CN108690726A - The method that extraction oil of badian is combined with distillation using ultrasonication - Google Patents
The method that extraction oil of badian is combined with distillation using ultrasonication Download PDFInfo
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- CN108690726A CN108690726A CN201810766145.0A CN201810766145A CN108690726A CN 108690726 A CN108690726 A CN 108690726A CN 201810766145 A CN201810766145 A CN 201810766145A CN 108690726 A CN108690726 A CN 108690726A
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- ultrasonication
- badian
- distillation
- oil
- leaf
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- 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
-
- 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
- C11B9/025—Recovery by solvent extraction
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to a kind of methods combining extraction oil of badian with distillation using ultrasonication, including win octagonal tree branches and leaves, multigelation, chopping, ultrasonication, filtering, the preparation processes such as distillation, water removal.The present invention handles octagonal tree branches and leaves using ultrasonication, there is mechanical effect, cavitation effect, fuel factor using ultrasonic wave, and the second order effects such as emulsify, spread, smashing, increase the permeability of cell wall, increase the movement velocity of the penetration power and medium molecule of medium, the dissolution for promoting active ingredient has many advantages, such as that easy to operate, recovery rate is high, extraction time is short, saves resource;The present invention carries out ultrasonic extraction under cryogenic, it is possible to reduce the loss of volatile oil improves the recovery rate of oil of badian.
Description
Technical field
The present invention relates to field of agricultural products processing, combine extraction octagonal using ultrasonication and distillation more particularly to a kind of
The method of fennel oil.
Background technology
Oil of badian is the mixture for the composition complexity extracted from positions such as Illicillm Verum Fruit, branch, leaves, has and kills
Worm, sterilization, anti-oxidant isoreactivity are widely used in food, medicine and cosmetic field.It is octagonal due to the difference of production technology
There are larger difference, purposes is also different for fennel oil chemical composition and physiological activity.Steam distillation extraction oil of badian be
Colourless to light yellow clear liquid, but yield is relatively low, and production cost is higher, is generally used for food additives or field of medicaments;
The oil of badian of organic solvent extraction is that green can be used as to brown viscous liquid containing ingredients such as volatile oil, vinegar and resins
The raw material and antioxidant of essence material;The Chinese anise oil quality of supercritical fluid extraction is preferable, but equipment is expensive, operating cost
It is high, it is difficult to realize industrialized production;Ultrasonic wave extraction is a kind of novel technology, compared with conventional method, and the time is short, efficiency
It is high, easy to operate, at low cost.But pass through retrieval and find, it is also fewer for the research of ultrasonic wave extraction oil of badian.
The disclosure of background above technology contents is only used for inventive concept and the technical solution that auxiliary understands the present invention, not
The prior art for necessarily belonging to present patent application, no tangible proof show the above present patent application the applying date
In the case of having disclosed, above-mentioned background technology should not be taken to the novelty and creativeness of evaluation the application.
Invention content
Present invention aims at a kind of method combining extraction oil of badian with distillation using ultrasonication is proposed, with solution
The technical problems such as certainly above-mentioned extraction cost of the existing technology is high, complicated for operation, efficiency is low, oil of badian poor quality.
A method of combine extraction oil of badian, specific technical solution as follows using ultrasonication and distillation.
A method of extraction oil of badian is combined using ultrasonication and distillation, is included the following steps:
S1:Fresh octagonal branch, leaf are won, multigelation is carried out to octagonal branch;
S2:Octagonal leaf is cut into filiform, water is added the leaf not cut through, impregnates 1-3h, solid-liquid ratio 1:15-1:40,
Ultrasonication 1-3h is carried out under the frequency of 600-1000w;
S3:The branches and leaves filtering that broken wall is crossed, filtrate are distilled, are removed water to get oil of badian.
The described method that extraction oil of badian is combined with distillation using ultrasonication, the processing method include with
Lower step:
S1:Fresh octagonal branch, leaf are won, multigelation is carried out to octagonal branch;
S2:Octagonal leaf is cut into filiform, water is added the leaf not cut through, impregnates 1-3h, solid-liquid ratio 1:23-1:32,
Ultrasonication 1.5-2.5h is carried out under the frequency of 700-900w;
S3:The branches and leaves filtering that broken wall is crossed, filtrate are distilled, are removed water to get oil of badian.
Described combines the method for extracting oil of badian using ultrasonication and distillation, and the branches and leaves described in step S1 are 3-
Branch, the leaf of the Chinese anise of picking in May, a diameter of 0.01-0.1cm of the branch.
Described combines the method for extracting oil of badian, the ultrasonication described in step S2 using ultrasonication and distillation
It is carried out under the conditions of 0-6 DEG C.
The described method for combining extraction oil of badian with distillation using ultrasonication, the ultrasonication time is
2h。
The method for combining extraction oil of badian with distillation using ultrasonication, the chopping is to cut leaf
At the filiform of 0.5-1.5mm.
The method for combining extraction oil of badian with distillation using ultrasonication, the temperature of the distillation are
50-70 DEG C, time 3-4h.
The method for combining extraction oil of badian with distillation using ultrasonication, the water removal need to use nothing
Aqueous sodium persulfate is stirred, dries 0.5-1h, and the dosage of the anhydrous sodium sulfate is the 10-15% of feed liquid gross weight.
Compared with prior art, the present invention there is advantageous effect below:
(1) present invention handles octagonal tree branches and leaves using ultrasonication, using ultrasonic wave there is mechanical effect, cavitation to imitate
The second order effects such as answer, fuel factor, and emulsify, spread, smashing, increase the permeability of cell wall, increase medium penetration power and
The movement velocity of medium molecule promotes the dissolution of active ingredient, has many advantages, such as that easy to operate, recovery rate is high, extraction time is short;
The process cycle of extraction oil of badian can be shortened, save the energy;
(2) present invention can make the broken wall of Chinese anise leaf using octagonal leaf elder generation's chopping in the technology for carrying out ultrasonication
Rate reaches 90%;
(3) octagonal leaf is cut into filament, is less than 0.01cm, the liquid in fresh leaf can be made to flow out, cause to volatilize
The waste of oil, the width more than 0.1cm cut can cause the recovery rate of oil of badian to reduce, some volatile oil cannot propose;
(4) method that the present invention first uses freeze thawing is handled loses part vigor by cell, is easy to extract oil of badian, contracting
The short technological process entirely extracted improves recovery rate;
(5) present invention carries out ultrasonic extraction under cryogenic, it is possible to reduce the loss of volatile oil improves oil of badian
Recovery rate;
(6) method that the present invention is combined using ultrasonication with distillation, promotes the extraction rate reached 10% of oil of badian,
Finished product is light yellow clear liquid, has strong Chinese anise smell, and it is low with solvent extraction face to solve steam distillation yield
Aberration has the problem of precipitation, oil of badian carry organic solvent smell.
Specific implementation mode
It is aforementioned broadly to have elaborated the feature and technical advantage of the present invention, so as to more fully understand the present invention's
Detailed description.The other feature and advantage of the present invention will be described below.It should be appreciated by those skilled in the art that the concept disclosed
It is used for changing or designing other structures based on being easily used as with specific embodiment to complete the phase of the present invention
Same purpose.Those skilled in the art are not it should also be appreciated that this equivalent construction offsets the spirit and scope of the present invention.
It is considered as the novel features of feature of the present invention, structure and operation method.However, it should profoundly recognize, provide
Each feature is merely to description and explanation, the definition without being intended to the limitation present invention.
Invention is further described in detail With reference to embodiment.It is emphasized that following the description is only
It is merely exemplary, the range being not intended to be limiting of the invention and its application.
One, specific embodiment
Embodiment 1
The method for combining extraction oil of badian with distillation using ultrasonication, specific technical solution are as follows:
S1:March picks branch, the leaf of Chinese anise, and a diameter of 0.01cm of branch freezes octagonal branch repeatedly
Melt;
S2:Octagonal leaf is cut into the filiform of 0.5mm, water is added the leaf not cut through, impregnates 1h, solid-liquid ratio 1:15,
Temperature is 0 DEG C, and ultrasonication 1h is carried out under the frequency of 600w;
S3:The branches and leaves that broken wall is crossed filter, and distillation 3h are carried out at 50 DEG C of filtrate, addition feed liquid gross weight is 10% anhydrous slufuric acid
Sodium is stirred, dries 0.5h water removals to get oil of badian.
Embodiment 2
The method for combining extraction oil of badian with distillation using ultrasonication, specific technical solution are as follows:
S1:Fresh octagonal branch, leaf are won, a diameter of 0.1cm of branch carries out multigelation to octagonal branch;
S2:Octagonal leaf is cut into the filiform of 1.5mm, water is added the leaf not cut through, impregnates 3h, solid-liquid ratio 1:40,
Temperature is 6 DEG C, and ultrasonication 3h is carried out under the frequency of 1000w;
S3:The branches and leaves that broken wall is crossed filter, and distillation 4h are carried out at 70 DEG C of filtrate, addition feed liquid gross weight is 15% anhydrous slufuric acid
Sodium is stirred, dries 1h water removals to get oil of badian.
Embodiment 3
The method for combining extraction oil of badian with distillation using ultrasonication, specific technical solution are as follows:
S1:Fresh octagonal branch, leaf are won, a diameter of 0.03cm of branch carries out multigelation to octagonal branch;
S2:Octagonal leaf is cut into the filiform of 0.5mm, water is added the leaf not cut through, impregnates 1h, solid-liquid ratio 1:23,
Temperature is 0 DEG C, and ultrasonication 1.5h is carried out under the frequency of 700w;
S3:The branches and leaves that broken wall is crossed filter, and distillation 3h are carried out at 55 DEG C of filtrate, addition feed liquid gross weight is 11% anhydrous slufuric acid
Sodium is stirred, dries 0.5h water removals to get oil of badian.
Embodiment 4
The method for combining extraction oil of badian with distillation using ultrasonication, specific technical solution are as follows:
S1:Fresh octagonal branch, leaf are won, a diameter of 0.07cm of branch carries out multigelation to octagonal branch;
S2:Octagonal leaf is cut into the filiform of 0.8mm, water is added the leaf not cut through, impregnates 3h, solid-liquid ratio 1:32,
Temperature is 2 DEG C, and ultrasonication 2.5h is carried out under the frequency of 900w;
S3:The branches and leaves that broken wall is crossed filter, and distillation 4h are carried out at 65 DEG C of filtrate, addition feed liquid gross weight is 13% anhydrous slufuric acid
Sodium is stirred, dries 1h water removals to get oil of badian.
Embodiment 5
The method for combining extraction oil of badian with distillation using ultrasonication, specific technical solution are as follows:
S1:Fresh octagonal branch, leaf are won, a diameter of 0.05cm of branch carries out multigelation to octagonal branch;
S2:Octagonal leaf is cut into the filiform of 1mm, water is added the leaf not cut through, impregnates 3h, solid-liquid ratio 1:32, temperature
Degree is 4 DEG C, and ultrasonication 2h is carried out under the frequency of 800w;
S3:The branches and leaves that broken wall is crossed filter, and distillation 3.5h are carried out at 60 DEG C of filtrate, addition feed liquid gross weight is 14% anhydrous sulphur
Sour sodium is stirred, dries 0.8h water removals to get oil of badian.
Comparative example 1
According to the preparation method of embodiment 1, remove the frequency control 600w or less of ultrasound.
Comparative example 2
According to the preparation method of embodiment 2, the FREQUENCY CONTROL by ultrasound is removed in 1000w or more.
Comparative example 3
According to the preparation method of embodiment 3, ultrasonication step is removed.
Comparative example 4
According to the preparation method of embodiment 5, removes and branch, leaf are subjected to multigelation.
Two, the detection of oil of badian
1. the detection method of sporoderm-broken rate
(1) it takes octagonal branch, foliage samples to be dried, is prepared into fine powder and micro mist;
(2) the step of 5-8 different weight is weighed within the scope of 0.05-1.5g (1) described fine powder, is dispersed in glycerine
In, it is microscopic count object to observe complete characteristic cell in fine powder by microscopic observation counting method, and carries out linear regression, draws mark
Directrix curve obtains regression curve equation, and correlation coefficient r in this step to regression curve equation is repeated and is more than 0.9, then carries out down
One step;
(3) micro mist and fine powder are weighed according to step (2) the method respectively, is observed by microscopic observation counting method wherein complete
Characteristic cell be microscopic count object, the microscopic features number of cells of fine powder and micro mist is calculated according to the following formula:
Wherein, X is the characteristic cell number in each visual field, and V is overall solution volume, and V ' is liquor capacity under coverslip, and W is
The sample amount of weighing;
According to the microscopic features number of cells of sample fine powder and micro mist, cell-wall breaking ratio is calculated according to the following formula:
Y=(A-B)/A × 100%
Wherein, Y is cell-wall breaking ratio, and A is micro mist microscopic features number of cells, and A is fine powder micro mist microscopic features cell
Number, B are micro mist microscopic features number of cells.
2. anethole assay
2.1 instruments and reagent
Japanese Shimadzu GC-14B gas chromatographs, Weil-McLain dragon chromatographic work station.
Anethole reference substance (trans-Anethol)s [It is provided by Sigma Co., USA, lot:S16146-453, content
99% (GC)s ];Naphthalene (analyzes pure, content 99%);Ethyl acetate (analysis is pure);Oil of badian control medicinal material is (by Chinese drug
Biological products assay institute provides.
2.2 methods and result
2..2.1 chromatographic condition chromatography column:With polyethylene glycol (PEG) -20M and silicone (OV-17) for fixer, apply
Cloth concentration is respectively 10% and 2%, and the carrier after coating is with (PEG is in injection port in 7: the 3 same column of ratio (weight ratio) loading
End), length 2m;Temperature programming:100 DEG C of pillar initial temperature keeps 5min;140 DEG C are risen to 4 DEG C/min, keeps 5min,
200 DEG C are risen to 10 DEG C/min, keeps 5min;Injector temperature:250℃;Detector:FID, 250 DEG C of temperature;Carrier gas N2:
60ml/min;Combustion-supporting gas air:50ml/min;Combustion gas H2:60ml/min;Sample size:1μl.Under above-mentioned chromatographic condition respectively into
Sample measures, the results showed that number of theoretical plate is calculated by anethole peak is not less than 10000, and anethole peak and internal standard compound naphthalene are and adjacent sets
Color separation spectral peak, which reaches, to be kept completely separate, and separating degree is more than 1.5, and anethole retention time is about 15min, and internal standard compound naphthalene retention time is about
For 13min.
2.2.2 the preparation of reference substance solution
Precision weighs fennel reference substance 2.06g in 25ml measuring bottles, and scale is dissolved and be diluted to ethyl acetate, is shaken up,
As anethole reference substance solution.
2.2.3 the preparation of inner mark solution
Precision weighs naphthalene 1.26g in 25ml measuring bottles, and scale is dissolved and be diluted to ethyl acetate, is shaken up, as interior
Mark solution.
2.2.4 the preparation of test solution
Oil of badian 0.18g is taken, it is accurately weighed, it sets in 10ml measuring bottles, inner mark solution 2ml is added in precision, adds acetic acid second
Ester is diluted to scale, shakes up, as test solution.
2.2.5 the investigation of linear relationship
It is accurate respectively to draw above-mentioned reference substance solution 0.5,1,2,3,4ml, it sets respectively in 10ml measuring bottles, in each accurate addition
Solution 2ml is marked, scale is diluted to ethyl acetate, is shaken up, by above-mentioned chromatographic condition, 1 μ l of each sample introduction are measured.With fennel
The ratio Y of brain integrating peak areas value and naphthalene integrating peak areas value carries out regression analysis to anethole sample size X, obtains regression equation.
2.2.6 the measurement of correction factor
Precision weighs naphthalene 1.25g, sets in 25ml measuring bottles, adds ethyl acetate to dissolve and is diluted to scale, shakes up, as interior
Mark solution.Precision weighs anethole reference substance 2.00g, sets in 25ml measuring bottles, and ethyl acetate is added to dissolve and be diluted to
Scale shakes up, as anethole reference substance solution.Precision measures above-mentioned contrast solution and each 2ml of inner mark solution, sets 10ml measuring bottles
In, add ethyl acetate to be diluted to scale, shake up, as standard solution.(i.e. 1 μ l, 16 μ g containing anethole;Containing 10 μ g of naphthalene).Take 1 μ l
Gas chromatograph is injected, continuous sample introduction 6 times calculates correction factor by average peak area.
2.2.7 sample measures
By operation preparation correction factor and sample solution under " correction factor measures and the preparation of test solution " item, then
It is accurate respectively to draw 1 μ l continuous sample introductions of correction factor solution 3 times, measure correction factor;Precision draws 1 μ l of test solution, into
Sample measures 2 times, and the percentage composition (g/g) of anethole in sample is calculated with internal standard method.
Test result see the table below.
1 oil of badian test result of table
The frequency that can be seen that ultrasound from above-mentioned experimental result is less than 600w, and broken wall is incomplete, the oil of badian of extraction
Amount it is few;Supersonic frequency higher than 1000w can improve sporoderm-broken rate but no apparent advantage, cannot be energy saving, save
Production cost;It is removed in comparative example 4 and octagonal branch, leaf is subjected to multigelation before carrying out ultrasonication, reduce eight
The sporoderm-broken rate of hornbeam branches and leaves cell, thus greatly reduces the recovery rate of oil of badian.
It, cannot the above content is specific/preferred embodiment further description made for the present invention is combined
Assert that the specific implementation of the present invention is confined to these explanations.General technical staff of the technical field of the invention is come
It says, without departing from the inventive concept of the premise, some replacements or modification can also be made to the embodiment that these have been described,
And these are substituted or variant all shall be regarded as belonging to protection scope of the present invention.
Claims (8)
1. a kind of method combining extraction oil of badian with distillation using ultrasonication, which is characterized in that include the following steps:
S1:Fresh octagonal branch, leaf are won, multigelation is carried out to octagonal branch;
S2:Octagonal leaf is cut into filiform, water is added the leaf not cut through, impregnates 1-3h, solid-liquid ratio 1:15-1:40,600-
Ultrasonication 1-3h is carried out under the frequency of 1000w;
S3:The branches and leaves filtering that broken wall is crossed, filtrate are distilled, are removed water to get oil of badian.
2. the method for combining extraction oil of badian with distillation using ultrasonication as described in claim 1, which is characterized in that
The processing method includes the following steps:
S1:Fresh octagonal branch, leaf are won, multigelation is carried out to octagonal branch;
S2:Octagonal leaf is cut into filiform, water is added the leaf not cut through, impregnates 1-3h, solid-liquid ratio 1:23-1:32,700-
Ultrasonication 1.5-2.5h is carried out under the frequency of 900w;
S3:The branches and leaves filtering that broken wall is crossed, filtrate are distilled, are removed water to get oil of badian.
3. the method for combining extraction oil of badian with distillation using ultrasonication as claimed in claim 1 or 2, feature exist
In:Branches and leaves described in step S1 are branch, the leaf for the Chinese anise picked the 3-5 months, a diameter of 0.01-0.1cm of the branch.
4. the method for combining extraction oil of badian with distillation using ultrasonication as claimed in claim 1 or 2, feature exist
In:Ultrasonication described in step S2 carries out under the conditions of 0-6 DEG C.
5. the method for combining extraction oil of badian with distillation using ultrasonication as claimed in claim 1 or 2, feature exist
In:The ultrasonication time is 2h.
6. the method for combining extraction oil of badian with distillation using ultrasonication as described in claim 1, it is characterised in that:
The chopping is that leaf is cut into the filiform of 0.5-1.5mm.
7. the method for combining extraction oil of badian with distillation using ultrasonication as described in claim 1, it is characterised in that:
The temperature of the distillation is 50-70 DEG C, time 3-4h.
8. the method for combining extraction oil of badian with distillation using ultrasonication as claimed in claim 1 or 2, feature exist
In:The water removal needs that 0.5-1h is stirred, dried using anhydrous sodium sulfate, and the dosage of the anhydrous sodium sulfate is feed liquid
The 10-15% of gross weight.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517146A (en) * | 2011-12-22 | 2012-06-27 | 江南大学 | Auxiliary method for extracting algal oil by surfactant in water phase |
| CN105802738A (en) * | 2016-06-06 | 2016-07-27 | 重庆大学 | Extraction method of Flos chrysanthemi indici volatile oil |
-
2018
- 2018-07-12 CN CN201810766145.0A patent/CN108690726A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517146A (en) * | 2011-12-22 | 2012-06-27 | 江南大学 | Auxiliary method for extracting algal oil by surfactant in water phase |
| CN105802738A (en) * | 2016-06-06 | 2016-07-27 | 重庆大学 | Extraction method of Flos chrysanthemi indici volatile oil |
Non-Patent Citations (2)
| Title |
|---|
| 刘文山等: "《中国食植物产品加工》", 31 January 2002, 中国城市出版社 * |
| 陈驹声: "《林产化工与产品》", 30 June 1993, 化学工业出版社 * |
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