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
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- CN
- China
- Prior art keywords
- toad
- carbon dioxide
- essential oil
- solvent system
- maggots
- 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
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 21
- 238000000926 separation method Methods 0.000 title claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 13
- 239000003921 oil Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 5
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 230000001007 puffing effect Effects 0.000 claims abstract 3
- 238000004332 deodorization Methods 0.000 claims abstract 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 34
- 239000002904 solvent Substances 0.000 claims description 31
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 238000001471 micro-filtration Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- CDXSJGDDABYYJV-UHFFFAOYSA-N acetic acid;ethanol Chemical compound CCO.CC(O)=O CDXSJGDDABYYJV-UHFFFAOYSA-N 0.000 claims description 2
- WEVYAHXRMPXWCK-UHFFFAOYSA-N acetonitrile Substances CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 2
- 239000000047 product Substances 0.000 claims 2
- 239000004927 clay Substances 0.000 claims 1
- 238000004042 decolorization Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 238000000108 ultra-filtration Methods 0.000 abstract description 2
- 235000019737 Animal fat Nutrition 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 abstract 1
- 241000700605 Viruses Species 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 235000019197 fats Nutrition 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- 230000000975 bioactive effect Effects 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003910 polypeptide antibiotic agent Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- VABXUJRZSJIASG-UHFFFAOYSA-N heptane methane Chemical compound [H]C([H])[H].[H]C([H])[H].[H]C([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])[H] VABXUJRZSJIASG-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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)
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 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201210179099 Expired - Fee Related CN102660383B (en) | 2012-06-02 | 2012-06-02 | Separation process of essential oil in toad maggots |
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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 Chrysocephala maggot as oil-bearing insect |
| CN101880591A (en) * | 2010-06-13 | 2010-11-10 | 中山大学 | Application of housefly maggot as oil insect |
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