AU2020101138A4 - A method for extracting litseacubeba essential oil by rapid flash evaporation - Google Patents
A method for extracting litseacubeba essential oil by rapid flash evaporation Download PDFInfo
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- AU2020101138A4 AU2020101138A4 AU2020101138A AU2020101138A AU2020101138A4 AU 2020101138 A4 AU2020101138 A4 AU 2020101138A4 AU 2020101138 A AU2020101138 A AU 2020101138A AU 2020101138 A AU2020101138 A AU 2020101138A AU 2020101138 A4 AU2020101138 A4 AU 2020101138A4
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- litseacubeba
- essential oil
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- distillation
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 83
- 240000002262 Litsea cubeba Species 0.000 title claims abstract description 71
- 235000012854 Litsea cubeba Nutrition 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000001704 evaporation Methods 0.000 title claims abstract description 16
- 230000008020 evaporation Effects 0.000 title claims abstract description 16
- 238000004821 distillation Methods 0.000 claims abstract description 31
- 239000003921 oil Substances 0.000 claims abstract description 24
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 230000032798 delamination Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 25
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 238000001256 steam distillation Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000000638 solvent extraction Methods 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000001289 litsea cubeba fruit oil Substances 0.000 description 4
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 description 3
- 229940043350 citral Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- VPKMGDRERYMTJX-CMDGGOBGSA-N 1-(2,6,6-Trimethyl-2-cyclohexen-1-yl)-1-penten-3-one Chemical compound CCC(=O)\C=C\C1C(C)=CCCC1(C)C VPKMGDRERYMTJX-CMDGGOBGSA-N 0.000 description 1
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- 235000001577 Lindera glauca Nutrition 0.000 description 1
- 244000245109 Lindera glauca Species 0.000 description 1
- 240000003731 Piper cubeba Species 0.000 description 1
- 235000002711 Piper cubeba Nutrition 0.000 description 1
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010981 turquoise Substances 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 229940045997 vitamin a Drugs 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
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention discloses a method for extracting litseacubeba essential oil by rapid
flash evaporation, the steps of which are as follows: wash litseacubeba fruits, soak fruits in a
saline solution with a mass concentration of 2%~5% for 30~90 min, then put fruits into a
distillation kettle, close the inlet of the distillation kettle, boil and distill with pressurized
steam at 0.1~0.5 MPa for 2~15 min under this pressure, quickly open a valve to a condenser
after distillation, make the essential oil steam enter into an oil separator after condensation,
and finally collect litseacubeba essential oil. This method has shorter process time
(20~40min), lower stream consumption, reduced production energy consumption, enhanced
yield of distilled essential oil and lower production and extraction cost of litseacubeba
essential oil compared with the existing steam distillation method for extracting litseacubeba
essential oil.
Description
Descriptions
A method for extracting litseacubeba essential oil by rapid flash evaporation
Technical Field The present inventionrelates to the extraction field of litseacubeba essential oil, in particular to a method for extracting litseacubeba essential oil by rapid flash evaporation.
Background Technology Litseacubeba, also known as mountain spicy tree fruit, pungent litse fruit, linderaglauca, and piper cubeba (Chinese medicine name), is deciduous leaf dungarunga or shrub of LauraceaeLitsea, mature in July and August by changing color from turquoise to dark red or black. Litseacubebais widely distributed in provinces (regions) of South China, and also distributed in Southeast Asian countries, with excellent properties, such as fast growth, barren tolerance, strong germination ability, easy reproduction and high yield. As one of the main spice economic tree species in China, litseacubebais widely distributed in Jiangxi Province with rich resources, and the essential oil extracted from its fruit and leaves has a wide range of application in foods, medicines, daily chemical products and so on. Litseacubeba essential oil is a natural essential oil with the highest export volume in China, the yield of litseacubeba essential oil is at least 70,000-80,000 tons in China, its import and export volume accounts for more than 80% of the total world trade each year,and China holds the international control of litseacubeba essential oil.
Citral extracted from litseacubeba essential oil is a very popular spice product in the market in short supply but in great demand, and its demand is increasing in the domestic market too. Meanwhile, citral is also an intermediate raw material in pharmaceutical industry for synthesis of -ionone, methyl ionone, vitamin A, citralnitrile and other products.
At present, the main methods for extraction of litseacubeba essential oil include steam distillation extraction, ultrasonic-assisted solvent extraction, microwave-assisted solvent extraction, supercritical carbon dioxide fluid extraction, and organic solvent extraction and so on. Among them, microwave-assisted solvent extraction and ultrasonic-assisted solvent extraction can promote and improve the yield of essential oil to a certain extent, but it is difficult for large-scale industrial production due to the presence of lots of problems such as solvent residue, low purity of essential oil and cumbersome production equipment. The supercritical carbon dioxide fluid extraction method has the advantages of high extraction efficiency and no solvent residue, but the production equipment is cumbersome, the production cost is high, and the feasibility of industrial production is not high. The organic solvent extraction method has the problems of low oil yield, residual solvent and low purity of essential oil, etc. In contrast, steam distillation extraction method has the advantages of simple process, easy access to equipment, low cost, stable yield and high purity of essential oil, etc., which is widely used by domestic and foreign manufacturers at present. However, the steam distillation method for extraction of litseacubeba essential oil used in the factory production has the problems of long extraction time, incomplete oil extraction and high labor intensity, etc. In order to enhance the extraction yield and processing efficiency and improve the quality of essential oil, the present invention provides a method for extracting litseacubeba essential oil by rapid flash evaporation, and realizes the efficient and rapid extraction of litseacubeba essential oil by means of pressurized boiling and rapid pressure release.
A reported method for extracting litseacubeba oil and citralfrom litseacubeba: freshly collected litseacubeba fruits are soaked in warm water for 1 day and then put into a distiller for extraction of essential oil. A reported method for extracting litseacubeba oil: complete and fresh litseacubeba fruits are added into the boiling water, distilled in water with the steam pressure of 0.2~0.3 MPa for 1.0~1.5h, and separated oil and water to obtain litseacubeba oil, which can improve the oil yield to a certain degree. Areported method for simultaneously preparing litseacubeba essential oil and kernel oil: oil is extracted by an improved aqueous extraction process, and fresh litseacubeba fruits are firstly crushed, and then homogenized, modified with acid, fractionated for essential oil, and separated for kernel oil tofinally obtain essential oil and kernel oil, respectively. A reported method for extracting litseacubeba oil and citral: litseacubeba essential oil is obtained by slightly damaging epidermis and adding ultrasonic vibration distillation.
To sum up, in the aspect of extraction and research of essential oil, fruit crushing, ultrasonic technology, simultaneous extraction technology of essential oil and kernel oil, and comprehensive utilization technology, etc., are used to improve and optimize the extraction of essential oil. The present invention also adopts steam distillation method, but the difference is that the essential oil is extracted by pressurized steam boiling and flashevaporation, which greatly shortens the extraction time of essential oil and reduces the extraction cost.
Invention Summary The present invention provides a method for extracting litseacubeba essential oil by rapid flash evaporation, solving the low extraction rate, long extraction time and other problems of essential oil in the process of extracting litseacubeba essential oil by steam distillation. The technical scheme of the present invention is realized as follows:
A method for extracting litseacubeba essential oil by rapid flash evaporation, comprising the following steps:
Step I: select high-quality litseacubeba fruits and wash them;
Step II: immerse litseacubeba fruits in a NaCl solution with a mass concentration of 2%~5% for 30~90 min;
Step III: put the soaked fruits into a distillation kettle, close the inlet of the distillation kettle, boil and distill with pressurized steam at 0.1~0.5 MPa, and maintain for 2~15 min under this pressure;
Step IV: after distillation, quickly open a valve to a condenser, make essential oil steam enterinto an oil-water separator after condensation, separate litseacubeba essential oil after complete delamination of oil and water in the separator, and the whole distillation process lasts 20~40 min.
In the method for extracting litseacubeba essential oil by rapid flash evaporation described in the present invention, the mass concentration of the NaCl solution described in Step II is 2%, and the soaking time of fruits in the NaCl solution is 30 min.
In the method for extracting litseacubeba essential oil by rapid flash evaporation described in the present invention, the steam pressure described in Step III is 0.3MPa, and the duration under this pressure is 12 min.
In the method for extracting litseacubeba essential oil by rapid flash evaporation described in the present invention, the total distillation duration described in Step IV is 30 min.
The implementation of the method for extracting litseacubeba essential oil by rapid flash evaporation described in the present inventioncan provide the following benefits:
1. This method has shorter process time, reduced production energy consumption, enhanced yield of distilled essential oil and lower production and extraction cost of litseacubeba essential oil compared with the existing steam distillation method.
2. The instruments and equipment used in this method are all commonly used ones, the equipment are simple, the operation is simple, and the required conditions are easy to achieve.
3. The raw materials used in this method are extremely available, cheap and rich in source.
Detailed Description of the Presently Preferred Embodiments The technical scheme in embodiments of the present invention will be clearly and completely described.
Embodiment 1 Soak litseacubeba fruits in a NaCl solution with a mass concentration of 2% for 30 min in advance, then put into a distillation kettle, and close the inlet of the distillation kettle. Distill with atmospheric pressure steam, keep the steam outlet valve open to a condenser, make the steam enter into an oil-water separator after condensation, separate oil and water by the separator and obtain litseacubeba essential oil. Separate litseacubeba essential oil after complete delamination of oil and water in the separator, weigh essential oil, and take the average weight after three distillations to obtain the weight of litseacubeba essential oil. The duration of the whole distillation process is 180 min. The yield of litseacubeba essential oil is calculated according to Formula (1):
Yield of litseacubeba essential oil = weight of litseacubeba essential oil/weight of litseacubeba fruits x 100% Formula (1)
The average yield of litseacubeba essential oil obtained by the above process is 6.030%.
Embodiment 2 Soak litseacubeba fruits in a NaCl solution with a mass concentration of 2% for 30 min in advance, then put into a distillation kettle, and close the inlet of the distillation kettle. Input steam, control inlet steam at this time under pressure of 0.20 MPa, distill for 8 min under this pressure, quickly open the steam outlet valve to acondenser after distillation, make the steam enter into an oil-water separator after condensation, separate oil and water by the separator and obtain litseacubeba essential oil. Separate litseacubeba essential oil after complete delamination of oil and water in the separator, weigh essential oil, and take the average weight after three distillationsto obtain the weight of litseacubeba essential oil. The duration of the whole distillation process is 30 min. The yield of litseacubeba essential oil is calculated according to Formula (1). The average yield of litseacubeba essential oil obtained by the above process is 6.239%.
Embodiment 3 Soak litseacubeba fruits in a NaCl solution with a mass concentration of 2% for 30 min in advance, then put into a distillation kettle, and close the inlet of the distillation kettle. Input steam, control inlet steam at this time under pressure of 0.25MPa, distill for 10 min under this pressure, quickly open the steam outlet valve to a condenser after distillation, make the steam enter into an oil-water separator after condensation, separate oil and water by the separator and obtain litseacubeba essential oil. Separate litseacubeba essential oil after complete delamination of oil and water in the separator, weigh essential oil, and take the average weight after three distillationsto obtain the weight of litseacubeba essential oil. The duration of the whole distillation process is 30 min. The yield of litseacubeba essential oil is calculated according to Formula (1). The average yield of litseacubeba essential oil obtained by the above process is 6.331 %.
Embodiment 4 Soak litseacubeba fruits in a NaCl solution with a mass concentration of 2% for 30 min in advance, then put into a distillation kettle, and close the inlet of the distillation kettle. Input steam, control inlet steam at this time under pressure of 0.30MPa, distill for 12 min under this pressure, quickly open the steam outlet valve to a condenser after distillation, make the steam enter into an oil-water separator after condensation, separate oil and water by the separator and obtain litseacubeba essential oil. Separate litseacubeba essential oil after complete delamination of oil and water in the separator, weigh essential oil, and take the average weight after three distillations to obtain the weight of litseacubeba essential oil. The duration of the whole distillation process is 30 min. The yield of litseacubeba essential oil is calculated according to Formula (1). The average yield of litseacubeba essential oil obtained by the above process is 6.338%.
The method for extracting litseacubeba essential oil by rapid flash evaporation described in the present invention allows high-pressure hot steam enter into oil cells and and penetrate into the inner space by means of pressurized boiling. Because the combined action of steam and heat produces the sufficient water distribution of steam and essential oil, when the high pressure steam is released, the hot steam molecules that have penetratedinto oil cells are released from more closed pores in the way of air flow, which drives a high-speed instantaneous flow of surrounding hot steam, resulting in mechanical ruptureof oil cell wall and full releaseofinner essential oil. These advantages overcome the defects of traditional steam distillation extraction, and realize the efficient and rapid extraction of litseacubeba essential oil.
The above embodiments only describe the preferred examples of the present invention and do not limit the scope of the present invention. Any modification, equivalent substitution and improvement, etc. made within the spirit and principle of the present invention shall be included in the protection range of the present invention.
Claims (4)
1. A method for extracting litseacubeba essential oil by rapid flash evaporation is characterized in that the method comprises the following steps: Step I: select high-quality litseacubeba fruits and wash them; Step II: immerse litseacubeba fruits in a NaCl solution with a mass concentration of 2%~5% for 30~90 min; Step III: put the soaked fruits into a distillation kettle, close the inlet of the distillation kettle, boil and distill with pressurized steam at 0.1~0.5 MPa, and maintain for 2~15 min under this pressure; Step IV: after distillation, quickly open a valve to a condenser, make essential oil steam enter into an oil water separator after condensation, separate litseacubeba essential oil after complete delamination of oil and water in the separator, and the whole distillation process lasts 20~40 min.
2. The method for extracting litseacubeba essential oil by rapid flash evaporation according to claim 1 is characterized in that the mass concentration of the NaCl solution described in Step II is 2%, and the soaking time of fruits in the NaCl solution is 30 min.
3. The method for extracting litseacubeba essential oil by rapid flash evaporation according to claim 1 is characterized in that the steam pressure described in Step III is 0.3MPa, and the duration under this pressure is 12 min.
4. The method for extracting litseacubeba essential oil by rapid flash evaporation according to claim 1 is characterized in that the total distillation duration described in Step IV is 30 min.
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| AU2020101138A AU2020101138A4 (en) | 2020-06-25 | 2020-06-25 | A method for extracting litseacubeba essential oil by rapid flash evaporation |
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| AU2020101138A AU2020101138A4 (en) | 2020-06-25 | 2020-06-25 | A method for extracting litseacubeba essential oil by rapid flash evaporation |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112156492A (en) * | 2020-09-29 | 2021-01-01 | 安徽联化新材料有限公司 | Hydroxyethyl methacrylate and processing device thereof |
| CN112205483A (en) * | 2020-09-18 | 2021-01-12 | 安顺鸿祥绿色产业有限责任公司 | Preparation method of litsea pungens composite oil |
| CN112280618A (en) * | 2020-09-23 | 2021-01-29 | 安顺鸿祥绿色产业有限责任公司 | Method for extracting litsea oil |
| CN113075016A (en) * | 2021-04-01 | 2021-07-06 | 上海应用技术大学 | Extraction process and activity determination method for ultrasonically-assisted flash extraction of osmanthus hydrolat |
| CN113913243A (en) * | 2021-09-17 | 2022-01-11 | 海南黎草纪新生物科技有限公司 | Method for extracting citronella hydrolat |
| CN114292701A (en) * | 2021-12-31 | 2022-04-08 | 河南省商业科学研究所有限责任公司 | Extraction method of peony essential oil |
| CN114481662A (en) * | 2021-12-22 | 2022-05-13 | 岳阳林纸股份有限公司 | Camphorwood oil extraction pulping method |
| CN115851377A (en) * | 2022-11-23 | 2023-03-28 | 江西省林业科学院 | Extraction method for improving quality of Pterocarpus marsupium essential oil and application thereof |
| CN115926889A (en) * | 2022-11-23 | 2023-04-07 | 中国热带农业科学院热带作物品种资源研究所 | Essential oil extraction method for reducing content of caprylic acid in noni pomace |
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2020
- 2020-06-25 AU AU2020101138A patent/AU2020101138A4/en not_active Ceased
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| CN112205483A (en) * | 2020-09-18 | 2021-01-12 | 安顺鸿祥绿色产业有限责任公司 | Preparation method of litsea pungens composite oil |
| CN112280618A (en) * | 2020-09-23 | 2021-01-29 | 安顺鸿祥绿色产业有限责任公司 | Method for extracting litsea oil |
| CN112156492A (en) * | 2020-09-29 | 2021-01-01 | 安徽联化新材料有限公司 | Hydroxyethyl methacrylate and processing device thereof |
| CN113075016A (en) * | 2021-04-01 | 2021-07-06 | 上海应用技术大学 | Extraction process and activity determination method for ultrasonically-assisted flash extraction of osmanthus hydrolat |
| CN113913243A (en) * | 2021-09-17 | 2022-01-11 | 海南黎草纪新生物科技有限公司 | Method for extracting citronella hydrolat |
| CN114481662A (en) * | 2021-12-22 | 2022-05-13 | 岳阳林纸股份有限公司 | Camphorwood oil extraction pulping method |
| CN114292701A (en) * | 2021-12-31 | 2022-04-08 | 河南省商业科学研究所有限责任公司 | Extraction method of peony essential oil |
| CN114292701B (en) * | 2021-12-31 | 2023-06-06 | 河南省商业科学研究所有限责任公司 | Extraction method of peony essential oil |
| CN115851377A (en) * | 2022-11-23 | 2023-03-28 | 江西省林业科学院 | Extraction method for improving quality of Pterocarpus marsupium essential oil and application thereof |
| CN115926889A (en) * | 2022-11-23 | 2023-04-07 | 中国热带农业科学院热带作物品种资源研究所 | Essential oil extraction method for reducing content of caprylic acid in noni pomace |
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