CN112322390A - Method for extracting essential oil of sequoia zhongshanensis - Google Patents
Method for extracting essential oil of sequoia zhongshanensis Download PDFInfo
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- CN112322390A CN112322390A CN202011128288.2A CN202011128288A CN112322390A CN 112322390 A CN112322390 A CN 112322390A CN 202011128288 A CN202011128288 A CN 202011128288A CN 112322390 A CN112322390 A CN 112322390A
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- CN
- China
- Prior art keywords
- essential oil
- extraction
- extract
- taxus chinensis
- sequoia
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- 241001116459 Sequoia Species 0.000 title claims abstract description 47
- 239000000341 volatile oil Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- 241001149649 Taxus wallichiana var. chinensis Species 0.000 claims abstract description 21
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims description 32
- 244000050510 Cunninghamia lanceolata Species 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 244000162450 Taxus cuspidata Species 0.000 claims 1
- 235000009065 Taxus cuspidata Nutrition 0.000 claims 1
- 238000007605 air drying Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001256 steam distillation Methods 0.000 abstract description 2
- 241000196324 Embryophyta Species 0.000 description 4
- 241000218652 Larix Species 0.000 description 3
- 235000005590 Larix decidua Nutrition 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 241001116468 Cunninghamia Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009402 cross-breeding Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 229930015704 phenylpropanoid Natural products 0.000 description 1
- 150000002995 phenylpropanoid derivatives Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting essential oil of taxus chinensis, which comprises the steps of freezing, ball-milling and crushing taxus chinensis leaves, extracting and separating by supercritical carbon dioxide to obtain essential oil of taxus chinensis, and byproducts of the essential oil and wax of the taxus chinensis; wherein the supercritical carbon dioxide extraction is carried out at a low temperature; and then, by steam distillation, the natural components of the essential oil of the sequoia intermedia can be effectively protected from being damaged, no chemical solvent is added, and the obtained essential oil of the sequoia intermedia is natural, pollution-free and pure and rich in smell, so that the technology and product quality guarantee is provided for the production of the essential oil of the sequoia intermedia and the development of related products. The invention has the characteristics of effectively protecting natural components of the sequoia intermedia essential oil from being damaged and having no chemical solvent addition residue.
Description
Technical Field
The invention relates to a method for extracting essential oil of sequoia zhongshanensis, in particular to a method for extracting essential oil of sequoia zhongshanensis, which can effectively protect natural components of the essential oil of the sequoia zhongshanensis from being damaged and has no chemical solvent added and residual.
Background
The said Chinese fir belongs to the genus of larch of the family of Cunninghamia, and is the general name of excellent clone obtained by cross breeding of three species of larch, Sequoia fortunei and Mexico larch.
The sequoia intermedia is a semi-evergreen tall tree, the crown of the tree is conical to wide oval, the leaves are dense, the tree trunk is straight, and the advantages of fast growth, salt and alkali resistance, strong separation resistance, less plant diseases and insect pests, excellent material, long green period, good landscape effect and the like are achieved. The Chinese fir has good ornamental value, is favorable for conserving water sources and maintaining water and soil, and is a novel greening tree species. Meanwhile, the fallen leaves of the sequoia intermedia can improve the soil environment and increase the soil fertility, and the root system of the sequoia intermedia can also play a role in improving the water body, so that the method is widely popularized and applied all over the country.
Supercritical carbon dioxide extraction is a chemical separation technology which is rapidly developed in nearly two-thirty years, and is applied to extraction of natural products by many scholars at home and abroad in recent years, and the achievement is remarkable. Supercritical fluid is a fluid whose temperature and pressure are above the critical temperature and critical pressure, and has the advantages of both liquid and gas. By adjusting the temperature and adding a proper entrainer, the components such as volatile oil, alkaloid, phenylpropanoid, flavonoid, organic phenolic acid, natural pigment and the like can be extracted from the plants. The supercritical carbon dioxide extraction technology usually adopts low-temperature extraction, and is not easy to destroy the heat sensitivity and aroma components of the raw materials, so the supercritical carbon dioxide extraction technology is particularly suitable for extracting volatile components.
At present, the utilization of the sequoia intermedia mainly utilizes the plant characteristics of trees, the deep development and application research of the sequoia intermedia is rare, and the research of extracting effective substances in sequoia intermedia plants does not appear.
Disclosure of Invention
The invention aims to provide a method for extracting essential oil of sequoia intermedia, which can effectively protect natural components of the essential oil of the sequoia intermedia from being damaged and has no chemical solvent added and residual.
The purpose of the invention can be realized by the following technical scheme:
a method for extracting essential oil of taxus chinensis comprises the following steps:
step one, stripping roots and branches of fresh China fir, taking China fir leaves, and softly cleaning the China fir leaves with clear water;
putting the cleaned Chinese fir leaves into dryness, and performing low-temperature blast drying to obtain dried Chinese fir leaves;
step three, immersing the Chinese fir leaves into liquid nitrogen, quickly freezing and drying, then taking out, and putting into a ball mill to be ground into solid particles;
step four, putting the particles into a supercritical carbon dioxide extraction device for extraction, and sequentially passing through a primary separation kettle and a secondary separation kettle to respectively obtain a primary extract and a secondary extract of the taxus chinensis;
step five, injecting distilled water into the primary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a primary mixture of the sequoia intermedia;
step six, distilling and extracting the primary mixture of the sequoia zhongshanensis to obtain a primary distilled extract;
step seven, injecting distilled water into the secondary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a secondary mixture of the sequoia intermedia;
step eight, distilling and extracting the secondary mixture of the sequoia intermedia to obtain a secondary distilled extract;
mixing the primary distilled extract and the secondary distilled extract to obtain the essential oil of the taxus chinensis;
the drying temperature of the low-temperature blast drying in the second step is 50-60 ℃;
the size of the solid particles in the third step is 50-80 meshes;
the distillation and extraction temperature in the sixth step and the eighth step is 50-60 ℃;
the volume ratio of the primary extract of the taxus chinensis to the distilled water in the step five is 1: 10;
the volume ratio of the secondary extract of the sequoia intermedia in the seventh step to the distilled water is 1: 10;
the heating temperature of the distillation extraction in the sixth step is 120 ℃, and the extraction temperature is 105 ℃; the extraction frequency is 6 hours/time, and the extraction times are 2 times;
heating temperature of distillation extraction in the step eight is 120 ℃, and extraction temperature is 105 ℃; the extraction frequency was 6 hours/time, and the extraction frequency was 2 times.
The invention provides a method for extracting essential oil of sequoia intermedia, which has the characteristics of effectively protecting natural components of the essential oil of sequoia intermedia from being damaged and having no chemical solvent addition residue. The high-valued and full-component utilization of the Chinese fir residues are innovated, and the high-quality development of the Chinese fir is realized.
Detailed Description
The purpose of the invention can be realized by the following technical scheme:
a method for extracting essential oil of taxus chinensis comprises the following steps:
step one, stripping roots and branches of fresh China fir, taking China fir leaves, and softly cleaning the China fir leaves with clear water;
putting the cleaned Chinese fir leaves into dryness, and performing low-temperature blast drying to obtain dried Chinese fir leaves;
step three, immersing the Chinese fir leaves into liquid nitrogen, quickly freezing and drying, then taking out, and putting into a ball mill to be ground into solid particles;
step four, putting the particles into a supercritical carbon dioxide extraction device for extraction, and sequentially passing through a primary separation kettle and a secondary separation kettle to respectively obtain a primary extract and a secondary extract of the taxus chinensis;
step five, injecting distilled water into the primary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a primary mixture of the sequoia intermedia;
step six, distilling and extracting the primary mixture of the sequoia zhongshanensis to obtain a primary distilled extract;
step seven, injecting distilled water into the secondary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a secondary mixture of the sequoia intermedia;
step eight, distilling and extracting the secondary mixture of the sequoia intermedia to obtain a secondary distilled extract;
mixing the primary distilled extract and the secondary distilled extract to obtain the essential oil of the taxus chinensis;
the drying temperature of the low-temperature blast drying in the second step is 50-60 ℃;
the size of the solid particles in the third step is 50-80 meshes;
the distillation and extraction temperature in the sixth step and the eighth step is 50-60 ℃;
the volume ratio of the primary extract of the taxus chinensis to the distilled water in the step five is 1: 10;
the volume ratio of the secondary extract of the sequoia intermedia in the seventh step to the distilled water is 1: 10;
the heating temperature of the distillation extraction in the sixth step is 120 ℃, and the extraction temperature is 105 ℃; the extraction frequency is 6 hours/time, and the extraction times are 2 times;
heating temperature of distillation extraction in the step eight is 120 ℃, and extraction temperature is 105 ℃; the extraction frequency was 6 hours/time, and the extraction frequency was 2 times.
The invention has the beneficial effects that:
the method comprises the steps of freezing, ball-milling and crushing Chinese fir leaves, and extracting and separating the Chinese fir leaves by supercritical carbon dioxide to obtain Chinese fir essential oil and byproducts thereof, namely Chinese fir heavy oil and Chinese fir wax; wherein the supercritical carbon dioxide extraction is carried out at a low temperature; and then, by steam distillation, the natural components of the essential oil of the sequoia intermedia can be effectively protected from being damaged, no chemical solvent is added, and the obtained essential oil of the sequoia intermedia is natural, pollution-free and pure and rich in smell, so that the technology and product quality guarantee is provided for the production of the essential oil of the sequoia intermedia and the development of related products.
The invention provides a method for extracting essential oil of sequoia intermedia, which has the characteristics of effectively protecting natural components of the essential oil of sequoia intermedia from being damaged and having no chemical solvent addition residue. The high-valued and full-component utilization of the Chinese fir residues are innovated, and the high-quality development of the Chinese fir is realized.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the invention as defined in the following claims.
Claims (8)
1. A method for extracting essential oil of taxus cuspidata is characterized by comprising the following steps;
step one, stripping roots and branches of fresh China fir, taking China fir leaves, and softly cleaning the China fir leaves with clear water;
putting the cleaned Chinese fir leaves into dryness, and performing low-temperature blast drying to obtain dried Chinese fir leaves;
step three, immersing the Chinese fir leaves into liquid nitrogen, quickly freezing and drying, then taking out, and putting into a ball mill to be ground into solid particles;
step four, putting the particles into a supercritical carbon dioxide extraction device for extraction, and sequentially passing through a primary separation kettle and a secondary separation kettle to respectively obtain a primary extract and a secondary extract of the taxus chinensis;
step five, injecting distilled water into the primary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a primary mixture of the sequoia intermedia;
step six, distilling and extracting the primary mixture of the sequoia zhongshanensis to obtain a primary distilled extract;
step seven, injecting distilled water into the secondary extract of the sequoia intermedia, and stirring and mixing uniformly to obtain a secondary mixture of the sequoia intermedia;
step eight, distilling and extracting the secondary mixture of the sequoia intermedia to obtain a secondary distilled extract;
and step nine, mixing the primary distilled extract and the secondary distilled extract to obtain the essential oil of the taxus chinensis.
2. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the drying temperature of the low-temperature forced air drying in the second step is 50-60 ℃.
3. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the size of solid particles in the step three is 50-80 meshes.
4. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the distillation extraction temperature in the sixth step and the eighth step is 50-60 ℃.
5. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the volume ratio of the primary extract of taxus chinensis to distilled water in the step five is 1: 10.
6. The method for extracting essential oil of sequoia intermedia as claimed in claim 1, wherein the volume ratio of the secondary extract of sequoia intermedia to distilled water in the seventh step is 1: 10.
7. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the heating temperature for distillation and extraction in the sixth step is 120 ℃, and the extraction temperature is 105 ℃; the extraction frequency was 6 hours/time, and the extraction frequency was 2 times.
8. The method for extracting essential oil of taxus chinensis as claimed in claim 1, wherein the heating temperature for distillation and extraction in the step eight is 120 ℃, and the extraction temperature is 105 ℃; the extraction frequency was 6 hours/time, and the extraction frequency was 2 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011128288.2A CN112322390A (en) | 2020-10-20 | 2020-10-20 | Method for extracting essential oil of sequoia zhongshanensis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011128288.2A CN112322390A (en) | 2020-10-20 | 2020-10-20 | Method for extracting essential oil of sequoia zhongshanensis |
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| CN112322390A true CN112322390A (en) | 2021-02-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011128288.2A Pending CN112322390A (en) | 2020-10-20 | 2020-10-20 | Method for extracting essential oil of sequoia zhongshanensis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113652305A (en) * | 2021-07-27 | 2021-11-16 | 中南林业科技大学 | Elaeagnus pungens essential oil extracted by supercritical carbon dioxide fluid and preparation method thereof |
| CN113951271A (en) * | 2021-11-24 | 2022-01-21 | 安徽农业大学 | Plant-derived synergist of emamectin benzoate |
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| CN104622759A (en) * | 2015-02-11 | 2015-05-20 | 广州赛莱拉干细胞科技股份有限公司 | Extracting method and application for adenium obesum leaf cell extract |
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| CN109673674A (en) * | 2018-12-18 | 2019-04-26 | 安徽农业大学 | Middle mountain China fir essential oil and its application in inhibition phytopathogen |
| CN110003982A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combined type borneol method of extraction of essential oil |
| CN110862869A (en) * | 2019-11-15 | 2020-03-06 | 广东暨晴生物医药科技有限公司 | By using supercritical CO2Method for preparing folium artemisiae argyi essential oil and byproducts thereof by extraction and secondary molecular distillation processes |
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2020
- 2020-10-20 CN CN202011128288.2A patent/CN112322390A/en active Pending
Patent Citations (7)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113951271A (en) * | 2021-11-24 | 2022-01-21 | 安徽农业大学 | Plant-derived synergist of emamectin benzoate |
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