CN103589515B - Supercritical carbon dioxide extraction method of high-purity lavender essential oil - Google Patents
Supercritical carbon dioxide extraction method of high-purity lavender essential oil Download PDFInfo
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- CN103589515B CN103589515B CN201310522497.9A CN201310522497A CN103589515B CN 103589515 B CN103589515 B CN 103589515B CN 201310522497 A CN201310522497 A CN 201310522497A CN 103589515 B CN103589515 B CN 103589515B
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- 244000178870 Lavandula angustifolia Species 0.000 title claims abstract description 69
- 235000010663 Lavandula angustifolia Nutrition 0.000 title claims abstract description 67
- 239000001102 lavandula vera Substances 0.000 title claims abstract description 24
- 235000018219 lavender Nutrition 0.000 title claims abstract description 24
- 239000000341 volatile oil Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- RHLVCLIPMVJYKS-UHFFFAOYSA-N 3-octanone Chemical compound CCCCCC(=O)CC RHLVCLIPMVJYKS-UHFFFAOYSA-N 0.000 claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012530 fluid Substances 0.000 claims abstract description 19
- WRYLYDPHFGVWKC-UHFFFAOYSA-N 4-terpineol Chemical compound CC(C)C1(O)CCC(C)=CC1 WRYLYDPHFGVWKC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract 2
- CZVXBFUKBZRMKR-UHFFFAOYSA-N lavandulol Chemical compound CC(C)=CCC(CO)C(C)=C CZVXBFUKBZRMKR-UHFFFAOYSA-N 0.000 abstract 2
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 abstract 1
- CZVXBFUKBZRMKR-JTQLQIEISA-N (R)-lavandulol Natural products CC(C)=CC[C@@H](CO)C(C)=C CZVXBFUKBZRMKR-JTQLQIEISA-N 0.000 abstract 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 1
- 239000000171 lavandula angustifolia l. flower oil Substances 0.000 abstract 1
- 229930007744 linalool Natural products 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000014860 sensory perception of taste Effects 0.000 description 4
- 235000011089 carbon dioxide Nutrition 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 244000290333 Vanilla fragrans Species 0.000 description 2
- 235000009499 Vanilla fragrans Nutrition 0.000 description 2
- 235000012036 Vanilla tahitensis Nutrition 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- UWKAYLJWKGQEPM-UHFFFAOYSA-N 3,7-dimethylocta-1,6-dien-3-yl acetate Chemical compound CC(C)=CCCC(C)(C=C)OC(C)=O UWKAYLJWKGQEPM-UHFFFAOYSA-N 0.000 description 1
- 206010013935 Dysmenorrhoea Diseases 0.000 description 1
- 235000001242 French lavender Nutrition 0.000 description 1
- 241000144081 Lavandula dentata Species 0.000 description 1
- 244000178860 Lavandula latifolia Species 0.000 description 1
- 240000007318 Lavandula pedunculata Species 0.000 description 1
- 235000001174 Lavandula pedunculata Nutrition 0.000 description 1
- 241001530572 Lavandula stoechas Species 0.000 description 1
- 235000010661 Lavandula stoechas Nutrition 0.000 description 1
- 241001227551 Lavandula x intermedia Species 0.000 description 1
- 241000337007 Oceania Species 0.000 description 1
- 206010042496 Sunburn Diseases 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002924 anti-infective effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 ethyl pentyl group Chemical group 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
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- 239000010453 quartz Substances 0.000 description 1
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- 210000002374 sebum Anatomy 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a supercritical carbon dioxide extraction method of high-purity lavender essential oil, comprising the following steps: (1) sprinkling an entrainer on lavender and carrying out continuous circulating extraction by the use of a supercritical carbon dioxide fluid; and (2) respectively pouring the extracted carbon dioxide fluid into a primary separator and a secondary separator for separation and discharging a wax component out of the primary separator; and discharging lavender oil out of the secondary separator, wherein the entrainer in the step (1) is one component selected from ethanol, 3-octanone, linalool, lavandulol, lavandayl acetate and 4-terpinenol or a mixture of the above components. The extracted lavender essential oil has high purity and its taste is more natural and pure.
Description
Technical field
The present invention relates to a kind of extracting process of Herba Lysimachiae foenumgraeci quintessence oil, particularly relate to a kind of method of supercritical carbon dioxide extraction high-purity lavender essential oil.
Background technology
Lavandula angustifolia (lavandula pedunculata) belongs to perennial undershrub for Labiatae lavandula angustifolia, about has 28 kinds, and from utilizing object to divide, lavandula angustifolia is divided into essential oil class and views and admires the large class of class two.Lavender for essential oil mainly contains 3 kinds, that is: 1. narrow leaf lavandula angustifolia Lavandula angustifolia Mill, also known as lavandula angustifolia, real lavandula angustifolia; 2. aspic L.latifolia Vill, also known as wide leaf lavandula angustifolia; 3. assorted lavandula angustifolia L.hybrida Rev, is the plant that lavandula angustifolia and aspic are hybridized.Lavender for ornamental mainly contains Helmsdale lavandula angustifolia Lavandula stoechas ' Helmsdale ' and tingia lavandula angustifolia Lavandula dentata etc.Lavandula angustifolia originates in Mediterranean, throughout Europe and Oceania archipelago, after also extensively planted in Britain and Yugoslavia, be a kind of perennial cold-resistant flowers, bluish voilet inflorescence grain husk is long beautiful, is suitable for flower footpath group planting or hedge planting, also can potted plantly views and admires.At Roman period, just oneself is quite general vanilla to lavandula angustifolia, because its effect is maximum, is called as " after vanilla ".
Since eighties of last century to rise the sixties lavandula angustifolia successively in Henan, Shaanxi, the ground such as Gansu and Xinjiang carries out the regional cultivation test of larger area, through facts have proved for many years, lavandula angustifolia is the highest with the fitness of Xinjiang natural environmental condition because of the habit that it likes light, happiness cools.At present, the planting area of Xinjiang lavandula angustifolia mainly concentrates on Yi Li, and the essential oil yield in this area's the highest time can account for more than 90% of the whole nation, is called as in " township of Chinese lavandula angustifolia ".In recent years, the technological development carrying out essential oil high value added product is puted forth effort by Xinjiang Yili of China formation, meets raw material and spice oil at home while the market requirement, is even on sale in Europe and market, the Central Asia.
Take from the essential oil of lavender flower fringe, delicate fragrance is pleasant, and graceful fragrance, as important perfume base, is widely used in the blending of foods and cosmetics.In addition, lavandula angustifolia is just widely used in medical aspect from ancient times, and this can trace back to B.C. the earliest.Persian in ancient times, Greece and Rome think that lavandula angustifolia has the effect of healing wound, and for the sterilization of hospital and ward.Oleum lavandula angustifolia also has relieving mental strain and helping sleep, chills out, and can alleviate dysmenorrhoea and premenstrual intense strain, also can promote cell regeneration, and balance sebum secretion, repairs and burn and sunburn, anti-infective, improves various dermatological conditions etc. and is used to pharmaceutical industries.Along with the change with consumption idea that improves constantly of people's quality of the life, the demand of people to natural perfume grows with each passing day, and objectively needs society to provide how better natural perfume, and this is that the development of lavandula angustifolia industry provides direction and power.
In worldwide, lavandula angustifolia kind complexity is various, and between each kind, derived essential oil and content thereof also exist again larger difference.Usual Herba Lysimachiae foenumgraeci quintessence oil is distributed in whole strain plant, and in spending, content is the highest, and the kind of lavender flower, growth year, collecting time etc. have impact on the output of Herba Lysimachiae foenumgraeci quintessence oil all to a great extent.The method obtaining extract at present from lavandula angustifolia mainly contains traditional steam distillation, organic solvent extractionprocess, supercritical carbon dioxide extraction method etc.How to select rational technical process, obtain higher purity and the sense of taste of the finished product is enjoyed more purely natural, be the problem that fragrance industry needs solution badly always.
Summary of the invention
For above shortcomings in prior art, technical problem to be solved by this invention is to provide a kind of method of supercritical carbon dioxide extraction high-purity lavender essential oil, and the Herba Lysimachiae foenumgraeci quintessence oil purity extracted is higher, and the sense of taste is enjoyed more purely natural.
Technical problem to be solved by this invention, is achieved by the following technical solution:
A method for supercritical carbon dioxide extraction high-purity lavender essential oil, is made up of following step:
(1) entrainment agent is sprayed in lavandula angustifolia, carries out continuous circulation extraction with supercritical carbon dioxide fluid;
(2) CO 2 fluid after extraction is entered successively in primary separator, second-stage separator and is separated, from primary separator, discharge wax component; Oleum lavandula angustifolia is discharged from second-stage separator;
Entrainment agent in described step (1) is one in ethanol, 3-octanone, phantol, acetic acid virtue chapter ester, lavandula angustifolia alcohol, acetic acid lavandula angustifolia ester and 4-terpinenol or its mixture.
The method of described supercritical carbon dioxide extraction high-purity lavender essential oil, is made up of following step:
(1) entrainment agent of the 0.2-0.4% accounting for lavandula angustifolia weight is sprayed in lavandula angustifolia, again lavandula angustifolia is added in extraction kettle, carries out continuous circulation extraction with supercritical carbon dioxide fluid, control extraction kettle temperature 40-55 DEG C, extraction pressure 10-30MPa, extraction time 1-3 hour;
(2) CO 2 fluid after extraction is entered successively in primary separator, second-stage separator and is separated, the flow of CO 2 fluid is 10-30 l/h, wherein, and primary separator pressure 8.5-9.5MPa, flash trapping stage actuator temperature 0-20 DEG C; Second-stage separator pressure 6-8MPa, the second-order separation actuator temperature 25-40 DEG C; Wax component is discharged from primary separator; From second-stage separator, discharge Oleum lavandula angustifolia, heating demulsification type, after water phase separated, obtain finished product Herba Lysimachiae foenumgraeci quintessence oil.The granular size of the lavandula angustifolia in described step (1) is 10-60 order.
Described lavandula angustifolia is selected from the colored fringe of lavandula angustifolia.
Entrainment agent in described step (1) is made up of by weight following component: ethanol 100 parts, 3-octanone 10-20 part, 4-terpinenol 30-50 part.
Described 3-octanone, English name: 3-Octanone, molecular formula: C
8h
16o, molecular weight: 128.21.Boiling point 157 ~ 162 DEG C, relative density 0.819.Chinese another name: ethyl pentyl group (first) ketone; Ethyl n-pentyl ketone; No. CAS: 106-68-3.
Described 4-terpinenol, English name: 4-Terpinenol, molecular formula: C
10h
18o, molecular weight: 154.25.Chinese another name: 4-Sheep's-parsley enol in the Meng, origanol, 1-Foxlene-4-alcohol, 1-methyl-4-sec.-propyl tetrahydrobenzene-4-alcohol.Physico-chemical property: be colourless liquid, be dissolved in the organic flux such as ethanol, there is optically active isomer, boiling point 208 ~ 214 DEG C, relative density 0.926 ~ 0.935.No. CAS: 562-74-3.
Relative to prior art, the invention has the advantages that: the Herba Lysimachiae foenumgraeci quintessence oil purity adopting the present invention to extract is higher, and the sense of taste is enjoyed more purely natural.
Embodiment
By embodiment, the invention will be further described, but the present invention not limited by following examples.
embodiment 1
The lavender flower fringe pulverizer dried in the shade picking up from Xinjiang Yili of China is ground into 30 object fine particles.
Take: ethanol 100 grams, 3-octanone 15 grams and 4-terpinenol 40 grams, be uniformly mixed, obtained mixing entrainment agent.
Mixing entrainment agent 2 grams is sprayed in 700 grams of lavender flower fringes, again the lavender flower fringe after process is added in 5 liters of extraction kettle charging baskets, pass into carbonic acid gas, boosting, continuous circulation extraction is carried out with supercritical carbon dioxide fluid, control extraction kettle temperature 45 C, extraction pressure 25MPa, extraction time 1 hour;
Entered successively in primary separator, second-stage separator by CO 2 fluid after extraction and be separated, the flow of CO 2 fluid is 20 ls/h, wherein, and primary separator pressure 9MPa, flash trapping stage actuator temperature 10 DEG C; Second-stage separator pressure 7MPa, the second-order separation actuator temperature 30 DEG C; Wax component is discharged from primary separator; From second-stage separator, discharge Oleum lavandula angustifolia, heating demulsification type, after water phase separated, obtain finished product Herba Lysimachiae foenumgraeci quintessence oil 24.9 grams.
embodiment 2:
The lavender flower fringe pulverizer dried in the shade picking up from Xinjiang Yili of China is ground into 30 object fine particles.
Entrainment agent ethanol 2 grams is sprayed in 700 grams of lavender flower fringes, again the lavender flower fringe after process is added in 5 liters of extraction kettle charging baskets, pass into carbonic acid gas, boosting, continuous circulation extraction is carried out with supercritical carbon dioxide fluid, control extraction kettle temperature 45 C, extraction pressure 25MPa, extraction time 1 hour;
Entered successively in primary separator, second-stage separator by CO 2 fluid after extraction and be separated, the flow of CO 2 fluid is 20 ls/h, wherein, and primary separator pressure 9MPa, flash trapping stage actuator temperature 10 DEG C; Second-stage separator pressure 7MPa, the second-order separation actuator temperature 30 DEG C; Wax component is discharged from primary separator; From second-stage separator, discharge Oleum lavandula angustifolia, heating demulsification type, after water phase separated, obtain finished product Herba Lysimachiae foenumgraeci quintessence oil 22.5 grams.
comparative example 1:
The lavender flower fringe pulverizer dried in the shade picking up from Xinjiang Yili of China is ground into 30 object fine particles.
Be added in 5 liters of extraction kettle charging baskets by 700 grams of lavender flower fringes, pass into carbonic acid gas, boosting, carries out continuous circulation extraction with supercritical carbon dioxide fluid, controls extraction kettle temperature 45 C, extraction pressure 25MPa, extraction time 1 hour;
Entered successively in primary separator, second-stage separator by CO 2 fluid after extraction and be separated, the flow of CO 2 fluid is 20 ls/h, wherein, and primary separator pressure 9MPa, flash trapping stage actuator temperature 10 DEG C; Second-stage separator pressure 7MPa, the second-order separation actuator temperature 30 DEG C; Wax component is discharged from primary separator; From second-stage separator, discharge Oleum lavandula angustifolia, heating demulsification type, after water phase separated, obtain finished product Herba Lysimachiae foenumgraeci quintessence oil 19.2 grams.
test case:
The difference of embodiment 1-2 and comparative example 1 is: with the addition of entrainment agent in embodiment 1 and embodiment 2, then do not add entrainment agent in comparative example 1.The entrainment agent that embodiment 1 adopts is by the composite mixing entrainment agent of ethanol, 3-octanone and 4-terpinenol, and the entrainment agent that embodiment 2 adopts is ethanol.
The test of validity feature composition relative content is carried out to embodiment 1, embodiment 2 and comparative example 1, the object of test be to compare in essential oil the most effectively, three kinds of compositions of most feature: the height of the relative content summation of phantol, phanteine and acetic acid lavandula angustifolia ester.It has been generally acknowledged that the relative content summation of these three kinds of characteristic components is higher in the world, the purity of Herba Lysimachiae foenumgraeci quintessence oil is higher, and its quality is higher.
Adopt Thermo Focus DSQ chromatograph-mass spectrometer:
Chromatographic column: VF-5ms quartz capillary chromatographic column (30m × 0.25mm × 0.25 μm, Varian)
Column temperature: 60 DEG C (keeping 2 min)-300 DEG C (heat-up rate: 20 DEG C/min, keeps 5 min)
Injector temperature: 250 DEG C
Transmission line temperature: 250 DEG C
Ion source temperature: 250 DEG C
Carrier gas (flow): He (1.0mL/min, >99.999%)
Sample size: 1.0 μ L
Splitting ratio: 250:1
Mass detector: EI source, 70eV
Mass range: 41-350 amu
Retrieval spectrum storehouse: NIST storehouse
Relative content calculates with area normalization method, and concrete test data sees the following form 1.
Table 1: the summation of three characteristic component relative contents
| ? | Content, % |
| Embodiment 1 | 74.2 |
| Embodiment 2 | 72.1 |
| Comparative example 1 | 69.8 |
Visible, the Herba Lysimachiae foenumgraeci quintessence oil purity adopting the present invention to extract is higher, and the sense of taste is enjoyed more purely natural.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope disclosed by the present invention; the change can expected without creative work or replacement, all should be encompassed within protection scope of the present invention.Therefore, the protection domain that protection scope of the present invention should limit with claims is as the criterion.
Claims (3)
1. a method for supercritical carbon dioxide extraction high-purity lavender essential oil, is characterized in that, is made up of following step:
(1) entrainment agent of the 0.2-0.4% accounting for lavandula angustifolia weight is sprayed in lavandula angustifolia, again lavandula angustifolia is added in extraction kettle, carries out continuous circulation extraction with supercritical carbon dioxide fluid, control extraction kettle temperature 40-55 DEG C, extraction pressure 10-30MPa, extraction time 1-3 hour;
(2) CO 2 fluid after extraction is entered successively in primary separator, second-stage separator and is separated, the flow of CO 2 fluid is 10-30 l/h, wherein, and primary separator pressure 8.5-9.5MPa, flash trapping stage actuator temperature 0-20 DEG C; Second-stage separator pressure 6-8MPa, the second-order separation actuator temperature 25-40 DEG C; Wax component is discharged from primary separator; From second-stage separator, discharge Oleum lavandula angustifolia, heating demulsification type, after water phase separated, obtain finished product Herba Lysimachiae foenumgraeci quintessence oil;
Entrainment agent in described step (1) is made up of by weight following component: ethanol 100 parts, 3-octanone 10-20 part, 4-terpinenol 30-50 part.
2. the method for supercritical carbon dioxide extraction high-purity lavender essential oil as claimed in claim 1, is characterized in that: the granular size of the lavandula angustifolia in described step (1) is 10-60 order.
3. the method for supercritical carbon dioxide extraction high-purity lavender essential oil as claimed in claim 1, is characterized in that: the lavandula angustifolia in described step (1) is selected from the colored fringe of lavandula angustifolia.
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