CN113372997A - Method for carrying out segmented temperature control extraction on main components of rosemary - Google Patents
Method for carrying out segmented temperature control extraction on main components of rosemary Download PDFInfo
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- CN113372997A CN113372997A CN202110669778.1A CN202110669778A CN113372997A CN 113372997 A CN113372997 A CN 113372997A CN 202110669778 A CN202110669778 A CN 202110669778A CN 113372997 A CN113372997 A CN 113372997A
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- 238000000605 extraction Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 241001529742 Rosmarinus Species 0.000 title claims abstract description 20
- 239000003921 oil Substances 0.000 claims abstract description 92
- 239000011550 stock solution Substances 0.000 claims abstract description 26
- GRWFGVWFFZKLTI-UHFFFAOYSA-N α-pinene Chemical compound CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 claims abstract description 22
- CRPUJAZIXJMDBK-UHFFFAOYSA-N camphene Chemical compound C1CC2C(=C)C(C)(C)C1C2 CRPUJAZIXJMDBK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000341 volatile oil Substances 0.000 claims abstract description 19
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- GRWFGVWFFZKLTI-IUCAKERBSA-N 1S,5S-(-)-alpha-Pinene Natural products CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 claims abstract description 11
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 claims abstract description 11
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Primaeres Camphenhydrat Natural products C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229930006739 camphene Natural products 0.000 claims abstract description 10
- ZYPYEBYNXWUCEA-UHFFFAOYSA-N camphenilone Natural products C1CC2C(=O)C(C)(C)C1C2 ZYPYEBYNXWUCEA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001256 steam distillation Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 claims description 20
- WEEGYLXZBRQIMU-UHFFFAOYSA-N Eucalyptol Chemical compound C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 claims description 18
- KGEKLUUHTZCSIP-HOSYDEDBSA-N [(1s,4s,6r)-1,7,7-trimethyl-6-bicyclo[2.2.1]heptanyl] acetate Chemical compound C1C[C@]2(C)[C@H](OC(=O)C)C[C@H]1C2(C)C KGEKLUUHTZCSIP-HOSYDEDBSA-N 0.000 claims description 16
- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 claims description 16
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims description 16
- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 claims description 16
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 claims description 10
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 claims description 10
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 claims description 10
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 10
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 claims description 10
- 241000723346 Cinnamomum camphora Species 0.000 claims description 10
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 claims description 10
- 229940116229 borneol Drugs 0.000 claims description 10
- 229930008380 camphor Natural products 0.000 claims description 10
- 229960000846 camphor Drugs 0.000 claims description 10
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 claims description 10
- 229930007744 linalool Natural products 0.000 claims description 10
- WTARULDDTDQWMU-RKDXNWHRSA-N (+)-β-pinene Chemical compound C1[C@H]2C(C)(C)[C@@H]1CCC2=C WTARULDDTDQWMU-RKDXNWHRSA-N 0.000 claims description 8
- WTARULDDTDQWMU-IUCAKERBSA-N (-)-Nopinene Natural products C1[C@@H]2C(C)(C)[C@H]1CCC2=C WTARULDDTDQWMU-IUCAKERBSA-N 0.000 claims description 8
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 claims description 8
- WTARULDDTDQWMU-UHFFFAOYSA-N Pseudopinene Natural products C1C2C(C)(C)C1CCC2=C WTARULDDTDQWMU-UHFFFAOYSA-N 0.000 claims description 8
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 claims description 8
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 claims description 8
- 229940088601 alpha-terpineol Drugs 0.000 claims description 8
- 229930006722 beta-pinene Natural products 0.000 claims description 8
- LCWMKIHBLJLORW-UHFFFAOYSA-N gamma-carene Natural products C1CC(=C)CC2C(C)(C)C21 LCWMKIHBLJLORW-UHFFFAOYSA-N 0.000 claims description 8
- 229940087305 limonene Drugs 0.000 claims description 8
- 235000001510 limonene Nutrition 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229930000044 secondary metabolite Natural products 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 description 13
- 229940115397 bornyl acetate Drugs 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 244000178231 Rosmarinus officinalis Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000000243 solution Substances 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
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)
- Fats And Perfumes (AREA)
Abstract
The invention relates to the technical field of secondary metabolite extraction, and discloses a method for carrying out segmented temperature control extraction on main components of rosemary, which comprises the following steps: the water in the jacket of the essential oil extraction tank is changed into heat conducting oil, the traditional steam distillation method is changed into an oil bath method, a temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction; the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 5 minutes; and when the oil temperature of the heat conducting oil is in a first temperature range, extracting alpha-pinene and camphene in the stock solution. The method for extracting the rosemary essential oil by segmented temperature control divides 5 types of main components with different weights according to functionality, can basically meet the type requirements of the current rosemary essential oil market, is suitable for large-scale factory production, and is convenient for rapid market circulation.
Description
Technical Field
The invention relates to the technical field of secondary metabolite extraction, in particular to a method for carrying out segmented temperature control extraction on main components of rosemary.
Background
Rosemary is shrub with a height of 2 m, cylindrical stems and old branches, is densely covered by white star-shaped fine villi, is native to European and North African Mediterranean coasts, is an aromatic oil plant, can extract oil from short branches of leaves and flowers 3 times per year, has an oil content of 0.19-1.7%, can be used as a raw material of soap or essence for daily use, and can also be used as a garden ornamental plant. According to different efficacies and market demands, rosemary essential oil is divided into verbenam type, 1, 8-cineole type, camphor type and the like.
The rosemary essential oil is mainly extracted and collected by steam distillation, because different components have different boiling points, some components with low boiling points are easily degraded at high temperature in a long-time extraction process or diluted by other components with high boiling points, so that the content of target components in the finally obtained product is insufficient; meanwhile, in order to prevent the components with low boiling point from being excessively damaged, essential oil manufacturers dare to carry out high-temperature extraction for a long time, and the components with high boiling point are easy to cause incomplete extraction, the invention provides a method for carrying out segmented temperature control extraction on the main components of rosemary.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for extracting the main components of rosemary by segmented temperature control, which has the advantages of suitability for large-scale factory production, convenience for rapid market circulation and the like, and solves the problems in the prior art.
(II) technical scheme
In order to realize the purposes of being suitable for large-scale industrial production and being convenient for the rapid circulation of the market, the invention provides the following technical scheme: a method for carrying out segmented temperature control extraction on main components of rosemary comprises the following steps:
1) changing the water in the outer sleeve of the essential oil extraction tank into heat conducting oil, and changing the traditional steam distillation method into an oil bath method;
2) the temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction;
3) the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 5 minutes;
4) extracting alpha-pinene and camphene in the stock solution when the oil temperature of the heat conducting oil is in a first temperature range;
5) the temperature of the conduction oil of the jacket is raised to 171.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a second temperature section, and the temperature section is continued for 5 minutes;
6) when the oil temperature of the heat-conducting oil is in a second temperature section, extracting beta-pinene, myrcene, limonene, 1, 8-cineole and p-cymene in the stock solution;
7) the temperature of the conduction oil of the jacket is raised to 198.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a third temperature section, and the temperature section is continued for 5 minutes;
8) when the oil temperature of the heat-conducting oil is in a third temperature section, extracting linalool in the stock solution;
9) the temperature of the conduction oil of the jacket is increased to 210.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fourth temperature section, and the temperature section is continued for 5 minutes;
10) extracting camphor and borneol from the stock solution when the oil temperature of the heat-conducting oil is in a fourth temperature section;
11) the temperature of the conduction oil of the jacket is increased to 222.5 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fifth temperature section, and the temperature section is continued for 5 minutes;
12) and when the oil temperature of the heat-conducting oil is in a fifth temperature section, extracting the borneol acetate, the alpha-terpineol and the verbenazone in the stock solution.
(III) advantageous effects
Compared with the prior art, the invention provides a method for extracting rosemary main components by segmented temperature control, which has the following beneficial effects:
the method for extracting the main components of rosemary by segmented temperature control divides the whole extraction process into five temperature segments, fully avoids the problem that some components with low boiling points are easily degraded by high temperature in the long-time extraction process in the traditional steam distillation process, or diluted by other high boiling point components, so that the content of the target component in the final product is sufficient, meanwhile, the method adopts a sectional temperature control mode, fully takes care of the purpose that the components with low boiling point are not excessively damaged, also avoids the problem of incomplete extraction of the components with high boiling point, although the single component can not be accurately obtained by the sectional temperature control extraction method, 5 types of main components with different weight measurement are divided according to functionality, can basically meet the type requirements of the current rosemary essential oil market, is suitable for large-scale industrial production, is convenient for the market to rapidly circulate, and has good economic benefit.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: a method for carrying out segmented temperature control extraction on main components of rosemary comprises the following steps:
1) changing the water in the outer sleeve of the essential oil extraction tank into heat conducting oil, and changing the traditional steam distillation method into an oil bath method;
2) the temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction;
3) the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 5 minutes;
4) when the oil temperature of the heat-conducting oil is in a first temperature range, extracting alpha-pinene and camphene in the stock solution, wherein the proportion of the alpha-pinene is 23.10 percent and the proportion of the camphene is 11.0 percent;
5) the temperature of the conduction oil of the jacket is raised to 171.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a second temperature section, and the temperature section is continued for 5 minutes;
6) when the oil temperature of the heat-conducting oil is in a second temperature section, extracting beta-pinene, myrcene, limonene, 1, 8-cineole and p-cymene in the stock solution, wherein the proportion of the beta-pinene is 7.78%, the proportion of the myrcene is 2.11%, the proportion of the limonene is 4.70%, the proportion of the 1, 8-cineole is 38.12%, and the proportion of the p-cymene is 0.99%;
7) the temperature of the conduction oil of the jacket is raised to 198.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a third temperature section, and the temperature section is continued for 5 minutes;
8) when the oil temperature of the heat-conducting oil is in a third temperature section, extracting linalool in the stock solution, wherein the linalool accounts for 1.10%;
9) the temperature of the conduction oil of the jacket is increased to 210.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fourth temperature section, and the temperature section is continued for 5 minutes;
10) when the oil temperature of the heat conducting oil is in a fourth temperature section, extracting the camphor and the borneol in the stock solution, wherein the proportion of the camphor is 11.16 percent, and the proportion of the borneol is 3.33 percent;
11) the temperature of the conduction oil of the jacket is increased to 222.5 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fifth temperature section, and the temperature section is continued for 5 minutes;
12) and when the oil temperature of the heat-conducting oil is in a fifth temperature section, extracting the borneol acetate, the alpha-terpineol and the verbenazone in the stock solution, wherein the proportion of the borneol acetate is 0.47%, the proportion of the alpha-terpineol is 1.31% and the proportion of the verbenazone is 0.85%.
Example two: a method for carrying out segmented temperature control extraction on main components of rosemary comprises the following steps:
1) changing the water in the outer sleeve of the essential oil extraction tank into heat conducting oil, and changing the traditional steam distillation method into an oil bath method;
2) the temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction;
3) the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 8 minutes;
4) when the oil temperature of the heat-conducting oil is in a first temperature range, extracting alpha-pinene and camphene from the stock solution, wherein the alpha-pinene accounts for 38.14% and the camphene accounts for 12.56%, and the alpha-pinene content is higher than 26.0% of the national standard content;
5) the temperature of the conduction oil of the jacket is raised to 171.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a second temperature section, and the temperature section is continued for 8 minutes;
6) when the oil temperature of the heat-conducting oil is in a second temperature range, extracting beta-pinene, myrcene, limonene, 1, 8-cineole and p-cymene in the stock solution, wherein the proportion of beta-pinene is 12.79%, the proportion of myrcene is 4.10%, the proportion of limonene is 7.57%, the proportion of 1, 8-cineole is 55.0%, the proportion of p-cymene is 2.03%, the extracted cost content reaches the content range of the national standard, and part of components reach or exceed the highest content of the national standard;
7) the temperature of the conduction oil of the jacket is raised to 198.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a third temperature section, and the temperature section is continued for 8 minutes;
8) when the oil temperature of the heat-conducting oil is in a third temperature section, extracting the linalool in the stock solution, wherein the percentage of the linalool is 2.46 percent and the maximum content of the linalool is close to the national standard and is 2.5 percent;
9) the temperature of the conduction oil of the jacket is increased to 210.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fourth temperature section, and the temperature section is continued for 8 minutes;
10) when the oil temperature of the heat conducting oil is in a fourth temperature section, extracting the camphor and the borneol in the stock solution, wherein the proportion of the camphor is 16.66 percent and the proportion of the borneol is 5.02 percent, and the content of the extracted components reaches the content range of the national standard, wherein the content of the borneol exceeds the highest content of the national standard;
11) the temperature of the conduction oil of the jacket is increased to 222.5 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fifth temperature section, and the temperature section is continued for 8 minutes;
12) and when the oil temperature of the heat transfer oil is in a fifth temperature section, extracting the bornyl acetate, the alpha-terpineol and the verbenazone in the stock solution, wherein the ratio of the bornyl acetate is 4.89%, the ratio of the alpha-terpineol is 3.01%, the ratio of the verbenazone is 6.04%, the content of the extracted components reaches the content range of national standard, and the content of the bornyl acetate and the content of the verbenazone are higher than the highest content of the national standard.
Example three: a method for carrying out segmented temperature control extraction on main components of rosemary comprises the following steps:
1) changing the water in the outer sleeve of the essential oil extraction tank into heat conducting oil, and changing the traditional steam distillation method into an oil bath method;
2) the temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction;
3) the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 10 minutes;
4) when the oil temperature of the heat-conducting oil is in a first temperature range, extracting alpha-pinene and camphene in the stock solution, wherein the proportion of the alpha-pinene is 63.78%, the proportion of the camphene is 19.10%, the content of the alpha-pinene is higher than 26.0% of the national standard content, and the content of the camphene is higher than 13.0% of the national standard content;
5) the temperature of the conduction oil of the jacket is raised to 171.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a second temperature section, and the temperature section is continued for 10 minutes;
6) when the oil temperature of the heat-conducting oil is in a second temperature section, extracting beta-pinene, myrcene, limonene, 1, 8-cineole and p-cymene in the stock solution, wherein the proportion of beta-pinene is 19.28%, the proportion of myrcene is 5.16%, the proportion of limonene is 11.27%, the proportion of 1, 8-cineole is 63.56%, and the proportion of p-cymene is 2.97%;
7) the temperature of the conduction oil of the jacket is raised to 198.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a third temperature section, and the temperature section is continued for 10 minutes;
8) when the oil temperature of the heat conduction oil is in a third temperature section, extracting the linalool in the stock solution, wherein the linalool accounts for 3.10%, and the extracted linalool has a maximum content higher than the national standard by 2.5%;
9) the temperature of the conduction oil of the jacket is increased to 210.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fourth temperature section, and the temperature section is continued for 10 minutes;
10) when the oil temperature of the heat conducting oil is in a fourth temperature range, extracting the camphor and the borneol in the stock solution, wherein the proportion of the camphor is 22.17 percent and the proportion of the borneol is 6.11 percent, the extracted camphor content is higher than the highest content of 22.0 percent of the national standard, and the borneol content is higher than the highest content of 5.0 percent of the national standard;
11) the temperature of the conduction oil of the jacket is increased to 222.5 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fifth temperature section, and the temperature section is continued for 10 minutes;
12) when the oil temperature of the heat conduction oil is in a fifth temperature section, extracting the bornyl acetate, the alpha-terpineol and the verbenazone in the stock solution, wherein the ratio of the bornyl acetate is 7.39%, the ratio of the alpha-terpineol is 4.30%, the ratio of the verbenazone is 7.17%, the extracted bornyl acetate is higher than the highest content of the national standard by 2.5%, the content of the verbenazone is higher than the highest content of the national standard by 4.0%, and the content of the verbenazone is higher than the highest content of the national standard by 2.5%.
The invention has the beneficial effects that: the method for extracting the main components of rosemary by segmented temperature control divides the whole extraction process into five temperature segments, fully avoids the problem that some components with low boiling points are easily degraded by high temperature in the long-time extraction process in the traditional steam distillation process, or diluted by other high boiling point components, so that the content of the target component in the final product is sufficient, meanwhile, the method adopts a sectional temperature control mode, fully takes care of the purpose that the components with low boiling point are not excessively damaged, also avoids the problem of incomplete extraction of the components with high boiling point, although the single component can not be accurately obtained by the sectional temperature control extraction method, 5 types of main components with different weight measurement are divided according to functionality, can basically meet the type requirements of the current rosemary essential oil market, is suitable for large-scale industrial production, is convenient for the market to rapidly circulate, and has good economic benefit.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A method for carrying out segmented temperature control extraction on main components of rosemary is characterized by comprising the following steps:
1) changing the water in the outer sleeve of the essential oil extraction tank into heat conducting oil, and changing the traditional steam distillation method into an oil bath method;
2) the temperature controller is arranged on the outer surface of the essential oil extraction tank, and the temperature controller is used for realizing time-interval temperature-controlled heating extraction;
3) the temperature of the conduction oil of the jacket is raised to 150.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a first temperature section, and the temperature section is continued for 5 minutes;
4) extracting alpha-pinene and camphene in the stock solution when the oil temperature of the heat conducting oil is in a first temperature range;
5) the temperature of the conduction oil of the jacket is raised to 171.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a second temperature section, and the temperature section is continued for 5 minutes;
6) when the oil temperature of the heat-conducting oil is in a second temperature section, extracting beta-pinene, myrcene, limonene, 1, 8-cineole and p-cymene in the stock solution;
7) the temperature of the conduction oil of the jacket is raised to 198.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a third temperature section, and the temperature section is continued for 5 minutes;
8) when the oil temperature of the heat-conducting oil is in a third temperature section, extracting linalool in the stock solution;
9) the temperature of the conduction oil of the jacket is increased to 210.0 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fourth temperature section, and the temperature section is continued for 5 minutes;
10) extracting camphor and borneol from the stock solution when the oil temperature of the heat-conducting oil is in a fourth temperature section;
11) the temperature of the conduction oil of the jacket is increased to 222.5 ℃ through a temperature controller, the temperature error is +/-5.0 ℃, the temperature is a fifth temperature section, and the temperature section is continued for 5 minutes;
12) and when the oil temperature of the heat-conducting oil is in a fifth temperature section, extracting the borneol acetate, the alpha-terpineol and the verbenazone in the stock solution.
Priority Applications (1)
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3950266A (en) * | 1973-11-28 | 1976-04-13 | Rutgers Research And Educational Foundation | Method of producing an antioxidant composition from rosemary and sage |
CN1654616A (en) * | 2005-01-24 | 2005-08-17 | 中国林业科学研究院林产化学工业研究所 | combined extraction method for rosemary essential oil and rosemary antioxidant |
CN103205314A (en) * | 2013-03-21 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Rosemary extract and application thereof in cigarettes |
CN103232892A (en) * | 2010-01-26 | 2013-08-07 | 田志勇 | Five-section extraction method for preparing mint essential oil by distillation |
CN105994406A (en) * | 2016-06-07 | 2016-10-12 | 西南林业大学 | Sterilizing rosemary incense tablet, and preparation method and application thereof |
CN106701326A (en) * | 2017-03-29 | 2017-05-24 | 董兰田 | Method for extracting mugwort essential oil with different volatility at different temperatures through segmented distillation refining |
US20170251715A1 (en) * | 2016-03-07 | 2017-09-07 | R.J. Reynolds Tobacco Company | Rosemary in a tobacco blend |
-
2021
- 2021-06-17 CN CN202110669778.1A patent/CN113372997A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3950266A (en) * | 1973-11-28 | 1976-04-13 | Rutgers Research And Educational Foundation | Method of producing an antioxidant composition from rosemary and sage |
CN1654616A (en) * | 2005-01-24 | 2005-08-17 | 中国林业科学研究院林产化学工业研究所 | combined extraction method for rosemary essential oil and rosemary antioxidant |
CN103232892A (en) * | 2010-01-26 | 2013-08-07 | 田志勇 | Five-section extraction method for preparing mint essential oil by distillation |
CN103205314A (en) * | 2013-03-21 | 2013-07-17 | 红云红河烟草(集团)有限责任公司 | Rosemary extract and application thereof in cigarettes |
US20170251715A1 (en) * | 2016-03-07 | 2017-09-07 | R.J. Reynolds Tobacco Company | Rosemary in a tobacco blend |
CN105994406A (en) * | 2016-06-07 | 2016-10-12 | 西南林业大学 | Sterilizing rosemary incense tablet, and preparation method and application thereof |
CN106701326A (en) * | 2017-03-29 | 2017-05-24 | 董兰田 | Method for extracting mugwort essential oil with different volatility at different temperatures through segmented distillation refining |
Non-Patent Citations (1)
Title |
---|
郭伊娜;韦藤幼;韦世元;林翠梧;韦万兴;: "迷迭香叶油与花油成分的分析与比较", 生物质化学工程, vol. 41, no. 3, pages 34 - 36 * |
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