus fragrans powder to the extracting agent is 1:5-1: 12(g: ml).
In the above method for extracting effective components from flos Osmanthi Fragrantis, preferably, the ratio of flos Osmanthi Fragrantis powder and extractant is 1 g: 9 ml.
Compared with the prior art, the extraction method of the invention greatly improves the loss of volatile components in the osmanthus or active components in cells which are difficult to dissolve out; can simultaneously extract various active substances in the sweet osmanthus, and greatly improves the available medicinal value of the sweet osmanthus.
Drawings
FIG. 1 is a graph showing the results of extraction and soaking of the four-season cinnamon with petroleum ether.
FIG. 2 is a graph showing the results of the extraction of the four seasons with petroleum ether and the soaking with liquid nitrogen.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
In the embodiment, the cinnamomum japonicum and the cinnamomum japonicum are extracted by adopting an ether extractant (50% of ethanol, 25% of ether and 25% of ethyl acetate) and a petroleum ether extractant (50% of ethanol, 25% of petroleum ether and 25% of ethyl acetate) respectively. The extraction agent is adopted to directly soak for 10 minutes and is compared with ultrasonic oscillation for 10 minutes, the osmanthus fragrans is directly soaked and is compared with soaking after liquid nitrogen grinding, the osmanthus fragrans is directly soaked and is compared with soaking after ultrasonic oscillation for 10 minutes, and the like, and a proper effective component extraction method is found by comparing the difference of different types of osmanthus fragrans under the same treatment.
In this example, a liquid phase method was performed by scanning with dual wavelengths, starting at 245nm and 210nm, and performing at a flow rate of 1.00 mL/min. The mobile phase is A: water phase, B: methanol. A chromatographic column: VP-ODSC18 column. The experiment was carried out in binary gradient using Shimadzu 20AT HPLC.
Example one
Adding the dried sweet osmanthus into 10ml of extracting agent (50% of ethanol, 25% of diethyl ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, discarding precipitate, and collecting supernatant for use; the supernatant from the centrifugation was separated by high performance liquid chromatography.
Example two
Grinding the dried sweet osmanthus into uniform powder by liquid nitrogen, and adding the powder into 10ml of an extracting agent (50% of ethanol, 25% of diethyl ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, discarding precipitate, and collecting supernatant for use; the supernatant from the centrifugation was separated by high performance liquid chromatography. The contents of the four-season cinnamon and the golden cinnamon are not obviously changed.
EXAMPLE III
Adding the dried sweet osmanthus into 10ml of extracting agent (50% of ethanol, 25% of diethyl ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, ultrasonically shaking for 10min, discarding the precipitate, and collecting the supernatant; the supernatant from the centrifugation was separated by high performance liquid chromatography. The content of the osmanthus fragrans is shown to increase, and the content of the osmanthus fragrans is shown to decrease.
Example four
Grinding the dried sweet osmanthus into uniform powder by liquid nitrogen, and adding the powder into 10ml of an extracting agent (50% of ethanol, 25% of diethyl ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, ultrasonically shaking for 10min, discarding the precipitate, and collecting the supernatant; the supernatant from the centrifugation was separated by high performance liquid chromatography. The contents of both the osmanthus fragrans and the four-season osmanthus fragrans are shown to be increased.
EXAMPLE five
Adding the dried sweet osmanthus into 10ml of an extracting agent (50% of ethanol, 25% of petroleum ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, discarding precipitate, and collecting supernatant for use; the supernatant from the centrifugation was separated by high performance liquid chromatography. The content of the osmanthus fragrans is shown to increase, and the content of the osmanthus fragrans is shown to decrease.
EXAMPLE six
Grinding the dried sweet osmanthus into uniform powder by liquid nitrogen, and adding the powder into 10ml of an extracting agent (50% of ethanol, 25% of petroleum ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, discarding precipitate, and collecting supernatant for use; the supernatant from the centrifugation was separated by high performance liquid chromatography. The contents of the Jingui and the Sijigui are slightly changed.
EXAMPLE seven
Adding the dried sweet osmanthus into 10ml of an extracting agent (50% of ethanol, 25% of petroleum ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, ultrasonically shaking for 10min, discarding the precipitate, and collecting the supernatant; the supernatant from the centrifugation was separated by high performance liquid chromatography. The Jingui and the Sijigui have no obvious change.
Example eight
Grinding the dried sweet osmanthus into uniform powder by liquid nitrogen, and adding the powder into 10ml of an extracting agent (50% of ethanol, 25% of petroleum ether and 25% of ethyl acetate); centrifuging the filtrate at 12000 r/min; centrifuging for 10 min; precipitating, ultrasonically shaking for 10min, discarding the precipitate, and collecting the supernatant; the supernatant from the centrifugation was separated by high performance liquid chromatography. The contents of the osmanthus fragrans and the four seasons osmanthus fragrans are obviously increased as shown by results.
In the above embodiment, in the range of the petroleum ether ratio of 1:5 to 1:9(g: ml), the extraction rate of the osmanthus essential oil is obviously increased along with the increase of the material-liquid ratio, and when the material-liquid ratio exceeds 1 g: 9ml, the extraction rate is not obviously increased. The reason is that for a certain amount of osmanthus fragrans, the larger the material-liquid ratio is, the larger the concentration difference of the contact surface of the osmanthus fragrans and petroleum ether is. The ultrasonic frequency is in the range of 20-60KHz, the extraction rate of the essential oil is increased along with the increase of the ultrasonic frequency, when the ultrasonic frequency is 60KHz, the extraction rate reaches the maximum value, and when the ultrasonic frequency exceeds 60KHz, the extraction rate is reduced along with the increase of the ultrasonic frequency.
Fig. 1 shows that the preserved sizang cassia is soaked in petroleum ether for 10 minutes after being dried, and the supernatant is detected by a liquid chromatograph. From the graph, it can be seen that the main component content can be extracted from petroleum ether soaking.
Fig. 2 shows the detection results of the active ingredients obtained by drying the preserved sika, grinding the dried sika into uniform powder by liquid nitrogen, and soaking the powder; as can be seen from the retention time shown in FIGS. 1 and 2, the main ingredients of the four-season cinnamon can be fully contacted with petroleum ether after being ground into powder, and can be released into the solution.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (9)
1. A method for extracting effective components from sweet osmanthus is characterized by comprising the following steps:
step a, grinding sweet osmanthus into uniform powder by liquid nitrogen;
b, putting the powder in the step a into an extracting agent, and fully mixing the powder in the step a in an ultrasonic oscillation mode; then centrifuging the filtrate, precipitating, discarding the precipitate, and collecting the supernatant;
and c, separating the supernatant obtained by centrifuging through high performance liquid chromatography.
2. The method for extracting effective components from osmanthus fragrans according to claim 1, wherein the extractant in the step b is petroleum ether.
3. The method for extracting effective components from osmanthus fragrans according to claim 1 or 2, wherein the extracting agent in the step b is a petroleum ether solution comprising 50% by volume of ethanol, 25% by volume of ethyl acetate and 25% by volume of petroleum ether.
4. The method for extracting the effective components in the osmanthus fragrans according to claim 1 or 2, wherein in the step b, the centrifugal rotating speed is 11000r/min to 13000 r/min; the centrifugation time is 8 min-12 min.
5. The method for extracting effective components from osmanthus fragrans according to claim 4, wherein in the step b, the centrifugal rotation speed is 12000 r/min; the centrifugation time was 10 min.
6. The method for extracting the effective components from the osmanthus fragrans according to claim 1 or 2, wherein in the step b, the ultrasonic oscillation frequency is 20-80 KHz; the ultrasonic oscillation time is 8-12 min.
7. The method for extracting effective components from osmanthus fragrans according to claim 6, wherein in the step b, the ultrasonic oscillation frequency is 60 KHz; the ultrasonic oscillation time is 10 min.
8. The method for extracting effective components from osmanthus fragrans according to claim 1 or 2, wherein in the step b, the ratio of the osmanthus fragrans powder to the extracting agent is 1:5 to 1:12(g: ml).
9. The method for extracting effective components from osmanthus fragrans according to claim 8, wherein in the step b, the ratio of the osmanthus fragrans powder to the extracting agent is 1g to 9 ml.
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| CN202011371851.9A CN112336767A (en) | 2020-11-30 | 2020-11-30 | Method for extracting effective components from sweet osmanthus |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654616A (en) * | 2005-01-24 | 2005-08-17 | 中国林业科学研究院林产化学工业研究所 | combined extraction method for rosemary essential oil and rosemary antioxidant |
| CN107674452A (en) * | 2017-11-17 | 2018-02-09 | 长沙理工大学 | A kind of method for extracting orange osmanthus anthoxanthin |
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2020
- 2020-11-30 CN CN202011371851.9A patent/CN112336767A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654616A (en) * | 2005-01-24 | 2005-08-17 | 中国林业科学研究院林产化学工业研究所 | combined extraction method for rosemary essential oil and rosemary antioxidant |
| CN107674452A (en) * | 2017-11-17 | 2018-02-09 | 长沙理工大学 | A kind of method for extracting orange osmanthus anthoxanthin |
Non-Patent Citations (1)
| Title |
|---|
| 郑义；等: "桂花精油提取工艺及其成分分析", 《江苏农业科学》 * |
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