CN102660383B - Separation process of essential oil in toad maggots - Google Patents
Separation process of essential oil in toad maggots Download PDFInfo
- Publication number
- CN102660383B CN102660383B CN 201210179099 CN201210179099A CN102660383B CN 102660383 B CN102660383 B CN 102660383B CN 201210179099 CN201210179099 CN 201210179099 CN 201210179099 A CN201210179099 A CN 201210179099A CN 102660383 B CN102660383 B CN 102660383B
- Authority
- CN
- China
- Prior art keywords
- toad
- essential oil
- toad maggot
- maggot
- pressure
- 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.)
- Expired - Fee Related
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides relates to an extraction separation process of animal fat, in particular to a separation process of essential oil in toad maggots. In consideration that fat components contained in the toad maggots have stronger bioactivity functions of resisting and inhibiting bacteria and resisting viruses, the separation process can be implemented by the following technical scheme: (1) puffing the toad maggots at a low temperature; (2) extracting oil from the toad maggots; (3) carrying out decoloration and deodorization treatment; (4) carrying out filtration and ultrafiltration; and (5) carrying out purification through ultrasonic standing wave liquid chromatography. The method has the following beneficial effect: on the basis of ensuring the bioactivity of the essential oil in the toad maggots, the essential oil in the toad maggots, prepared through separation by adopting the special process, has the advantages of high purity, low cost and easiness in industrial production.
Description
Technical field
The present invention relates to a kind of extraction and separation process of animal grease, especially the separating technology of toad maggot essential oil.
Background technology
The toad maggot is take toad as raw material, processes the maggot that generates through Chinese medicine, contains a large amount of lubricant components in the maggot, and a large amount of basic researchs show that the lubricant component that the toad maggot contains has stronger antibiotic, antibacterial, antiviral bioactive functions.
Application number 201110007300.9 discloses the toad maggot and has separated toad peptide antibiotic and antimicrobial preparation method thereof, take the toad maggot as raw material, adopt water solvent extraction process or dilute alkaline soln extraction process or dilute alcohol solution extraction process, one or more technique purification process in the techniques such as coupled ion exchange resin absorption method, ultrafiltration and micro-filtration, gel chromatography, ultrasonic standing wave preparative liquid chromatogram, vacuum lyophilization is prepared into the toad peptide antibiotic again.
ZL200410013742.4 discloses and has adopted Chinese medicine to cultivate the method for toad maggot, can mass industrialized production toad maggot.
Animal grease extraction and separation method commonly used has the techniques such as milling process, organic solvent lixiviation process, heating stripping method.
Summary of the invention
The lubricant component that contains in view of the toad maggot has stronger antibiotic, antibacterial, antiviral bioactive functions, the invention provides a kind of separating technology of toad maggot essential oil.
Purpose of the present invention can be achieved through the following technical solutions:
(1) toad maggot low temperature expanding: the dry toad maggot of 1000g is packed in the normal temperature expanding apparatus, and be 0.1～3 Mpa to being forced into pressure in installing, hold-time 1～30min, then relief pressure is to normal pressure rapidly, and the toad maggot is by expanded;
(2) extract toad maggot oil: in the expanded solvents system of packing into the extraction element, and adding expanded solvents, be forced into 2～8Mpa and form the expanded solvents system, the maintenance pressure time is 10～30min, keeping temperature is 10～30 ℃, toad maggot oil in the material is extracted out, then with Pressure Drop to normal pressure, form the mixed solution of toad maggot and expanded solvents;
(3) decolouring, take off flavor processes: will add 100～500g atlapulgite in the 1000g mixed solution or gac stirs, place 2～48h under the normal temperature;
(4) filtration and micro-filtration: filter with membrane pore size 20～60 μ m filters, the Microfilter with membrane pore size 0.5～10 μ m filters again, collection filtrate;
(5) ultrasonic standing wave liquid chromatography purifying: filtrate is dissolved in the solvent system, pump into ultrasonic standing wave preparative liquid chromatogram, filtrate and solvent system volume ratio are 1:50～200, the ultrasonic sound intensity 0.2～5KW, frequency 500～1000kHz, UV-detector wavelength 280nm, flow 10～1000mL/min, continuous separate is from being purified into toad maggot essential oil.
Present method is to guarantee on the bioactive basis of toad maggot essential oil, the toad maggot essential oil that adopts special process to separate preparation have purity height, cost low, be easy to suitability for industrialized production, extraction efficiency high, save the energy, do not have the advantage of environmental pollution, the toad maggot essential oil concentration of separation reaches 93～96%.
Description of drawings
Fig. 1 is the structural representation of expanded solvents system extraction element.
Embodiment
Embodiment one: present embodiment is separated toad maggot essential oil according to following step:
(1) the dry toad maggot of 1000g is packed in the normal temperature expanding apparatus (CN200520108339.X), and to being filled with carbonic acid gas in installing and being forced into 0.1～3 Mpa, hold-time 1～30min, then relief pressure is to normal pressure rapidly, and the toad maggot is by expanded;
(2) the toad maggot after expanded joins in the expanded solvents system extraction element, add 1～10kg liquefied carbon dioxide and 0.1～2kg ethyl acetate, be forced into 2～8Mpa, forming the expanded solvents system and keeping temperature is 10～30 ℃, time is 10～30min, then the stripping of toad maggot in material oil reduces that pressure forms the mixed solution of toad maggot and ethyl acetate to normal pressure in the device;
(3) with adding 100～500g atlapulgite in the 1000g mixed solution, place 2～24h under the normal temperature;
(4) filter with membrane pore size 20～60 μ m filters, the Microfilter with membrane pore size 0.5～10 μ m filters again, collects filtrate;
(5) filtrate is dissolved in the solution system that is formed according to the 4:1:1 volume ratio by normal heptane-glacial acetic acid-ethanol, pump into ultrasonic standing wave preparative liquid chromatogram (CN200920274485.8), filtrate and solvent system volume ratio are 1:50～200, the ultrasonic sound intensity 0.2～5KW, frequency 500～1000kHz, flow 10～1000mL/min, UV-detector wavelength 280nm, continuous separate is from being purified into toad maggot essential oil;
(6) essential oil packing.
As shown in Figure 1, the system of expanded solvents described in present embodiment extraction element is by spherical expanded solvents system extractor 1, head tank 2, solid-liquid separator 3, gas-solid separator 4, finished pot 5, external source carbonic acid cylinder 6, carbon dioxide storage tank 7, carbonic acid gas circulating pressure pump 8 and solvent tank 9 form, spherical expanded solvents system extractor 1 by pipeline respectively with head tank 2, solid-liquid separator 3, carbonic acid gas circulating pressure pump 8 and solvent tank 9 are connected, solid-liquid separator 3 is connected with gas-solid separator 4, gas-solid separator 4 is connected with finished pot 5 and carbon dioxide storage tank 7 respectively by pipeline, and carbon dioxide storage tank 7 is connected with external source carbonic acid cylinder 6 and carbonic acid gas circulating pressure pump 8 respectively by pipeline.
Embodiment two: present embodiment is separated toad maggot essential oil according to following step:
(1) during the dry toad maggot of 1000g is packed the normal temperature expanding apparatus into, be filled with 1～5kg nitrogen and be forced into 0.5～1Mpa, the maintenance pressure time is 2～10min, and then relief pressure is to normal pressure rapidly, and the toad maggot is by expanded;
(2) the toad maggot after expanded is packed in the expanded solvents system extraction element, and add 1～10kg liquid carbon dioxide and 0.1～0.5kg dimethyl formamide, be forced into 2～6Mpa and form the expanded solvents system, the maintenance pressure time is 10～30min, keeping temperature is 10～30 ℃, toad maggot oil in the material is extracted out, then with Pressure Drop to normal pressure, form the mixed solution of toad maggot and dimethyl formamide;
(3) stir adding the 100g gac in the 1000g mixed solution, place 24～48h under the normal temperature condition;
(4) filter with membrane pore size 10～60 μ m filters, the Microfilter with membrane pore size 0.5～10 μ m filters again, collects filtrate;
(5) filtrate is dissolved in the solvent system that is formed according to the volume ratio of 10:3:5 by normal heptane-methane dioxide-acetonitrile, pump into ultrasonic standing wave preparative liquid chromatogram, filtrate and solvent system volume ratio are 1:50～100, the ultrasonic sound intensity 0.5～5KW, frequency 500～1000KHz, flow 10～1000mL/min, UV-detector wavelength 280nm, continuous purification go out toad maggot essential oil;
(6) essential oil packing.
Claims (3)
1. the separating technology of a toad maggot essential oil is characterized in that described separating technology is:
(1) toad maggot low temperature expanding: the dry toad maggot of 1000g is packed in the normal temperature expanding apparatus, and be 0.1～3 Mpa to being forced into pressure in installing, hold-time 1～30min, then relief pressure is to normal pressure rapidly, and the toad maggot is by expanded;
(2) extract toad maggot oil: in the expanded solvents system of packing into the extraction element, and add 1～10kg liquefied carbon dioxide and 0.1～2kg ethyl acetate, be forced into 2～8Mpa and form the expanded solvents system, the maintenance pressure time is 10～30min, keeping temperature is 10～30 ℃, toad maggot oil in the material is extracted out, then with Pressure Drop to normal pressure, form the mixed solution of toad maggot and expanded solvents, described expanded solvents system extraction element is by spherical expanded solvents system extractor (1), head tank (2), solid-liquid separator (3), gas-solid separator (4), finished pot (5), external source carbonic acid cylinder (6), carbon dioxide storage tank (7), carbonic acid gas circulating pressure pump (8) and solvent tank (9) form, spherical expanded solvents system extractor (1) by pipeline respectively with head tank (2), solid-liquid separator (3), carbonic acid gas circulating pressure pump (8) and solvent tank (9) are connected, solid-liquid separator (3) is connected with gas-solid separator (4), gas-solid separator (4) is connected with finished pot (5) and carbon dioxide storage tank (7) respectively by pipeline, and carbon dioxide storage tank (7) is connected with external source carbonic acid cylinder (6) and carbonic acid gas circulating pressure pump (8) respectively by pipeline;
(3) decolouring, take off flavor processes: will add 100～500g atlapulgite in the 1000g mixed solution or gac stirs, place 2～48h under the normal temperature;
(4) filtration and micro-filtration: filter with membrane pore size 20～60 μ m filters, the Microfilter with membrane pore size 0.5～10 μ m filters again, collection filtrate;
(5) ultrasonic standing wave liquid chromatography purifying: filtrate is dissolved in the solvent system that is comprised of according to the 4:1:1 volume ratio normal heptane-glacial acetic acid-ethanol, pump into ultrasonic standing wave preparative liquid chromatogram, filtrate and solvent system volume ratio are 1:50～200, the ultrasonic sound intensity 0.2～5KW, frequency 500～1000kHz, UV-detector wavelength 280nm, flow 10～1000mL/min, continuous separate is from being purified into toad maggot essential oil.
2. the separating technology of toad maggot essential oil according to claim 1 is characterized in that in the described step (2), and the expanded solvents system is forced into 2～6Mpa by 1～10kg liquid carbon dioxide and 0.1～0.5kg dimethyl formamide and forms.
3. the separating technology of toad maggot essential oil according to claim 1 is characterized in that in the described step (5), solvent system is comprised of the volume ratio of normal heptane-methane dioxide-acetonitrile according to 10:3:5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210179099 CN102660383B (en) | 2012-06-02 | 2012-06-02 | Separation process of essential oil in toad maggots |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210179099 CN102660383B (en) | 2012-06-02 | 2012-06-02 | Separation process of essential oil in toad maggots |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102660383A CN102660383A (en) | 2012-09-12 |
| CN102660383B true CN102660383B (en) | 2013-04-24 |
Family
ID=46769967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210179099 Expired - Fee Related CN102660383B (en) | 2012-06-02 | 2012-06-02 | Separation process of essential oil in toad maggots |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102660383B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100490C (en) * | 1999-12-01 | 2003-02-05 | 中国科学院动物研究所 | Separation and extraction process of effective component in resource insect |
| CN1798567A (en) * | 2003-05-30 | 2006-07-05 | 三得利株式会社 | Antistress agent |
| CN1869180A (en) * | 2006-06-26 | 2006-11-29 | 王爱民 | Method of extracting fly maggot oil |
| CN101057873A (en) * | 2007-05-15 | 2007-10-24 | 沈荣法 | Method for preparing hepatitis B virus resisting maggot protein powder and its maggot oil and fatty acid |
| CN101348749B (en) * | 2008-09-05 | 2011-11-09 | 王晓峰 | Method for producing fat from screwworm |
| CN101805672B (en) * | 2010-03-08 | 2012-01-25 | 中山大学 | Biodiesel and preparation method thereof |
| CN101880590A (en) * | 2010-06-13 | 2010-11-10 | 中山大学 | Application of Chrysomya megacephala larvae as oil insects |
| CN101880591A (en) * | 2010-06-13 | 2010-11-10 | 中山大学 | Application of housefly maggots as oil material insects |
-
2012
- 2012-06-02 CN CN 201210179099 patent/CN102660383B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102660383A (en) | 2012-09-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104398542B (en) | A kind of method of the extraction and purification flavones from the plant containing flavones | |
| CN103467540B (en) | A kind of method extracting rhodioside from Root of Kirilow Rhodiola | |
| CN102178003A (en) | Process for extracting tea polyphenol | |
| CN106866759B (en) | The technique of grosvenor momordica flavonoid is produced from the waste liquid that Momordica-Glycosides decolorizing resin column is discharged | |
| CN105272956A (en) | Industrial method for preparing roselle anthocyanin from roselle | |
| CN1634914A (en) | Method for producing high pure tea polyphenol with low caffeine | |
| CN101701013A (en) | Method for extracting proanthocyanidin from pine bark by taking water as solvent | |
| CN104059163A (en) | Novel method for preparing Qinghai Qaidam lycium barbarum polysaccharide in extraction and separation manner | |
| CN1301252C (en) | Production method of high purity tea polyphenol and caffeine | |
| CN102488042A (en) | Method for catching tea aroma in instant tea powder production process | |
| CN103613661A (en) | Method of extracting high-purity phycocyanin | |
| CN101560150B (en) | Method for extracting shikimic acid from aniseed | |
| CN103012544A (en) | Method for extracting saponin and polysaccharide from tea-seed pancake | |
| CN102533442B (en) | Method for purifying biodiesel | |
| CN104098633A (en) | Method for extracting anthocyanin from huckleberry | |
| CN103815405B (en) | The production system of cistanche extracts | |
| CN102660383B (en) | Separation process of essential oil in toad maggots | |
| CN104788515B (en) | Method for preparing high-purity water-soluble oleuropein by reduced pressure ultrasonic-assisted extraction | |
| CN110592167B (en) | Purslane polypeptide extract and preparation method thereof | |
| CN108329363A (en) | The minimizing technology of quinhydrones in alpha-arbutin conversion fluid | |
| CN103241747A (en) | Method for purifying KI in perfluoroalkylethyl acrylate synthesized by-product | |
| CN107245046B (en) | A method of extracting separating pepper total alkaloids and capsicum red pigment from capsicum | |
| CN105362300A (en) | Method for using seaweed to prepare concentrated solution rich in seaweed polyphenols | |
| CN102274386A (en) | Method for extracting total isoflavones from Allium mongolicum Regel | |
| CN105315314A (en) | Industrial production method for extracting stachyose from radix rehmanniae |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130424 Termination date: 20180602 |