CN103007570B - A kind of method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil - Google Patents
A kind of method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil Download PDFInfo
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- CN103007570B CN103007570B CN201210524330.1A CN201210524330A CN103007570B CN 103007570 B CN103007570 B CN 103007570B CN 201210524330 A CN201210524330 A CN 201210524330A CN 103007570 B CN103007570 B CN 103007570B
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Abstract
A method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil, drying and crushing that it comprises the steps: (1): by cloudy for Chinese medicine to half-dried, be crushed to 30 ~ 40 orders, be placed in extraction kettle; (2) dewater: control extraction kettle pressure 8 ~ 28MPa, temperature 35 ~ 75 DEG C, separating still pressure 4 ~ 12Mpa, temperature 20 ~ 60 DEG C, dehydration 0.5 ~ 1h; (3) extract and separate: control extraction kettle temperature 36 ~ 39 DEG C, pressure 26 ~ 28MPa, separating still I pressure 9 ~ 11MPa, temperature 46 ~ 54 DEG C, extraction 1.5 ~ 3h; (4) pre-freeze is refined: by first essential oil in the centrifugal 5 ~ 20min of 0 ~ 8 DEG C of pre-freeze 4 ~ 8h, 6000 ~ 14000r/min or through 70 ~ 110 μm of filtering with microporous membrane.Energy consumption of the present invention is low, and essential oil loss is few, and extraction efficiency is high, environmentally safe; Product quality is high, and purity is high, no solvent residue.<!--1-->
Description
Technical field
Invention relates to a kind of method prepared by integrated Chinese medicine material dehydration, extraction of essential oil and essential oil, especially relates to a kind of employing supercritical CO
2abstraction technique dewaters to Chinese medicine material, extract, prepare the method for essential oil of traditional Chinese medicine.
Background technology
Essential oil of traditional Chinese medicine refers to that a class is obtained through refining from the position such as flower, leaf, root, skin, stem, branch, fruit, seed of fragrant Chinese medicine, has the oily mater of characteristic perfume.Ingredient more complicated, mainly contains terpene hydrocarbons, arene, alcohols, aldehydes, ketone, ethers, ester class and phenols etc.Essential oil of traditional Chinese medicine as a kind of important functional component in cough-relieving, relieving asthma, eliminate the phlegm, antibacterial, anti-inflammatory, wind dispelling, stomach invigorating, antipyretic, analgesia, spasmolysis, desinsection, sterilization, anticancer, diuresis, step-down, cardiac stimulant, antiallergic activity, enzyme inhibition activity, antimutagenic activity, anti-oxidant etc. in there is stronger biologically active.The main functional component of the diaphoretic medicine that we commonly use, promoting flow of qi and blood circulation medicine, aromatic damp-resolving drug is all essential oil.
At present, the extracting method of essential oil of traditional Chinese medicine is generally steam distillation and organic solvent extraction, and minority adopts supercritical CO
2abstraction technique extracts.It is long to there is extraction time in steam distillation and organic solvent extraction, energy consumption is high, yield is low, the problems such as contaminated environment, and have employed poisonous organic solvent in leaching process, Extracting temperature is higher, composition suffers Oxidative demage, thus causes the product quality that obtains poor, purity is lower, also there is the problems such as harmful organic solvent residual.
Supercritical CO
2abstraction technique because extraction temperature is low, efficiency is high, product without advantages such as chemical residuals, be widely used in natural product extraction.But supercritical CO
2fluid extraction requires higher (< 8%) to feed moisture content, and essential oil is a kind of highly volatile and the material all very responsive to light, oxygen, heat, therefore adopting traditional dewatering to exist, loss is large, active destroys the problems such as serious.Even if dried raw material adopts supercritical CO
2extract the product obtained and be also often even entirely paste containing a large amount of pastes, need the requirement that could meet essential oil market through complicated preparation process.And freeze drying is for the moment difficult to reach industrial requirement due to the reason such as technology, cost, therefore raw material dehydration and the component damages that brings is large etc. that problem limits supercritical CO always
2the application of abstraction technique in extraction of essential oil.
Summary of the invention
The invention provides and a kind ofly integrate raw material dehydration, essential oil extraction, the essential oil method of refining.The method adopts supercritical CO
2technology is dewatered to Chinese medicine material, avoids light, oxygen, the destruction of heat to composition, has simple and convenient, loses low, active component and retains complete advantage.Leaching process by state modulator, directly by supercritical CO
2drying enters supercritical CO
2extract, simple to operate, efficiency is high, and energy consumption is low.Subtractive process adopts the centrifugal or filter method of physics, fast and simple, with low cost.
This invention products obtained therefrom has the advantages such as quality is good, composition reservation is complete, no solvent residue, environmentally safe.
The object of the invention is to be achieved through the following technical solutions.
A kind of method that it comprises the steps: 1, integrated Chinese medicine material is dry, prepared by extraction of essential oil and essential oil, it is dry that it comprises the steps: (1): will be placed in shady and cool dry place and dry half-dried; (2) pulverize: by the Chinese medicine after drying, be crushed to 30 order ~ 40 orders; (3) dewater: the Chinese medicine after pulverizing is loaded extraction kettle, with high-pressure pump by cooled liquid CO
2squeeze into extraction kettle, controlling extraction kettle pressure is 8MPa ~ 28MPa, and extraction kettle temperature is 35 DEG C ~ 75 DEG C, separating still pressure 4Mpa ~ 12Mpa, and separating still temperature is 20 DEG C ~ 30 DEG C, dehydration 0.5h ~ 1h, and the rear moisture that dewatered is released from separating still; (4) extract: extraction kettle temperature controlled to be 36 DEG C ~ 39 DEG C, extraction kettle pressure is 26MPa ~ 28MPa, dynamic extraction 1.5h ~ 3h; (5) be separated: the CO being dissolved with essential oil
2fluid enters in separating still and is separated from extraction kettle, and the Stress control of separating still I is 9MPa ~ 11MPa, and temperature is 46 DEG C ~ 54 DEG C, and the Stress control of separating still II is 4Mpa ~ 5Mpa, and temperature is 40 DEG C ~ 50 DEG C; (6) pre-freeze: be separated the essential oil and 0 DEG C ~ 8 DEG C pre-freeze 4h ~ 8h that obtain; (7) refining: the first essential oil after pre-freeze, obtain refining essential oil through centrifugal or filtration, centrifugal rotational speed is 6000r/min ~ 14000r/min, centrifugation time 5min ~ 20min, and pore size filter is 70 μm ~ 110 μm.
The essential oil of traditional Chinese medicine extracted through method of the present invention measures through GC-MS, and the derived essential oil kind number obtained is than existing supercritical CO
2extracting process has more more than 1 times, illustrates that the essential oil of traditional Chinese medicine composition utilizing the present invention to extract obtains complete reservation.
In a word, advantage of the present invention is: can integrate raw material dehydration, essential oil extracts, essential oil is refined.Raw material dehydration technique is simple and convenient, and product loss is low; Extraction process flow process is simple, and extraction time is short, and extraction efficiency is high, environmentally safe, effectively can protect the functional component in essential oil.Process for purification is fast and simple, and cost is low, and products obtained therefrom quality is pure, free from extraneous odour, no solvent residue, and functional component retains complete, can meet market demands completely, have very high medical value.
The present invention, to making full use of natural resources of Chinese medicinal materials, promotes that the modernization of Chinese medicine is significant.
Detailed description of the invention
Use the present invention to obtain through refining essential oil of traditional Chinese medicine more existing research in recovery rate, composition reservation to improve a lot.
embodiment 1
The rhizoma atractylodis dried in the shade by 1Kg, put into the barrel of extraction kettle after being crushed to 30 orders, ice chest refrigeration opened, the temperature of extraction kettle is set to 65 DEG C, and the temperature of separating still I is set to 25 DEG C, opens CO
2steel cylinder, CO
2from steel cylinder out, enter in ice chest through gas purifier I and liquefy, then start high-pressure pump, by CO
2through clarifier II, extraction kettle squeezed into by preheater I, and boost to 16MPa and dewater, moisture is with CO
2enter piece-rate system again after entering preheater II preheating, the pressure regulating separating still I is release moisture from separating still I after 4MPa, 1h.Regulate extraction kettle temperature to be 37 DEG C, pressure is 26Mpa, makes CO
2become fluid and carry out essential oil extraction, the CO containing essential oil
2fluid enters piece-rate system again after preheater II preheating, and controlling separating still I temperature is 46 DEG C, and pressure is 9Mpa, separating still II temperature 40 DEG C, and pressure is 4Mpa, essential oil and CO
2realize being separated and release bottom separating still I and separating still II, CO
2by flowmeter, enter ice chest liquefaction through clarifier I, recycle.After 1.5h, the product collected must be refined essential oil 62.8g through the centrifugal 5min of 10000r/min after pre-freeze 4h at 4 DEG C, extraction yield is 6.28%.
Through detecting sample according to GC-MS essential oil assay method, detecting 135 kinds of compositions altogether, mainly containing: γ-elemene 3.16%, 4 (14), 11-folium eucalypti diene 4.49%; Sagittol 7.21%; Curcuma zedoary furans alkene 3.76%; To phenyl benzaldehyde 13.38%; 4,4'-dimethyl-2,2'-di-2-ethylhexylphosphine oxide pentamethylene-3,3'-diene 3.28%; 5-methyl isophthalic acid-phenyl-monovinylacetylene-5-alcohol 15.44%; Diisooctyl phthalate 15.58%; 4,4'-dimethyl-2,2'-di-2-ethylhexylphosphine oxide pentamethylene-3,3'-diene 2.11%; 1-acenaphthene alcohol 2.05%.
By contrast, Zhao Ying, Song Dan, Jiang Huaizhong, the method recovery rate waited is: 4.2%, and (GC-MS GC-MS analyzes rhizoma atractylodis supercritical CO only to detect 79 kinds of compositions
2extract composition [J]. Chinese patent drug, 2008,12(30): 1819-1821).Yang Ling, Ou Yangzhen, Su Shulan, the recovery rate waited is: 13.80%, only detect 67 kinds of compositions (Atractylis lancea volatile oil supercritical extraction process and Gc-ms [J]. Jiangsu University's journal (medicine), 2007,5(17): 393-7395).
embodiment 2
The Ligusticum wallichii dried in the shade by 1Kg, is crushed to 40 orders, and controlling dehydration separating still temperature is 70 DEG C, and pressure is 18Mpa, and separating still I temperature is 30 DEG C, and pressure is 6Mpa, and dewatering time is 1h.The pressure controlling extraction kettle is 28MPa, temperature is set to 39 DEG C, the pressure of separating still I is adjusted to 11MPa, temperature is set to 52 DEG C, being separated II pressure is 5Mpa, and temperature is 45 DEG C, extracts 2 hours, collect after essential oil filters through 30 μm after 2 DEG C of pre-freeze 4h and must refine essential oil 87.8g, extraction yield is 8.78%.
Through detecting sample according to GC-MS essential oil assay method, detecting 142 kinds of compositions altogether, mainly containing: 1-(2,4-3,5-dimethylphenyl)-1-acetone 3.64%; Positive fourth subunit phthalic amide 3.12%; Umbrella willow ketone 6.42%; 1-phenyl-1-hexanol 11.93%; (2E)-1-phenyl-2-butene-1-ol 30.76%; Linoleic acid 2.71%; Phthalic acid list ethylhexyl 11.66%.
By contrast, Zeng Zhi, Xie Runqian, Tan Lixian, the recovery rate waited is: 7.60%, only detects 34 kinds of compositions (steam distillation and supercritical COs
2the GC-MS analysis and identification [J] of extract chemical composition. applied chemistry, 2011,8(28): 956-962).
Claims (6)
1. for extracting a Chinese herb dewatering for essential oil of traditional Chinese medicine, it is characterized in that, carrying out supercritical CO
2dehydration: load extraction kettle after being pulverized by half-dried Chinese medicine, controlling extraction kettle pressure is 8MPa ~ 28MPa, and extraction kettle temperature is 35 DEG C ~ 75 DEG C, separating still pressure 4MPa ~ 12MPa, and separating still temperature is 20 DEG C ~ 60 DEG C.
2. the Chinese herb dewatering of claim 1, wherein extraction kettle pressure is 16 ~ 28MPa, and/or extraction kettle temperature is 65 ~ 75 DEG C.
3. extract a method for essential oil of traditional Chinese medicine, it is characterized in that, comprise the steps: (1) supercritical CO
2dehydration; (2) supercritical CO
2extraction, supercritical CO wherein
2dehydration as claimed in claim 1 or 2.
4. a kind of method extracting essential oil of traditional Chinese medicine of claim 3, is characterized in that, described supercritical CO
2extraction is: extraction kettle temperature controlled to be 36 DEG C ~ 39 DEG C, extraction kettle pressure is 26MPa ~ 28MPa, dynamic extraction 1.5h ~ 3h.
5. the method for claim 3 or 4, also comprise the steps: (3) centrifugal or filter.
6. the method for claim 5, is characterized in that, described centrifugal centrifugal rotational speed is 6000r/min ~ 14000r/min, and the pore size filter of described filtration is 70 μm ~ 110 μm.
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| CN103710152B (en) * | 2013-10-28 | 2016-04-27 | 黄山神草生物科技有限公司 | A kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil |
| CN110055130A (en) * | 2019-03-06 | 2019-07-26 | 中国热带农业科学院农产品加工研究所 | A kind of preparation method and application of natural plants hydrosol |
| CN112760169A (en) * | 2020-12-02 | 2021-05-07 | 桂林理工大学 | Acer truncatum seed essential oil, and preparation method and application thereof |
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| EP0065106A2 (en) * | 1981-05-15 | 1982-11-24 | SKW Trostberg Aktiengesellschaft | Process for producing concentrated extracts from fresh plants or parts thereof, especially from fresh spices |
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| CN101508937A (en) * | 2009-03-12 | 2009-08-19 | 中山大学 | Supercritical method for extracting nutmeg essential oil with carbonic anhydride |
| CN101624557A (en) * | 2009-07-31 | 2010-01-13 | 重庆市日用化学工业研究所 | Method for extracting neroli absolute by supercritical carbon dioxide |
| CN101831302A (en) * | 2010-05-06 | 2010-09-15 | 广州和博生物科技有限公司 | Liquid oil-instant and stable rosemary antioxidant and preparation method thereof |
| CN102344854A (en) * | 2011-09-08 | 2012-02-08 | 南京泽朗医药科技有限公司 | Method for extracting volatile oil from cynoglossum lanceolatum |
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2012
- 2012-12-10 CN CN201210524330.1A patent/CN103007570B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0065106A2 (en) * | 1981-05-15 | 1982-11-24 | SKW Trostberg Aktiengesellschaft | Process for producing concentrated extracts from fresh plants or parts thereof, especially from fresh spices |
| US5017397A (en) * | 1990-04-25 | 1991-05-21 | Uy Nguyen | Process for extracting antioxidants from Labiatae herbs |
| CN101019908A (en) * | 2007-03-20 | 2007-08-22 | 中国科学院山西煤炭化学研究所 | Supercritical extraction process of water extracted and alcohol deposited safflower residue |
| CN101508937A (en) * | 2009-03-12 | 2009-08-19 | 中山大学 | Supercritical method for extracting nutmeg essential oil with carbonic anhydride |
| CN101624557A (en) * | 2009-07-31 | 2010-01-13 | 重庆市日用化学工业研究所 | Method for extracting neroli absolute by supercritical carbon dioxide |
| CN101831302A (en) * | 2010-05-06 | 2010-09-15 | 广州和博生物科技有限公司 | Liquid oil-instant and stable rosemary antioxidant and preparation method thereof |
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