CN101204403A - Supercritical extraction processing purified propolis - Google Patents
Supercritical extraction processing purified propolis Download PDFInfo
- Publication number
- CN101204403A CN101204403A CNA2007101915826A CN200710191582A CN101204403A CN 101204403 A CN101204403 A CN 101204403A CN A2007101915826 A CNA2007101915826 A CN A2007101915826A CN 200710191582 A CN200710191582 A CN 200710191582A CN 101204403 A CN101204403 A CN 101204403A
- Authority
- CN
- China
- Prior art keywords
- propolis
- supercritical extraction
- extraction
- purification
- temperature
- 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.)
- Pending
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- 241000241413 Propolis Species 0.000 title claims abstract description 16
- 229940069949 propolis Drugs 0.000 title claims abstract description 16
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 4
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000284 extract Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 flavone compound Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000007766 cera flava Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Jellies, Jams, And Syrups (AREA)
Abstract
The invention provides a purification method of propolis, which comprises the steps of taking propolis as a raw material, extracting effective components in the propolis by using a carbon dioxide supercritical extraction method, and performing purification method by combining gas chromatography-mass spectrometry and controlling temperature and air pressure.
Description
Technical field
The present invention relates to a kind of method of purification of chemical compound, especially a kind of method of purification of propolis.
Background technology
Owing to contain impurity such as Cera Flava, bee body, wood flour and silt in the natural propolis, before use, should carry out roguing earlier extracts refining, traditional method is to leach with ethanol to extract, the effective ingredient that extracts is based on flavone compound, and the effective ingredient that extracts is not a lot, and this has just limited the use of propolis greatly.
Summary of the invention
The present invention is directed to the defective of prior art, a kind of method of purification of propolis is provided.
To achieve these goals, the present invention takes following measure to realize:
A kind of method of purification of propolis includes raw material, and instrument is characterized in that with the propolis being raw material, utilizes the effective ingredient in the carbon dioxide supercritical fluid extraction method bee glue extracting, by gas chromatography-mass spectrography, and the method for purification of control temperature and air pressure.
The present invention has following characteristics with respect to prior art: the present invention adopts supercritical extraction to have characteristics such as low temperature, nontoxic, separation rate height, and this method is used for effective bee glue components and extracts and far surpass traditional Ethanol Method and extract.
The specific embodiment
In concrete the enforcement, following details is arranged:
1. propolis carbon dioxide supercritical extraction method: utilizing the supercritical extraction instrument, is that 46 ℃, extracting pressure are 25MP by extraction temperature, and separation temperature and pressure are respectively 50 ℃ and 7MP, 35 ℃ and 5-6MP, and the extraction time is 3 hours.
2. quantitative analysis: gas chromatography-mass spectrography analyser supercritical extraction propolis is done qualitative and quantitative analysis, the chromatographic column condition is, 5% benzyl polysiloxanes fused-silica capillary column, 260 ℃ of injector temperatures, 80 ℃ of column compartment initial temperatures (3min) rise to 260 ℃ (keeping 30min), carrier gas with 8 ℃ of/minute heating rates, high pure nitrogen, press 71kpa, flow velocity 1ml/min, split ratio 15: 1 before the post, the mass spectrum condition is 280 ℃ a interface temperature, the ionization mode is EI, and electron energy is 70Ev, and ion source temperature is 230 ℃, 150 ℃ of quadrupole rod temperature, tuning manner is that standard is tuning, and the mass scanning mode is SCAN, and solvent delay is 3min, sweep limits is 50-550amu, and electron multiplier voltage is 1635V.
Sample treatment: get the propolis 0.1g of 2 kinds of method extractions respectively, the ethanol with 95% carries out ultrasonic dissolution according to 1: 4 ratio and filters, and 5000r/min is centrifugal, gets supernatant 1 μ l sample introduction.
In the reality, supercritical extraction is suitable for that added value height, content are low, the material of thermal sensitivity, volatile and difficult extraction, and its purification efficiency is higher by 30% than general.
Claims (2)
1. the method for purification of a propolis includes raw material, and instrument is characterized in that with the propolis being raw material, utilizes the effective ingredient in the carbon dioxide supercritical fluid extraction method bee glue extracting, by gas chromatography-mass spectrography, and the method for purification of control temperature and air pressure.
2. according to claim 1, it is characterized in that utilizing the supercritical extraction instrument, is that 46 ℃, extracting pressure are 25MP by extraction temperature, and separation temperature and pressure are respectively 50 ℃ and 7MP, 35 ℃ and 5-6MP, and the extraction time is 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101915826A CN101204403A (en) | 2007-12-13 | 2007-12-13 | Supercritical extraction processing purified propolis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101915826A CN101204403A (en) | 2007-12-13 | 2007-12-13 | Supercritical extraction processing purified propolis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101204403A true CN101204403A (en) | 2008-06-25 |
Family
ID=39565032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101915826A Pending CN101204403A (en) | 2007-12-13 | 2007-12-13 | Supercritical extraction processing purified propolis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101204403A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370667A (en) * | 2011-10-26 | 2012-03-14 | 江苏江大源生态生物科技有限公司 | Method for separating beeswax in propolis through supercritical CO2 |
| CN102512483A (en) * | 2012-01-10 | 2012-06-27 | 吉林大学 | Medicinal composition soft capsules for improving anoxia tolerance and preparation method for medicinal composition soft capsules |
| CN102860971A (en) * | 2012-09-19 | 2013-01-09 | 江苏江大源生态生物科技有限公司 | Compound toothpaste with functions of antisepsis, anti-inflammation, acid prevention and desensitization, and preparation method thereof |
-
2007
- 2007-12-13 CN CNA2007101915826A patent/CN101204403A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102370667A (en) * | 2011-10-26 | 2012-03-14 | 江苏江大源生态生物科技有限公司 | Method for separating beeswax in propolis through supercritical CO2 |
| CN102512483A (en) * | 2012-01-10 | 2012-06-27 | 吉林大学 | Medicinal composition soft capsules for improving anoxia tolerance and preparation method for medicinal composition soft capsules |
| CN102860971A (en) * | 2012-09-19 | 2013-01-09 | 江苏江大源生态生物科技有限公司 | Compound toothpaste with functions of antisepsis, anti-inflammation, acid prevention and desensitization, and preparation method thereof |
| CN102860971B (en) * | 2012-09-19 | 2014-03-26 | 江苏江大源生态生物科技有限公司 | Compound toothpaste with functions of antisepsis, anti-inflammation, acid prevention and desensitization, and preparation method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080625 |