CN103007570A - Integrated method for dehydrating traditional Chinese medicine materials, extracting essential oil and preparing essential oil - Google Patents
Integrated method for dehydrating traditional Chinese medicine materials, extracting essential oil and preparing essential oil Download PDFInfo
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- CN103007570A CN103007570A CN2012105243301A CN201210524330A CN103007570A CN 103007570 A CN103007570 A CN 103007570A CN 2012105243301 A CN2012105243301 A CN 2012105243301A CN 201210524330 A CN201210524330 A CN 201210524330A CN 103007570 A CN103007570 A CN 103007570A
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Abstract
The invention discloses an integrated method for dehydrating traditional Chinese medicine materials, extracting essential oil and preparing the essential oil. The integrated method comprises the following steps: (1) drying and grinding, namely half drying the traditional Chinese medicine materials in a dark place, grinding the materials to have 30-40 meshes, and placing into an extraction kettle; (2) dehydrating, namely controlling the pressure of the extraction kettle to be 8-28 MPa, the temperature of the extraction kettle to be 35-75 DEG C, the pressure of a separation kettle to be 4-12 MPa and the temperature of the separation kettle to be 20-60 DEG C, and dehydrating for 0.5-1 h; (3) extracting and separating, namely controlling the temperature of the extraction kettle to be 36-39 DEG C, the pressure of the extraction kettle to be 26-28 MPa, the pressure of a separation kettle I to be 9-11 MPa and the temperature of the separation kettle I to be 46-54 DEG C, and extracting for 1.5-3 h; and (4) pre-freezing and refining, namely pre-freezing the initial essential oil for 4-8 h at the temperature of 0-8 DEG C, and centrifuging for 5-20 min at the speed of 6000-14000 r/min or filtering by a microfiltration membrane of 70-110 mum. The integrated method has the characteristics of low energy consumption, low loss of the essential oil, high extraction efficiency, no environmental pollution, high product quality, high purity and no solvent residue.
Description
Technical field
Invention relates to the method for a kind of integrated Chinese medicine material dehydration, extraction of essential oil and essential oil preparation, especially relates to a kind of employing supercritical CO
2Abstraction technique dewaters, extracts, prepares the method for essential oil of traditional Chinese medicine to Chinese medicine material.
Background technology
Essential oil of traditional Chinese medicine refers to that a class obtains through refining from positions such as the flower of fragrant Chinese medicine, leaf, root, skin, stem, branch, fruit, seeds, has the oily mater of characteristic perfume.The 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, antibiotic, anti-inflammatory, wind dispelling, stomach invigorating, analgesic, analgesia, spasmolysis, desinsection, sterilization, anticancer, diuresis, step-down, cardiac stimulant, antiallergic activity, enzyme inhibition activity, antimutagenic activity, the aspect such as anti-oxidant have stronger biologically active.The major function composition of the diaphoretic medicine that we commonly use, promoting flow of qi and blood circulation medicine, aromatic damp-resolving drug all is 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.Steam distillation and organic solvent extraction exist extraction time long, energy consumption is high, yield is low, the problems such as contaminated environment, and adopted poisonous organic solvent in the leaching process, to extract temperature higher, composition suffers Oxidative demage, thereby causes the product quality that obtains relatively poor, purity is lower, also has the harmful problems such as organic solvent residual.
Supercritical CO
2Abstraction technique is widely used aspect natural product extraction because extraction temperature is low, efficient is high, product is without advantages such as chemical residuals.But supercritical CO
2Fluid extraction is had relatively high expectations (＜8%) to the raw material water content, and essential oil is a kind of highly volatile and to light, oxygen, heat very responsive material all, therefore adopts traditional dewatering to have that loss is large, active to destroy the problems such as serious.Even dried raw material adopts supercritical CO
2The product that extraction obtains also often contains a large amount of pastes even is entirely paste, needs could satisfy the requirement in essential oil market through complicated preparation process.And freeze drying is difficult to reach industrial requirement for the moment owing to reasons such as technology, costs, so raw material dehydration and the composition loss that brings be large etc., and problem is limiting supercritical CO always
2The application of abstraction technique aspect extraction of essential oil.
Summary of the invention
The invention provides a kind of method that raw material dewaters, essential oil extracts, essential oil is made with extra care that integrates.The method adopts supercritical CO
2Technology is dewatered to Chinese medicine material, has avoided light, oxygen, heat to the destruction of composition, has simple and conveniently, lose advantage low, that the active component reservation is complete.Leaching process can be controlled by parameter, directly by supercritical CO
2Drying enters supercritical CO
2Extract, simple to operate, efficient is high, and energy consumption is low.Subtractive process adopts the centrifugal or filter method of physics, and is fast and simple, with low cost.
This invention products obtained therefrom has the advantages such as quality is good, the composition reservation is complete, no solvent residue, environmentally safe.
The objective of the invention is to be achieved through the following technical solutions.
It comprises the steps: 1, a kind of integrated Chinese medicine material is dry, the method for extraction of essential oil and essential oil preparation, and it comprises the steps: (1) drying: will place shady and cool dry place to dry half-dried; (2) pulverize: the Chinese medicine after will drying is crushed to 30 orders ~ 40 orders; (3) dehydration: the extraction kettle of packing into of the Chinese medicine after will pulverizing, with high-pressure pump with cooled liquid CO
2Squeeze into extraction kettle, control extraction kettle pressure is 8 MPa ~ 28 MPa, and the extraction kettle temperature is 35 ℃ ~ 75 ℃, separating still pressure 4 Mpa ~ 12 Mpa, and the separating still temperature is 20 ℃ ~ 30 ℃, 0.5 h that dewaters ~ 1 h, moisture was emitted from separating still after dehydration was finished; (4) extraction: the extraction kettle temperature is controlled to be 36 ℃ ~ 39 ℃, and extraction kettle pressure is 26 MPa ~ 28 MPa, dynamic extraction 1.5 h ~ 3 h; (5) separate: the CO that is dissolved with essential oil
2Fluid enters in the separating still from extraction kettle and separates, and the pressure of separating still I is controlled to be 9 MPa ~ 11 MPa, and temperature is 46 ℃ ~ 54 ℃, and the pressure of separating still II is controlled to be 4 Mpa ~ 5 Mpa, and temperature is 40 ℃ ~ 50 ℃; (6) pre-freeze: separate essential oil and 0 ℃ ~ 8 ℃ pre-freeze 4 h ~ 8 h of obtaining; (7) refining: the first essential oil after the pre-freeze, obtain refining essential oil through centrifugal or filtration, centrifugal rotational speed is 6000 r/min ~ 14000 r/min, centrifugation time 5min ~ 20min, pore size filter are 70 μ m ~ 110 μ m.
Measure through GC-MS through the essential oil of traditional Chinese medicine that method of the present invention is extracted, the derived essential oil kind number that obtains is than existing supercritical CO
2Extracting process has more more than 1 times, illustrates that the essential oil of traditional Chinese medicine composition that utilizes the present invention to extract has obtained complete reservation.
In a word, advantage of the present invention is: can integrate raw material dehydration, essential oil extraction, essential oil and make with extra care.The raw material dewatering process is simple and convenient, and product loss is low; The extraction process flow process is simple, and extraction time is short, and extraction efficiency is high, and environmentally safe can be protected the functional component in the essential oil effectively.Process for purification is fast and simple, and cost is low, and the products obtained therefrom quality is pure, free from extraneous odour, and no solvent residue, functional component keeps complete, and fully satisfying the market requirement has very high medical value.
The present invention promotes the modernized significant of Chinese medicine to taking full advantage of natural resources of Chinese medicinal materials.
The specific embodiment
Using the present invention to obtain through refining essential oil of traditional Chinese medicine improves a lot in existing research aspect recovery rate, the composition reservation.
Embodiment 1
With the rhizoma atractylodis that 1 Kg dries in the shade, be crushed to the barrel of putting into extraction kettle behind 30 orders, the ice chest refrigeration is opened, the temperature setting of extraction kettle is set to 65 ℃, the temperature setting of separating still I is set to 25 ℃, opens CO
2Steel cylinder, CO
2From steel cylinder out, enter in the ice chest through the gas purifier I and to liquefy, then start high-pressure pump, with CO
2Through the clarifier II, the preheater I is squeezed into extraction kettle, boosts to 16 MPa and dewaters, and moisture is with CO
2Enter piece-rate system after entering the preheating of preheater II, the pressure of regulating the separating still I is 4 MPa, emits moisture from the separating still I behind 1 h again.Regulating the extraction kettle temperature is 37 ℃, and pressure is 26 Mpa, makes CO
2Become fluid and carry out the essential oil extraction, contain the CO of essential oil
2Enter piece-rate system after the preheating of fluid process preheater II, control separating still I temperature is 46 ℃ again, and pressure is 9 Mpa, 40 ℃ of separating still II temperature, and pressure is 4 Mpa, essential oil and CO
2Realize separating and bottom separating still I and separating still II, emitting CO
2By flowmeter, enter ice chest liquefaction through the clarifier I, recycle.1.5 behind the h product of collecting must be made with extra care essential oil 62.8 g in 4 ℃ of lower pre-freeze 4 h by centrifugal 5 min of 10000 r/min, extraction yield is 6.28%.
Through according to GC-MS essential oil assay method test sample, detect altogether 135 kinds of compositions, mainly contain: 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 that waits is: 4.2%, (the GC-MS GC-MS is analyzed the 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 that waits 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
With the Ligusticum wallichii that 1Kg dries in the shade, be crushed to 40 orders, control dehydration separating still temperature is 70 ℃, and pressure is 18Mpa, and separating still I temperature is 30 ℃, and pressure is 6Mpa, dewatering time is 1h.The pressure of control extraction kettle is 28MPa, temperature setting is set to 39 ℃, the pressure of separating still I is adjusted to 11MPa, temperature setting is set to 52 ℃, separating II pressure is 5Mpa, and temperature is 45 ℃, extracts 2 hours, collect essential oil and must make with extra care essential oil 87.8g after 2 ℃ of pre-freeze 4h filter by 30 μ m, extraction yield is 8.78%.
Through according to GC-MS essential oil assay method test sample, detect altogether 142 kinds of compositions, mainly contain: 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, Ceng Zhi, Xie Runqian, Tan Lixian, the recovery rate that waits is: 7.60%, only detect 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 (5)
1. a Chinese herb dewatering is characterized in that, carries out supercritical CO
2Dehydration: the extraction kettle of packing into of the Chinese medicine after will pulverizing, controlling extraction kettle pressure is 8 MPa ~ 28 MPa, the extraction kettle temperature is 35 ℃ ~ 75 ℃, separating still pressure 4 Mpa ~ 12 Mpa, the separating still temperature is 20 ℃ ~ 60 ℃.
2. a method of extracting essential oil of traditional Chinese medicine is characterized in that, comprises the steps: (1) supercritical CO
2Dehydration; (2) supercritical CO
2Extraction, supercritical CO wherein
2Dehydration as claimed in claim 1.
3. a kind of method of extracting essential oil of traditional Chinese medicine of claim 2 is characterized in that described supercritical CO
2Extraction is: the extraction kettle temperature is controlled to be 36 ℃ ~ 39 ℃, and extraction kettle pressure is 26 MPa ~ 28 MPa, dynamic extraction 1.5 h ~ 3 h.
4. claim 2 or 3 method comprise the steps: that also (3) are centrifugal or filter.
5. the method for claim 4 is characterized in that, described centrifugal centrifugal rotational speed is 6000 r/min ~ 14000 r/min, and the pore size filter of described filtration is 70 μ m ~ 110 μ m.
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Cited By (3)
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| CN103710152A (en) * | 2013-10-28 | 2014-04-09 | 黄山神草生物科技有限公司 | Method for using supercritical carbon dioxide for extraction of 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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| 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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