CN103789094A - Method for extracting agilawood essential oil from agilawood chips - Google Patents
Method for extracting agilawood essential oil from agilawood chips Download PDFInfo
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Abstract
The invention relates to a method for extracting agilawood essential oil from agilawood chips with extremely low aroma content. The method comprises the following steps: grinding the agilawood chips, extracting by taking ethanol as a solvent at a relatively low temperature of 30-60 DEG C or performing continuous microwave extraction by taking ethanol with a solvent; freezing the obtained preliminary extract at (-7)-(-18) DEG C for 5-20h; performing suction filtration when the extract is cold, and performing reduced-pressure recovery of the solvent to obtain an extract; adding an adsorbent of which the weight is 0.5-2(w:w) times the weight of the extract into the extract, and uniformly mixing the two to obtain a dry sample; loading the sample to a glass chromatographic column with a length-diameter ratio of 5-15; flushing the column with the mixed solvent, and collecting the eluent; and evaporating out the mixed solvent at a vacuum degree of 0.02-0.09MPa in a water bath with the temperature of 40-65 DEG C to obtain the agilawood essential oil. By adopting the method provided by the invention, the obtained agilawood essential oil product has light brown color, uniform and transparent appearance and good fluidity; and the process enriches and protects the aromatic thermosensitive components in the agilawood to the greatest degree, and the aroma is pure and full.
Description
Technical field
The present invention relates to volatile oil, be specifically related to from measuring extraction extremely low agalloch eaglewood wood chip, separation refining agalloch eaglewood essential oil containing perfume.
Background technology
Agalloch eaglewood is that thymelaeceae agalloch eaglewood belongs to (Aquilaria agalocha Roxb.) or thymelaeceae agalloch eaglewood belongs to resinous position in Lignum Aquilariae Resinatum [Aquilaria sinensis (Lour.) Gilg] trees.Northeast, Indonesia archipelago and Papua New Guinea archipelago of mainly originating from the South Asian Subcontinent, be referred to as import agalloch eaglewood; China agalloch eaglewood mainly originates from the provinces and regions such as Guangdong, Hainan, Yunnan, Fujian, is referred to as domestic agalloch eaglewood.In agalloch eaglewood, being mainly flavour ingredient is with sesquiterpene and containing oxygen derivative class, aromatics, lipid acid and lipid thereof and chromogen ketone etc.Agalloch eaglewood derives from agallochum and is subject to the secreted resin of the impact such as exterior injury or pathology own, it is parasitic that it is invaded by the microorganism of Menanotus flavoliven, under the effect of thalline endoenzyme, there are a series of variations, and through depositing for many years and a kind of special material that is rich in fragrance forming.
Having many uses of agalloch eaglewood, it has the effect except numbness of promoting the circulation of QI to relieve pain, establishing-Yang clinically, and functional dyspepsia, acute episode of cor pulmonale by combination, stomachache etc. are had to significant curative effect; Agalloch eaglewood is as a kind of Chinese medicine, it has helping inspiration to relieve asthma, be open to the custom have one's ideas straightened out, the effect such as unimpeded gaseous pulse.At ancient Chinese, agalloch eaglewood has very high status in numerous spices, often makes main note and uses, and its fragrance is thick and heavy lasting, and economic worth is high.
Publication number is the extracting method that the application for a patent for invention of CN103184102A discloses a kind of agalloch eaglewood essential oil, and the method has following steps, first cuts down Lignum Aquilariae Resinatum tree, removes whitewood, carves agalloch eaglewood thin slice; Again agalloch eaglewood thin slice is ground into the agalloch eaglewood powder of 40 mesh sieves; Then agalloch eaglewood powder is added to extraction kettle with normal butane, adopts subcritical fluid extraction technology directly to extract agalloch eaglewood essential oil; Subsequently the slag after the agalloch eaglewood essential oil extracting is for the first time added to extraction kettle with 95% ethanol and extracts for the second time extraction agalloch eaglewood essential oil; Wherein, for the first time extraction conditions and for the second time extraction conditions be: extraction time is 0.5～1.5h, and resolution temperature is 60 ℃, extract temperature 50 C, extraction pressure is 0.4～0.5MPa.Described in above-mentioned patent application, method is in fact that agalloch eaglewood face cream is extracted, and this face cream oleaginousness is very high, and price is extremely expensive, thus deduct a percentage point relatively simple, need not refining pure metallization processes, thus obtained agalloch eaglewood essential oil product price is also very high.
Publication number is that the application for a patent for invention of CN103351954A discloses a kind of technique with supercritical carbon dioxide extraction agalloch eaglewood essential oil, this technique comprises the following steps: (1) pulverizes agalloch eaglewood, alcohol immersion with 95% 12 hours, the mass ratio of agalloch eaglewood and ethanol is 1 ︰ 5; (2) agalloch eaglewood is filtered, get alcohol immersion liquid Rotary Evaporators rotary evaporation and obtain agalloch eaglewood lotion; (3) agalloch eaglewood lotion being put into supercritical extraction reactor extracts, flash trapping stage, the processing parameter of supercritical extraction operation arranges as follows: extracting pressure 21-25Mpa, temperature 45-47 ℃, CO 2 fluid flow is 2-6L/h, separating pressure is 8Mpa, and separation temperature is all 40 ℃, collects agalloch eaglewood essential oil.Described in above-mentioned patent application, method length consuming time, higher to equipment requirements, and production cost is also higher simultaneously.
Research paper has in the past been reported steam distillation, solvent refluxing extraction method and supercritical carbon dioxide process.Steam distillation oil yield is extremely low, extraction temperature is high, the time is long, simultaneously, high temperature causes destruction and the loss of part volatile component, as, Wu Zhicheng etc. study a literary composition (Wu Zhicheng at the Gas Chromatography Fingerprint of LIGNUM AQUILARIAE SINENSIS from Hainan of China volatile oil, Huang Weiqian, Hu Guanglin etc. the Gas Chromatography Fingerprint research [J] of LIGNUM AQUILARIAE SINENSIS from Hainan of China volatile oil. chemical analysis metering .2009,18 (3): 23-24) in, adopt GC-MS technology for detection steam distillation to obtain the chemical composition of essential oil, obtain 14 aroma components; Complicated component that solvent-extraction process is carried, the equal difficulty of quality and outward appearance reaches market demands, as, Hao Lanfang etc. are at agalloch eaglewood Analysis of The Essential Oil one literary composition (Hao Lanfang, Li Huifen, week is bright. agalloch eaglewood Analysis of The Essential Oil [J]. and herbal medicine, 2010,14 (02): 210～211.), adopt GC-MS technology for detection solvent method to obtain the chemical composition of essential oil, obtain 40 aroma components; It is the expensive agalloch eaglewood raw material design for floorboard with high oil content that supercritical methanol technology is extracted, and is not suitable for the extraction of essential oil in the agalloch eaglewood of utmost point low levels, as, the supercritical CO of the essential oil in agalloch eaglewood such as Deng Hongmei
2extraction and GC-MS analyze a literary composition (Deng Hongmei, Zhou Rujin, Tong Hanqing. the supercritical CO of essential oil in agalloch eaglewood
2extraction and GC-MS thereof analyze [J] .2008, and 23 (06): 633～635.), adopt GC-MS technology for detection supercritical CO
2method obtains the chemical composition of essential oil, obtains 54 aroma components.
Chen Zhixiong etc. are at " dynamically-microwave assisting method extracts the pilot process research of an agalloch eaglewood essential oil " literary composition (Chen Zhixiong, Fan Yaming, He Zhizhou etc. dynamically-microwave assisting method extracts the pilot process research [J] of agalloch eaglewood essential oil. food science and technology, 2012, 37 (08): 200～203.) disclose a kind of extracting method that extracts agalloch eaglewood essential oil, the method is pulverized agalloch eaglewood, utilize dynamically-microwave-assisted technology, agalloch eaglewood is extracted as extracting solvent using ethanol-water, and to low temperature, the closely-related raw meal particle size of dynamic process, solid-to-liquid ratio, factor and solvent polarity that mass flow and preheating temperature etc. are relevant are studied, thereby obtain following best pilot process parameter: alcohol concn is 93%, raw meal particle size is 40 orders, solid-to-liquid ratio is 1:8.5, mass flow 78L/h, 45 ℃ of preheating temperatures, 15 ℃ of temperature rises, extract with this understanding 2 times.Under the condition of above-mentioned optimal processing parameter, the productive rate of agalloch eaglewood crude extract is 6.9%, and linaloe oil yield is 0.68%, and product mobility and transparency are good, has the distinctive permanent fragrance of agalloch eaglewood.This article primary study the impacts on leaching process and extraction yield such as pilot scale stage each major influence factors-material particles size, solid-to-liquid ratio, mass flow, the separation purifying technique of agalloch eaglewood essential oil is not studied.
Summary of the invention
In view of prior art exists above-mentioned deficiency, technical problem solved by the invention is to provide a kind of Technology of the extraction separation agalloch eaglewood essential oil that is easy to implement, is easy to suitability for industrialized production.
According to the feature that in agalloch eaglewood essential oil, some aroma component can only just not be destroyed at a lower temperature, be chosen at lower temperature extract by solvents under microwave irradiation or heating condition, just extract obtains through the column chromatography technology of subzero fractionation, absorption and Desorption separation the agalloch eaglewood essential oil that fragrance is complete, thereby takes full advantage of agalloch eaglewood resource.Its technique is:
The scheme that the present invention solves the problems of the technologies described above is:
A method of extracting agalloch eaglewood essential oil from agalloch eaglewood wood chip, the method is made up of following steps:
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 20～80 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder, add 5～15 times of (w ︰ ethanol that v) volumetric concentration is 70～100%, temperature be 30～60 ℃, microwave power (W) with the ratio of material flow (L/h) condition that is 10～55 under carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 2～5 times with same condition again, and merging filtrate obtains the alcoholic solution liquid of microwave extraction; Or,
Get agalloch eaglewood powder, add 5～15 times of (w ︰ ethanol that v) volumetric concentration is 70～100%, be to extract 0.5～12h under the condition of 30～60 ℃ in temperature, centrifugation, collect filtrate, it is that 70～100% ethanol is to extract 2～5 times under the condition of 1 ︰ 3～1 ︰ 7 in solid-to-liquid ratio that filter residue adds volumetric concentration, and merging filtrate, obtains alcohol extract;
Be that 0.05～0.1MPa and bath temperature are under 40～80 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution liquid of obtained microwave extraction or alcohol extract in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5～20h at-7～-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5～2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 5～15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 40～65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02～0.09MPa in vacuum tightness, obtain agalloch eaglewood essential oil.Wherein, described sorbent material is silica gel; Described mixed solvent is Shi You Mi ︰ chloroform=1 ︰ 0～10 ︰ 1(V ︰ V) sherwood oil-chloroform solvent, Shi You Mi ︰ acetone=60 ︰ 1～1 ︰ 1(V ︰ V) sherwood oil-acetone solvent or Shi You Mi ︰ ethyl acetate=60 ︰ 1～1 ︰ 1(V ︰ V) sherwood oil-ethyl acetate solvent.
In aforesaid method, the preferred value of the length-to-diameter ratio of described glass chromatography column is 8～15; The particle diameter of described silica gel is 60～400 orders, preferential 200～300 orders.
The method of the invention compared with prior art has following beneficial effect:
The content that the present invention is directed to agalloch eaglewood essential oil in agalloch eaglewood wood chip is only the physicochemical property of contained chemical composition in 0.1～1% feature and agalloch eaglewood essential oil; first extract under the low temperature conditions of 30～60 ℃ take aqueous ethanol as solvent; selecting length-to-diameter ratio is that 5～15 glass chromatography column carries out purifying again; not only protect to greatest extent fragrant heat-sensitive ingredients; make in gained agalloch eaglewood essential oil aroma component up to 58～68 kinds more than; thereby product fragrance is pure and complete; outward appearance homogeneous transparent, good fluidity.In addition, the present invention also has advantages of that method is simple and is easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the GC-MS total ion current figure of a specific embodiment gained agalloch eaglewood essential oil.
Fig. 2 is the GC-MS total ion current figure of another specific embodiment gained agalloch eaglewood essential oil.
Embodiment
Embodiment 1
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 20 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 300L volumetric concentration is 70% ethanol, in temperature being at 30 ℃, controlling microwave power is that 3200W and material flow are that 320L/h(is that the ratio of microwave power and material flow is 10) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 2 times with same condition again, and merging filtrate obtains microwave extraction alcoholic solution liquid;
Be that 0.05MPa and bath temperature are under 40 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5h at-7 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, length-to-diameter ratio is 15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 40 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 275ml(productive rate is 1.10%).In this example, mixed solvent used is sherwood oil-chloroform solvent of Shi You Mi ︰ chloroform=6 ︰ 1; Sorbent material used is 60～120 order silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 20 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 70% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains microwave extraction alcoholic solution;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 1.2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 10, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 340ml(productive rate is 1.36%).
In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=10 ︰ 1; Sorbent material used is 200～300 order silica gel.
Embodiment 3
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 20 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 100% ethanol, in temperature being at 60 ℃, controlling microwave power is that 2400W and material flow are that 43L/h(is that the ratio of microwave power and material flow is 55) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 4 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.1MPa and bath temperature are under 80 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 20h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.09MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 50ml(productive rate is 0.2%).
In this example, mixed solvent used is sherwood oil-ethyl acetate solvent of Shi You Mi ︰ ethyl acetate=30 ︰ 1; Sorbent material used is 300～400 object silica gel.
Embodiment 4
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 70% ethanol, in temperature being at 30 ℃, controlling microwave power is that 3200W and material flow are that 320L/h(is that the ratio of microwave power and material flow is 10) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 5 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.09MPa and bath temperature are under 40 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5h at-7 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 5 glass chromatography column, rush post with mixed solvent, collect elutriant, in 65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 435ml(productive rate is 1.74%).
In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=6 ︰ 1; Sorbent material used is 60～120 object silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains the alcoholic solution liquid of microwave extraction;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution liquid of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 1.2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 8 glass chromatography column, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 370ml(productive rate is 1.48%).In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=10 ︰ 1; Sorbent material used is 60～120 object silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 100% ethanol, in temperature being at 60 ℃, controlling microwave power is that 2400W and material flow are that 43L/h(is that the ratio of microwave power and material flow is 55) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 2 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.1MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 20h at-7 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 18 glass chromatography column, rush post with mixed solvent, collect elutriant, in 65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 87.5ml(productive rate is 0.35%).
In this example, mixed solvent used is sherwood oil-ethyl acetate solvent of Shi You Mi ︰ ethyl acetate=20 ︰ 1; Sorbent material used is 300～400 order silica gel.
Embodiment 7
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 80 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 300L volumetric concentration is 70% ethanol, in temperature being at 30 ℃, controlling microwave power is that 3200W and material flow are that 320L/h(is that the ratio of microwave power and material flow is 10) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.05MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5h at-7 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 5 glass chromatography column, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 450ml(productive rate is 1.80%).
In this example, mixed solvent used is sherwood oil-chloroform solvent of Shi You Mi ︰ chloroform=6 ︰ 1; Sorbent material used is 60～120 object silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 80 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 4 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcohol liquid of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 1.2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 10 glass chromatography column, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 412.5ml(productive rate is 1.65%).In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=10 ︰ 1; Sorbent material used is 200～300 object silica gel.
Embodiment 9
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 80 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 100% ethanol, in temperature being at 60 ℃, controlling microwave power is that 2400W and material flow are that 43L/h(is that the ratio of microwave power and material flow is 55) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 4 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction;
Be that 0.1MPa and bath temperature are under 80 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 20h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 102.5ml(productive rate is 0.41%).In this example, mixed solvent used is sherwood oil-ethyl acetate solvent of Shi You Mi ︰ ethyl acetate=10 ︰ 1; Sorbent material used is 300～400 object silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 20 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 300L volumetric concentration is 70% ethanol, is to extract 12h under the condition of 30 ℃ in temperature, centrifugation, collects filtrate, and it is that 80% ethanol is to extract 5 times under the condition of 1 ︰ 3 in solid-to-liquid ratio that filter residue adds volumetric concentration, merging filtrate, obtains alcohol extract;
Be that 0.05MPa and bath temperature are under 40 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained alcohol extract in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5h at-7 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 10 glass chromatography column, rush post with mixed solvent, collect elutriant, in 40 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 377.5ml(productive rate is 1.51%).In this example, mixed solvent used is sherwood oil-chloroform solvent of Shi You Mi ︰ chloroform=6 ︰ 1; Sorbent material used is 60～120 object silica gel.
Embodiment 11
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, is to extract 6h under the condition of 50 ℃ in temperature, centrifugation, collects filtrate, and it is that 70% ethanol is to extract 4 times under the condition of 1 ︰ 5 in solid-to-liquid ratio that filter residue adds volumetric concentration, merging filtrate, obtains alcohol extract;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained alcohol extract in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 1.2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 307.5ml(productive rate is 1.23%).In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=10 ︰ 1; Sorbent used is 200～300 object silica gel.
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 80 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 100L volumetric concentration is 100% ethanol, is to extract 2.5h under the condition of 60 ℃ in temperature, centrifugation, collects filtrate, and it is that 95% ethanol is to extract 2 times under the condition of 1 ︰ 7 in solid-to-liquid ratio that filter residue adds volumetric concentration, merging filtrate, obtains alcohol extract;
Be that 0.1MPa and bath temperature are under 80 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained alcohol extract in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 20h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 18 glass chromatography column, rush post with mixed solvent, collect elutriant, in 65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.07MPa in vacuum tightness, obtaining agalloch eaglewood essential oil 62.5ml(productive rate is 0.25%).In this example, mixed solvent used is sherwood oil-ethyl acetate solvent of Shi You Mi ︰ ethyl acetate=1 ︰ 0; Sorbent used is 300～400 object silica gel.
Embodiment 13(flavour ingredient is identified)
One, embodiment 5 gained agalloch eaglewood essence oil identifying
The agalloch eaglewood essential oil that above-described embodiment 5 is obtained adopts its chemical composition of GC-MS technical measurement, obtains GC-MS total ion current figure as shown in Figure 1.Concrete measuring method is as described below:
(1) sampling method: adopt the sampling of solid-phase microextraction (SPME) head space.Select PDMS fiber head (redness), get essential oil 1.0 μ L, be placed in the extraction of head space bottle SPME device.Extraction temperature: 80 ℃; Extraction time: 30m in; Desorption temperature: 220 ℃.
(2) measuring method: SPME thermal desorption split stream sampling, splitting ratio 80 ︰ 1; Injector temperature is 220 ℃; DB-5 quartz capillary column (30m × 0.23mmID × 0.25m); Carrier gas: helium; Flow velocity: 1mL/min; Heating schedule: 60 ℃ of initial temperatures, keep 3min, rise to 130 ℃ with 6 ℃/min, then rise to 180 ℃ with 2 ℃/min, finally rise to 270 ℃ with 10 ℃/min; Mass spectrum condition: EI source, electron energy: 70eV; Detect voltage 380V; Detect mass range of ions: m/z33～450u; 230 ℃ of interface temperature; 220 ℃ of ion source temperatures.
Adopt NIST database retrieval, the corresponding mass spectrum of each chromatographic peak as calculated machine spectrum storehouse positive and negative two, to retrieval qualitative identification, is selected the result for retrieval of higher matching degree, and the key odorant composition of embodiment 5 gained agalloch eaglewood essential oils is as shown in table 1 below.
The GC-MS analytical results of table 1 embodiment 5 gained agalloch eaglewood essential oils
Two, embodiment 11 gained agalloch eaglewood essence oil identifying
The agalloch eaglewood essential oil that above-described embodiment 11 is obtained adopts its chemical composition of GC-MS technical measurement, obtains GC-MS total ion current figure as shown in Figure 2.Concrete measuring method is identical with the authentication method of above-described embodiment 5 gained agalloch eaglewood essential oils, and result is as shown in existing table 2.
The GC-MS analytical results of table 2 embodiment 11 gained agalloch eaglewood essential oils
Adopting the agalloch eaglewood essential oil using the same method to above-described embodiment 1～4 and 6～10 and 12 detects, wherein, GC-MS total ion current figure and Fig. 1 that embodiment 1～4 and 6～9 obtains are basically identical, and GC-MS total ion current figure and Fig. 2 that embodiment 10 and 12 obtains are basically identical; Adopt NIST database retrieval, the corresponding mass spectrum of each chromatographic peak as calculated machine is composed storehouse positive and negative two to retrieval qualitative identification, select the result for retrieval of higher matching degree, wherein, embodiment 1～4 is the same with table 1 with the chemical composition in 6～9 gained agalloch eaglewood essential oils, and embodiment 10 is the same with table 2 with the chemical composition in 12 gained agalloch eaglewood essential oils.
The impact of embodiment 14(elutriant on effect)
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains microwave extraction alcoholic solution;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained microwave extraction liquid in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, medicinal extract is divided into 8 parts, and to adding w) sorbent material doubly of its weight 1.2(w ︰ in every part of medicinal extract, the two is mixed as dry-eye disease, be splined on respectively length-to-diameter ratio and be 8 glass chromatography column, every silica gel column chromatography rushes post with different elutriants, collecting elutriant, in 50 ℃ of water-baths, is to volatilize solvent under 0.07MPa in vacuum tightness, obtain agalloch eaglewood essential oil, its result is as shown in table 3.In this example, in glass chromatography column used, the particle diameter of silica gel is 60～120 orders.
The impact of the selection of different elutriants on separating effect in table 3 column chromatography for separation process
The impact of embodiment 15(chromatography column length-to-diameter ratio on effect)
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains microwave extraction alcoholic solution;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained microwave extraction liquid in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, medicinal extract is divided into 8 parts, and to adding w) sorbent material doubly of its weight 0.5(w ︰ in every part of medicinal extract, the two is mixed as dry-eye disease, be splined on respectively length-to-diameter ratio 0～5, 5～10, 10～15, 15～20 with the glass chromatography column that is greater than these 5 kinds of different length-to-diameter ratios of scope of 20, rush post with mixed solvent, collect elutriant, in 50 ℃ of water-baths, be to volatilize mixed solvent under 0.07MPa in vacuum tightness, obtain agalloch eaglewood essential oil, its result is as shown in table 4.In this example, mixed solvent used is sherwood oil-acetone solvent of Shi You Mi ︰ acetone=10 ︰ 1; In glass chromatography column used, the particle diameter of silica gel is 60～120 orders.
The impact of the ratio (H/D) of sorbent material height of materials H and column internal diameter D on separating effect in table 4 chromatography column
By the agalloch eaglewood essential oil after column chromatography purification in embodiment 5 under the condition of 20 ℃, becoming mass concentration with 95% alcohol dilution is respectively 1/10,1/100,1/1000 solution, pick respectively the solution of these 3 kinds of concentration with Wen Xiangzhi, Wen Xiangzhi is swung in air to 1min, after volatilizing ethanol, hear its fragrance, its result is as shown in table 5 again.
Table 5 is evaluated the experimental result of agalloch eaglewood essential oil fragrance
Adopt the agalloch eaglewood essential oil using the same method to above-described embodiment 1～4 and 6～12 and carry out fragrance evaluation, the result of gained is consistent with table 5, illustrates that obtained agalloch eaglewood essential oil concentration is high, can dilute 1000 times and use above.
Embodiment 17
Under the condition of 20 ℃, get and in 2 embodiment 16, dilute the agalloch eaglewood essential oil solution of 100 times in wrist place,, hear its fragrance at interval of 4h, probe into the retention time of essential oil fragrance, its result is as shown in table 6.
The experimental result of table 6 agalloch eaglewood essential oil fragrance retention time
Adopting uses the same method carries out fragrance retention time to the agalloch eaglewood essential oil of above-described embodiment 1～4 and 6～12 and probes into, the result of gained is consistent with table 6, illustrate that obtained agalloch eaglewood essential oil fragrance is sustainable more than 16 hours, its fragrance is quiet and tastefully laid out lastingly, is suitable for preparing high-grade perfume and other daily use chemicals spices.
The impact of the different sorbent material of embodiment 18(on effect)
(1) will near agalloch eaglewood Edgeworthia chrysantha place, be broken into the agalloch eaglewood powder of 40 mesh sieves containing the wood dust of a small amount of face cream;
(2) get agalloch eaglewood powder 20kg, adding 200L volumetric concentration is 95% ethanol, in temperature being at 50 ℃, controlling microwave power is that 4800W and material flow are that 160L/h(is that the ratio of microwave power and material flow is 30) carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 3 times with same condition again, and merging filtrate obtains microwave extraction alcoholic solution;
Be that 0.09MPa and bath temperature are under 60 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by obtained microwave extraction liquid in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 12h at-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, and medicinal extract is divided into 4 parts, and respectively to adding w) aluminum oxide, macroporous resin D doubly of its weight 0.5(w ︰ in every part of medicinal extract
101, polymeric amide or 200～300 object silica gel absorbers, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 8 glass chromatography column, rush post with different blended bonding solvent, collecting elutriant, in 50 ℃ of water-baths, is to volatilize mixed solvent under 0.07MPa in vacuum tightness, obtain agalloch eaglewood essential oil, its result is as shown in table 7.
The impact of the different sorbent materials of table 7 on separating effect
Claims (4)
1. a method of extracting agalloch eaglewood essential oil from agalloch eaglewood wood chip, the method is made up of following steps:
(1) near the wood dust containing a small amount of face cream agalloch eaglewood Edgeworthia chrysantha place is broken into 20～80 object agalloch eaglewood powder;
(2) get agalloch eaglewood powder, add 5～15 times of (w ︰ ethanol that v) concentration is 70～100%, temperature be 30～60 ℃, microwave power (W) with the ratio of material flow (L/h) condition that is 10～55 under carry out continuous microwave extraction, vacuum filtration, collect filtrate, filter residue is carried 2～5 times with same condition again, and merging filtrate obtains the alcoholic solution of microwave extraction; Or,
Get agalloch eaglewood powder, add 5～15 times of (w ︰ ethanol that v) concentration is 70～100%, be to extract 0.5～12h under the condition of 30～60 ℃ in temperature, centrifugation, collect filtrate, it is that 70～100% ethanol is to extract 2～5 times under the condition of 1 ︰ 3～1 ︰ 7 in solid-to-liquid ratio that filter residue adds volumetric concentration, and merging filtrate, obtains alcohol extract;
Be that 0.05～0.1MPa and bath temperature are under 40～80 ℃ of conditions, to reclaim the medicinal extract that at 60 ℃ of ethanol simmer down tos, relative density is 0.8～1.5 by the alcoholic solution of obtained microwave extraction or alcohol extract in vacuum tightness, obtain just extract of agalloch eaglewood;
(3) by just extract freezing 5～20h at-7～-18 ℃ of the agalloch eaglewood of step (2) gained, take advantage of cold-draw filter, decompression and solvent recovery obtains medicinal extract, to adding w) sorbent material doubly of its weight 0.5～2(w ︰ in medicinal extract, the two is mixed as dry-eye disease, be splined on length-to-diameter ratio and be 5～15 glass chromatography column, rush post with mixed solvent, collect elutriant, in 40～65 ℃ of water-baths, be evaporate to dryness mixed solvent under 0.02～0.09MPa in vacuum tightness, obtain agalloch eaglewood essential oil; Wherein, described sorbent material is silica gel; Described mixed solvent is Shi You Mi ︰ chloroform=1 ︰ 0～10 ︰ 1(V ︰ V) sherwood oil-chloroform solvent, Shi You Mi ︰ acetone=60 ︰ 1～1 ︰ 1(V ︰ V) sherwood oil-acetone solvent or Shi You Mi ︰ ethyl acetate=60 ︰ 1～1 ︰ 1(V ︰ V) sherwood oil-ethyl acetate solvent.
2. a kind of method of extracting agalloch eaglewood essential oil from agalloch eaglewood wood chip according to claim 1, is characterized in that, the length-to-diameter ratio of described glass chromatography column is 8～15.
3. a kind of method of extracting agalloch eaglewood essential oil from agalloch eaglewood wood chip according to claim 1 and 2, is characterized in that, the particle diameter of described silica gel is 60～400 orders.
4. a kind of method of extracting agalloch eaglewood essential oil from agalloch eaglewood wood chip according to claim 3, is characterized in that, described particle diameter is 200～300 orders.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2151787C1 (en) * | 1998-11-30 | 2000-06-27 | Товарищество с ограниченной ответственностью Научно-производственная коммерческая фирма "Техноком" | Method of fermentation of essential-oil raw |
| CN101665401A (en) * | 2009-09-24 | 2010-03-10 | 山东大学 | Method for separating alkene effective constituents in ginger essential oil |
| FR2960000A1 (en) * | 2010-05-12 | 2011-11-18 | Univ D Avignon Et Des Pays De Vaucluse | Reducing amount of furocoumarins in preparation of essential oil, comprises submitting portion of plant containing furocoumarins to microwave radiation, placing obtained extract to fall by gravity out of microwave oven and recovering oil |
| CN103184102A (en) * | 2013-01-14 | 2013-07-03 | 中山市国林沉香科学研究所 | Extraction method and application of agilawood essential oil |
-
2014
- 2014-01-21 CN CN201410028499.7A patent/CN103789094A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2151787C1 (en) * | 1998-11-30 | 2000-06-27 | Товарищество с ограниченной ответственностью Научно-производственная коммерческая фирма "Техноком" | Method of fermentation of essential-oil raw |
| CN101665401A (en) * | 2009-09-24 | 2010-03-10 | 山东大学 | Method for separating alkene effective constituents in ginger essential oil |
| FR2960000A1 (en) * | 2010-05-12 | 2011-11-18 | Univ D Avignon Et Des Pays De Vaucluse | Reducing amount of furocoumarins in preparation of essential oil, comprises submitting portion of plant containing furocoumarins to microwave radiation, placing obtained extract to fall by gravity out of microwave oven and recovering oil |
| CN103184102A (en) * | 2013-01-14 | 2013-07-03 | 中山市国林沉香科学研究所 | Extraction method and application of agilawood essential oil |
Non-Patent Citations (2)
| Title |
|---|
| 袁观富，等: ""海南沉香精油挥发性成分的GC-MS测定及呈香分析"", 《广州大学学报（自然科学版）》 * |
| 陈志雄，等: ""动态-微波辅助法提取沉香精油的中试工艺研究"", 《食品科技》 * |
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Application publication date: 20140514 |