CN112679314A - Preparation process of sclareol - Google Patents
Preparation process of sclareol Download PDFInfo
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- CN112679314A CN112679314A CN202011589282.5A CN202011589282A CN112679314A CN 112679314 A CN112679314 A CN 112679314A CN 202011589282 A CN202011589282 A CN 202011589282A CN 112679314 A CN112679314 A CN 112679314A
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- sclareol
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- preparing
- countercurrent
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- XVULBTBTFGYVRC-HHUCQEJWSA-N sclareol Chemical compound CC1(C)CCC[C@]2(C)[C@@H](CC[C@](O)(C)C=C)[C@](C)(O)CC[C@H]21 XVULBTBTFGYVRC-HHUCQEJWSA-N 0.000 title claims abstract description 118
- XVULBTBTFGYVRC-UHFFFAOYSA-N Episclareol Natural products CC1(C)CCCC2(C)C(CCC(O)(C)C=C)C(C)(O)CCC21 XVULBTBTFGYVRC-UHFFFAOYSA-N 0.000 title claims abstract description 59
- LAEIZWJAQRGPDA-UHFFFAOYSA-N Manoyloxid Natural products CC1(C)CCCC2(C)C3CC=C(C)OC3(C)CCC21 LAEIZWJAQRGPDA-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 94
- 239000002904 solvent Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 244000182022 Salvia sclarea Species 0.000 claims description 25
- 235000002911 Salvia sclarea Nutrition 0.000 claims description 24
- 239000003208 petroleum Substances 0.000 claims description 19
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 13
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001691 salvia sclarea Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002137 ultrasound extraction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 229940112950 sage extract Drugs 0.000 description 8
- 238000005086 pumping Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 244000124853 Perilla frutescens Species 0.000 description 2
- 235000004348 Perilla frutescens Nutrition 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 241000207923 Lamiaceae Species 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- IMKJGXCIJJXALX-SHUKQUCYSA-N Norambreinolide Chemical compound CC([C@@H]1CC2)(C)CCC[C@]1(C)[C@@H]1[C@]2(C)OC(=O)C1 IMKJGXCIJJXALX-SHUKQUCYSA-N 0.000 description 1
- 241001072909 Salvia Species 0.000 description 1
- 235000017276 Salvia Nutrition 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IMKJGXCIJJXALX-UHFFFAOYSA-N ent-Norambreinolide Natural products C1CC2C(C)(C)CCCC2(C)C2C1(C)OC(=O)C2 IMKJGXCIJJXALX-UHFFFAOYSA-N 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 235000002020 sage Nutrition 0.000 description 1
- 229940096995 sclareolide Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation process of sclareol, and relates to the technical field of plant extraction. The preparation process of the sclareol comprises the steps of taking sclareol as a raw material and an organic solvent as a solvent, carrying out continuous countercurrent extraction, and recovering the solvent to prepare the sclareol product. The preparation process of sclareol of the invention not only retains the advantages of a plurality of traditional processes, but also creates a plurality of advantages which can not be achieved by the traditional processes: the method has the advantages of high extraction speed, sufficient extraction of effective components, high extraction yield, low solvent consumption, high feed liquid concentration, reduced evaporation concentration and other subsequent treatment processes, short extraction time, extraction of materials in a mild dynamic environment, low heating temperature, less damage of the effective components, low impurity content in the feed liquid, continuous production and high treatment capacity.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to a preparation process of sclareol, and particularly relates to a technical process for preparing sclareol extract from sclareol hay.
Background
Sclareol is a natural raw material for synthesizing high-grade ambergris flavor ambergris ether and tobacco flavoring agent sclareolide. It is a natural perfume obtained by extracting and separating flowers, leaves and stems of natural plant clary sage and purifying. The traditional extraction method of sclareol is intermittent extraction, has long extraction time, large solvent amount, high extraction temperature, high energy consumption, low extraction efficiency and low extraction yield (the extraction yield is calculated by the net content of sclareol in the obtained sclareol extract, the content of sclareol in the sclareol is compared by gas phase detection, and the traditional extraction method has the extraction yield of less than 90 percent and is mostly about 80 percent), so the waste is large.
Disclosure of Invention
The invention aims to provide a novel extraction process technology, so that the extraction of sclareol is more economic, efficient, energy-saving and environment-friendly, thereby improving the economic value of sclareol and bringing better economic benefit to vast farmers.
The invention relates to a preparation process of Sclareol (Sclareol), which takes Sclareol (Salvia SclareL) of a sage plant of Labiatae as a raw material and an organic solvent as a solvent to prepare a Sclareol product through continuous countercurrent extraction, and compared with the traditional preparation method, the preparation process has the advantages of high efficiency, energy saving, high extraction rate and the like, and the specific scheme is as follows:
the preparation process of sclareol includes continuous countercurrent extraction of sclareol material with organic solvent as solvent and recovering solvent to obtain sclareol product.
Preferably, the solvent is an alkane solvent, preferably a polar alkane solvent.
Further, the solvent is at least one of petroleum ether, heptane, hexane, methanol, toluene, ethanol, acetone and water, preferably petroleum ether or methanol. The hexane is preferably cyclohexane or n-hexane; the heptane is preferably n-heptane.
Preferably, the mass ratio of the raw materials to the solvent is 1: 2-4.
Preferably, the extraction temperature of said countercurrent extraction is comprised between 30 ℃ and 100 ℃.
Preferably, the extraction temperature of the countercurrent extraction is 60 ± 10 ℃.
Preferably, the extraction time of the countercurrent extraction is 30 to 120 minutes.
Preferably, the equipment for countercurrent extraction is continuous countercurrent extraction equipment or continuous countercurrent ultrasonic extraction equipment.
Preferably, the raw material is fresh or dried flower, stem, leaf of Perilla frutescens Britt Var Acuta Thunb, or oven-dried residue after extraction of Perilla frutescens Britt Var Acuta L.Var.Var.Var.Var.Var.Var.Var.Var.Va. Further, the raw materials are prepared by airing and drying mature clary sage herb or airing and drying residues of mature fresh clary sage herb after steam distillation, and then crushing the residues so as to improve the solvent permeability during extraction and improve the extraction rate; and then the crushed hay is put into an extraction device for extraction.
According to the preparation process of sclareol, the extracted feed liquid is concentrated and the solvent is recovered, so that the sclareol product has the sclareol content of not less than 45%, the average content of 50-60% and the extraction rate of more than 95%. The highest content of sclareol in the sclareol product obtained by the traditional method is 45 percent, and basically ranges from 40 percent to 45 percent, and the extraction yield is generally less than 90 percent and mostly about 80 percent.
The invention relates to a method for producing sclareol based on a countercurrent extraction principle or by using countercurrent extraction equipment or a device prepared based on the countercurrent extraction principle. The extraction equipment involved can be all countercurrent extraction equipment based on the countercurrent extraction principle, which is characterized in that: the material to be extracted and the solvent can keep relative motion, so that the concentration of the material liquid is diffused and updated continuously, and the leaching speed of the material liquid is high. The method creates a plurality of advantages which cannot be achieved by the traditional process while keeping the advantages of the traditional process: the method has the advantages of high extraction speed, sufficient extraction of effective components, high extraction yield, low solvent consumption, high feed liquid concentration, reduced evaporation concentration and other subsequent treatment processes, short extraction time, extraction of materials in a mild dynamic environment, low heating temperature, less damage of the effective components, low impurity content in the feed liquid, continuous production and high treatment capacity.
Detailed Description
In order to more fully understand the technical contents of the present invention, the technical solutions of the present invention will be further described and illustrated with reference to specific embodiments.
Example 1
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent extractor at a constant speed, adding 6500Kg of petroleum ether into the continuous countercurrent extractor at the other end of a solvent feed inlet, controlling the extraction temperature of the extractor to be 60 ℃, controlling the extraction time to be 90 minutes according to the amount of materials and solvents, pumping feed liquid into a solvent recovery tank to recover the solvents, decompressing a concentration kettle to remove residual petroleum ether, and obtaining 66.4Kg of clary sage extract, wherein the content of sclareol is 52.3%, and the extraction yield is 91.4%.
Comparative example 1
Adding 2000Kg of crushed clary sage hay into an extraction tank, adding 6500Kg of petroleum ether, heating to 60 ℃ for extraction for 90 minutes, transferring the feed liquid into a concentration kettle, and recovering the petroleum ether; and (3) decompressing the concentration kettle to remove residual petroleum ether to obtain 55.7Kg of clary sage extract, wherein the content of sclareol is 49.6 percent, and the extraction yield is 72.7 percent.
Example 2
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent ultrasonic extractor at a constant speed, adding 6500Kg of petroleum ether into the continuous countercurrent ultrasonic extractor at a constant speed in a solvent feed inlet at the other end, controlling the extraction temperature of the extractor to be 50 ℃, controlling the extraction time to be 60 minutes according to the amount of materials and solvents, controlling the ultrasonic power to be 60KW, pumping the feed liquid into a solvent recovery tank to recover the solvents, decompressing a concentration kettle to remove residual petroleum ether, and obtaining 74.6Kg of clary sage extract, wherein the content of sclareol is 51.9%, and the extraction yield is 101.5%.
Comparative example 2
Adding 2000Kg of crushed clary sage hay into an extraction tank, adding 6500Kg of petroleum ether, heating to 50 ℃ for extraction for 60 minutes, transferring the feed liquid into a concentration kettle, and recovering the petroleum ether; decompressing the concentration kettle to remove the residual petroleum ether, and obtaining 52.3Kg of sclareol extract, wherein the content of sclareol is 48.5 percent, and the extraction yield is 66.3 percent.
Example 3
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent ultrasonic extractor at a constant speed, adding 6500Kg of methanol into the continuous countercurrent ultrasonic extractor at the other end of a solvent feed inlet, controlling the extraction temperature of the extractor at 50 ℃, controlling the extraction time at 60 minutes according to the amount of materials and solvents, controlling the ultrasonic power at 60KW, pumping the feed liquid into a solvent recovery tank to recover the solvents, decompressing a concentration kettle to remove residual methanol to obtain 78.9Kg of clary sage extract, wherein the content of clary sage alcohol is 50.3%, and the extraction yield is 104.2%.
Comparative example 3
Adding 2000Kg of crushed clary sage hay into an extraction tank, adding 6500Kg of methanol, heating to 50 ℃ for extraction for 60 minutes, transferring the feed liquid into a concentration kettle, and recovering petroleum ether; decompressing the concentration kettle to remove the residual petroleum ether, and obtaining 63.6Kg of sclareol extract, wherein the content of sclareol is 46.1 percent, and the extraction yield is 77.1 percent.
Example 4
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent ultrasonic extractor at a constant speed, adding 6500Kg of n-hexane into the continuous countercurrent ultrasonic extractor at a constant speed in a solvent feed inlet at the other end, controlling the extraction temperature of the extractor to be 50 ℃, controlling the extraction time to be 60 minutes according to the amount of materials and solvents, controlling the ultrasonic power to be 60KW, pumping the feed liquid into a solvent recovery tank to recover the solvents, decompressing a concentration kettle to remove residual methanol, and obtaining 76.2Kg of clary sage extract, wherein the content of clary sage alcohol is 51.3%, and the extraction yield is 102.8%.
Example 5
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent ultrasonic extractor at a constant speed, adding 6500Kg of n-heptane into the continuous countercurrent ultrasonic extractor at a constant speed in a solvent feed inlet at the other end, controlling the extraction temperature of the extractor to be 50 ℃, controlling the extraction time to be 60 minutes according to the amount of materials and solvents, controlling the ultrasonic power to be 60KW, pumping the feed liquid into a solvent recovery tank to recover the solvents, decompressing a concentration kettle to remove residual methanol, and obtaining 75.4Kg of clary sage extract, wherein the content of clary sage alcohol is 51.6%, and the extraction yield is 102.3%.
Example 6
Uniformly adding 2000Kg of crushed clary sage hay into a feed inlet of a continuous countercurrent ultrasonic extractor at a constant speed, adding 6500Kg of toluene into the continuous countercurrent ultrasonic extractor at the other end of a solvent feed inlet, controlling the extraction temperature of the extractor at 50 ℃, controlling the extraction time at 60 minutes according to the amount of materials and solvents, controlling the ultrasonic power at 60KW, pumping the feed liquid into a solvent recovery tank to recover the solvents, and decompressing a concentration kettle to remove residual methanol to obtain 78.4Kg of clary sage extract, wherein the content of clary sage alcohol is 50.1%, and the extraction yield is 103.3%.
Comparative example tank extraction
Adding 500Kg of crushed clary sage hay into an extraction tank, adding 1000Kg of petroleum ether, heating to 65 ℃ for extraction for 120 minutes, transferring the feed liquid into a concentration kettle, and recovering the petroleum ether; adding 1000Kg of petroleum ether, heating to 65 deg.C, extracting for 90 min, and removing residual petroleum ether under reduced pressure to obtain 16.7Kg of clary sage extract with sclareol content of 45.6% and extraction yield of 80.2%.
In the technology, the determination method of the sclareol content in the sclareol extract is a meteorological internal standard method, and the specific conditions are as follows: the instrument is an Agilent gas detector and a capillary gas chromatographic column, the model is DB-624, and the internal standard substance is dibutyl phthalate. The temperature of the column oven is 250 ℃, the temperature of the injection port is 270 ℃, and the temperature of the detector is 280 ℃.
The calculation method of the extraction yield comprises the following steps: the sclareol content of the sclareol hay was generally about 1.8% to 2.0% (specifically, the average content was 1.9% in the test, which is calculated from the difference in the production area and the water content of the sclareol hay, and thus, some results were found to be greater than 100%). The calculation method of the extracted sclareol comprises the following steps: the weight of the extract obtained by extraction is multiplied by the content of the extract. The calculation method of the extraction yield comprises the following steps: the extracted sclareol was divided by the weight of the hay and divided by the average content of 1.9.
The technical contents of the present invention are further illustrated by the examples, so as to facilitate the understanding of the reader, but the embodiments of the present invention are not limited thereto, and any technical extension or re-creation based on the present invention is protected by the present invention.
Claims (10)
1. A process for preparing sclareol features that the sclareol is prepared from sclareol as raw material and organic solvent through continuous countercurrent extraction, recovering solvent and preparing sclareol product.
2. The process for preparing sclareol according to claim 1, wherein the solvent is an alkane solvent.
3. The process of claim 1, wherein the solvent is at least one of petroleum ether, heptane, hexane, methanol, toluene, ethanol, acetone, and water.
4. The process for preparing sclareol according to claim 1, wherein the mass ratio of the raw material to the solvent is 1: 2-4.
5. The process for preparing sclareol according to claim 1, wherein the extraction temperature of the countercurrent extraction is between 30 ℃ and 100 ℃.
6. The process for preparing sclareol according to claim 5, wherein the extraction temperature of the countercurrent extraction is 60 ± 10 ℃.
7. The process for producing sclareol as claimed in claim 5, wherein the extraction time of the countercurrent extraction is 30 to 120 minutes.
8. The process for preparing sclareol according to claim 1, wherein the countercurrent extraction apparatus is a countercurrent extractor, a pot-type countercurrent extraction apparatus, a continuous countercurrent extraction apparatus, a pot-type continuous countercurrent extraction apparatus, or a continuous countercurrent ultrasonic extraction apparatus.
9. The process of claim 1, wherein the raw material is fresh or dried flowers, stems, leaves of Salvia sclarea, or oven-dried residue after extraction of Salvia sclarea oil.
10. The process for preparing sclareol according to claim 1, wherein the content of sclareol in the sclareol product is not less than 30%.
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| CN202011589282.5A CN112679314A (en) | 2020-12-29 | 2020-12-29 | Preparation process of sclareol |
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| CN202011589282.5A CN112679314A (en) | 2020-12-29 | 2020-12-29 | Preparation process of sclareol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196476A (en) * | 2021-09-08 | 2022-03-18 | 广州东智盟化妆品有限公司 | Extraction method of whitening and freckle-removing perilla frutescens essential oil and extract |
| CN114573421A (en) * | 2022-03-17 | 2022-06-03 | 北京理工大学 | Method for extracting and purifying sclareol from sclareol fermentation liquor |
| CN115636729A (en) * | 2022-10-31 | 2023-01-24 | 焦作市馨之源科技有限公司 | Method and device for purifying sclareol |
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Application publication date: 20210420 |
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