CN109880694A - A kind of soxhlet type method of borneol essential oil - Google Patents
A kind of soxhlet type method of borneol essential oil Download PDFInfo
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- CN109880694A CN109880694A CN201910283296.5A CN201910283296A CN109880694A CN 109880694 A CN109880694 A CN 109880694A CN 201910283296 A CN201910283296 A CN 201910283296A CN 109880694 A CN109880694 A CN 109880694A
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Abstract
The application provides a kind of soxhlet type method of borneol essential oil, belongs to from raw materials recovery or purification essential oil technical field.Borneol camphortree leaf is taken, is dried；In agitating ball mill, dry borneol camphortree leaf mechanical activation is obtained into powder；Powder is mixed with organic solvent by solid-liquid ratio, heating carries out Soxhlet extraction, obtains borneol essential oil crude product；Borneol essential oil crude product is concentrated in a vacuum, obtains finished product borneol essential oil.The application is applied to extraction of essential oil, has many advantages, such as that extraction efficiency is high, specific aim and accuracy are significant, higher polar compound can be extracted and extract the ingredient of macromolecule.
Description
Technical field
This application involves a kind of soxhlet type method of borneol essential oil, belong to from raw materials recovery or purification essence oil tech neck
Domain.
Background technique
Natural borneol original name kapur, also known as d-Bomeol are to be permitted as natural rare Chinese medicine medicinal material and food additives
Indispensable good adjuvant in more borneol products.The history that natural borneol is used as drug in China is more than 1500.Study table
Bright, borneol is proven to have anti-inflammatory, antithrombotic and excellent antioxidation.
Borneol essential oil is suitble to prepare flavouring essence for tobacco, medical essence, cosmetics and a variety of drugs, and borneol essential oil value is high, uses
Way is wide, and borneol development prospect is wide.However in recent years, few about the research report for extracting borneol essential oil.Borneol essential oil mentions
Taking most-often used is traditional steam distillation, and traditional steam distillation is that borneol is put into alembic directly to distill, and is steamed
The mixed vapour evaporated obtains oil water mixture by condensation, and borneol essential oil can be obtained in oil water mixture essential oil water-oil separating again.
The problems such as that there are recovery rates is low for this method, time-consuming, energy consumption is high, product purity is low.
Summary of the invention
In view of this, the application provides, a kind of extraction efficiency is high, specific aim and accuracy are significant, it is higher to extract
Polar compound and extract macromolecule ingredient borneol essential oil soxhlet type method.
To achieve the above object, the technical solution that the application takes is as follows:
A kind of soxhlet type method of borneol essential oil, comprising the following steps: (1) take borneol camphortree leaf, dry；(2) it is stirring
It mixes in ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) by solid-liquid ratio by powder with it is organic
Solvent is mixed, and heating carries out Soxhlet extraction, obtains borneol essential oil crude product；(4) borneol essential oil crude product is concentrated in a vacuum,
Obtain finished product borneol essential oil.
In extraction scheme provided by this programme, cooperation Soxhlet extraction is ground with mechanical activation and realizes obtaining for borneol essential oil
, in the pretreatment process of mechanical activation, mechanical force destroys plant cell wall, and refines particle, and cooperation Soxhlet mentions
It takes, the ingredient of higher polar compound and macromolecule is extracted in material, and the recovery rate of borneol essential oil can reach
0.45%, the accuracy and specific aim highly significant of extraction.
On the basis of the studies above, we study drying, the results showed that when be dried to moisture content be 8-
When 12%, on the basis of being suitable for drying cost, the water content in raw material not only can be effectively reduced, cooperate with mechanical lapping, have
Effect improves the efficiency pulverized.
On the basis of the studies above, we study mechanical activation, and have been determined that more preferred stirring is ground
Grinding machine parameter: the revolving speed 90-130r/min of agitating ball mill, the time of mechanical activation are 3-7min.Under the grinding condition,
Before borneol essential oil is extracted in distillation, mechanical activation processing is first passed through after borneol camphortree leaf is dried, mechanical activation is by borneol camphor tree
Leaf destroys the cell wall of plant under the mechanical forces such as friction, collision, impact, shearing, and refines particle, so that borneol
Essential oil in camphor tree is more easier to extract, to improve the recovery rate of essential oil.
On the basis of the studies above, we also study the solid-liquid ratio in Soxhlet extraction, and have determined more excellent
The Soxhlet extraction solid-liquid ratio of choosing: the organic solvent of the Soxhlet extraction is petroleum ether, and solid-liquid ratio (raw material powder: organic solvent) is
1:1-1:13.Research is found: when solid-liquid ratio is 1:1, the recovery rate (at this time be about 0.385%) of essential oil although relatively low, but still
So it is higher than the essential oil yield (about 0.35-0.36%) of traditional water distillation；With the increase of solid-liquid ratio, raw material powder is organic molten
Dissolution rate in agent increases therewith, thus effective dissolution rate of purpose essential oil is incremented by therewith, and reaches this when solid-liquid ratio is 1:9
Under the conditions of peak value (about 0.46%)；Continue to increase solid-liquid ratio, then since raw material powder is limited, extraction of essential oil rate does not have bright
Aobvious to increase, therefore, solid-liquid ratio is suitable for control in 1:1-1:13, and preferably 1:7-1:11.
On the basis of carrying out the studies above, we test the temperature during Soxhlet extraction, and obtain more
Preferred Extracting temperature is 65-95 DEG C.When selecting Soxhlet extraction mode, after temperature reaches to a certain degree, extracting could be normal
It carries out, therefore in the research at initial stage, we determined that minimum Extracting temperature is 65 DEG C, essential oil yield is about 0.39- at this time
0.4%, higher than the essential oil yield (about 0.35-0.36%) of traditional water distillation；With increasing for Extracting temperature, raw material powder exists
Liveness enhancing in organic solvent, and macro manifestations are the increase of dissolution rate, thus effective dissolution rate of purpose essential oil is therewith
It is incremented by, and reaches stable when temperature is increased to 80-85 DEG C；Continue to heat up, then excessively high temperature can interfere raw material powder having
Dissolution rate in solvent, thus heat up at this time and positive effect is not constituted to essential oil yield.Therefore suitable Extracting temperature is
65-95 DEG C, and preferably 75-85 DEG C, ideal extraction effect can be obtained.
On the basis of carrying out the studies above, we test the time during Soxhlet extraction, and obtain more
Preferred extraction time is 0.5-4h.When selecting Soxhlet extraction mode, the influence of extraction time is relatively simple, i.e. essential oil yield
Extension at any time and be incremented by, and amplification is significant in 1-2h, and in 2-3h, amplification reduces and increment continues；Continue to extend and extract
Time, then amplification is no longer obvious.Therefore, comprehensive treatment effect is considered with processing cost, is suitable for selecting extraction time in 0.5-
4h, and preferably 2-3.5h.
Detailed description of the invention
Fig. 1 is influence of the solid-liquid ratio to borneol essential oil yield；
Fig. 2 is influence of the Extracting temperature to borneol essential oil yield；
Fig. 3 is influence of the extraction time to borneol essential oil yield；
Fig. 4 is the representative processes flow chart of the application.
Specific embodiment
In the extraction scheme of the essential oil provided by present application, the principal element for influencing essential oil yield is divided into: dry, machine
Three tool activation, Soxhlet extraction aspects:
A. the dry water content being mainly concerned with after drying mode and degree of drying i.e. drying.Borneol essential oil raw material mainly selects
From borneol camphortree leaf, it is contemplated that the characteristic of the characteristics such as a large amount of property of the raw material, disunity and borneol essential oil is suitable for using nature
The mode dried carries out；In terms of degree of drying, moisture content is excessively high, can be unfavorable for mechanical activation, also can band in subsequent distillation
Enter a large amount of moisture, causes essential oil entirety recovery rate relatively low.On the basis of by our lot of experiments, water content is selected
It is set to 8-12%, the water content in raw material not only can be effectively reduced, also effectively improve the efficiency pulverized.
B. mechanical activation is mainly concerned with the grinding mode and revolving speed or specific breakage rate of selection.In grinding mode side
Face, we have selected agitating ball mill, complete grinding while agitating, raw material is enable rapidly and uniformly to grind sufficiently, and
By revolving speed control in 90-130r/min, the time of mechanical activation is 3-7min, can meet grinding and adequately require.
Influence of the following case mainly with regard to surfactant and distillation is analyzed.
C. Soxhlet extraction includes three aspect of selected solid-liquid ratio, Extracting temperature and extraction time, hereafter main just above-mentioned
Factor influences the acquisition of essential oil to carry out concrete case explanation and analysis, referring specifically to embodiment 1-3.
Embodiment 1: the influence of different feed liquid comparison essential oil yield
It determines that solid-liquid ratio is not less than 1:1 using petroleum ether as organic solvent in present case, in preliminary test, can protect at this time
Demonstrate,prove essential oil yield 0.38% or more (higher than it is same under the conditions of traditional essential oil yield 0.36%).In the solid-liquid ratio range
Interior, we have selected seven nodes of 1:1,1:3,1:5,1:7,1:9,1:11 and 1:13 to carry out representative trend experiment, as a result
It is shown in Figure 1.It will be seen from figure 1 that when being tested using above-mentioned seven kinds of solid-liquid ratios, with the raising of solid-liquid ratio, essential oil
Yield increases accordingly, and essential oil yield increases significantly, and when solid-liquid ratio reaches 1:5, essential oil yield is near 0.42%；Continue
Increasing solid-liquid ratio, then amplification decreases, and reaches peak value (about 0.46%) under this condition when solid-liquid ratio is 1:9, after
Continuous to increase solid-liquid ratio, when solid-liquid ratio increases to 1:9-1:13, essential oil yield is no longer significantly increased, and it is attached to be maintained at 0.46%
Closely.
Therefore the research of dip time is carried out in following experiment with the solid-liquid ratio of 1:9.
Embodiment 2: influence of the different Extracting temperatures to essential oil yield
On the basis of embodiment 1, we carry out the Extracting temperature in Soxhlet extraction (remaining parameter is referring to embodiment 1)
Experiment, the results showed that in conjunction with Fig. 2, when Extracting temperature is arranged at 65 DEG C, the recovery rate of essential oil has reached 0.39%, is higher than
The essential oil yield 0.35-0.36% of traditional water distillation；With the rise of extracting temperature, recovery rate is almost linear therewith is incremented by；
When reaching 80 DEG C, essential oil yield reaches peak value (0.46%) under this condition；Continue to increase temperature, then it may be excessively high because of temperature
Cause solvent boiling excessively, the dissolution of purpose essential oil is hindered, and recovery rate does not have and rises appreciably, and is substantially remained in
Near 0.45-0.46%.Therefore, under comprehensive consideration, Extracting temperature is suitable for being set as 65-95 DEG C, and at preferably 75-85 DEG C,
Extraction of essential oil effect is preferable.
Embodiment 3: influence of the different extraction times to essential oil yield
In embodiment 1 and on the basis of embodiment 2, our, (remaining parameter was referring to implementation the extraction times to Soxhlet extraction
Example 1) it is tested, the results showed that in conjunction with Fig. 3, as the extraction time of raw material powder in organic solvent extends, essential oil yield
Gradually promoted, upon extracting between when reaching 3h, extraction of essential oil rate amplification reaches maximum, and extraction of essential oil rate is 0.458% at this time；After
It renews long extraction time, extraction time, amplification was no longer significant in 3-4h, and essential oil yield tends towards stability in 0.458%-0.46%
Near.Therefore, comprehensive treatment effect is considered with processing cost, and extraction time selects in 0.5-4h, and when preferably 2-3.5h, essence
Oil extract effect is preferable.
On the basis of above-mentioned experiment and analysis of cases, we are in such a way that mechanical activation grinds cooperation Soxhlet extraction to raw material
Powder is handled, and using following step as representative,
(1) borneol camphortree leaf is taken, is dried；(2) in agitating ball mill, dry borneol camphortree leaf mechanical activation is obtained into powder
End；(3) powder is added by solid-liquid ratio and organic solvent, heating extraction for a period of time, obtains borneol crude oil；(4) it is concentrated in vacuo: will
Borneol crude oil is concentrated in a vacuum, obtains finished product borneol essential oil,
In conjunction with Fig. 4 and four concrete cases (embodiment 4,5,6,7) selected, whole annotate is done to the extraction scheme of the application
It releases.
Embodiment 4
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 90r/min
7min is activated, powder is obtained；
(3) Soxhlet extraction: being that powder and organic solvent (petroleum ether is selected in present case), heating is added in 1:9 by solid-liquid ratio
To 85 DEG C of extraction 2h, borneol crude oil is obtained；
(4) it is concentrated in vacuo: obtained borneol crude oil being concentrated in a vacuum, obtains borneol essential oil, borneol extraction of essential oil rate
It is 0.41% or so.
Embodiment 5
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 100r/min
5min is activated, powder is obtained；
(3) Soxhlet extraction: being that powder and organic solvent (petroleum ether is selected in present case), heating is added in 1:9 by solid-liquid ratio
To 85 DEG C of extraction 2h, borneol crude oil is obtained；
(4) it is concentrated in vacuo: obtained borneol crude oil being concentrated in a vacuum, obtains borneol essential oil, borneol extraction of essential oil rate
It is 0.42% or so.
Embodiment 6
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 110r/min
5min is activated, powder is obtained；
(3) Soxhlet extraction: being that powder and organic solvent (petroleum ether is selected in present case), heating is added in 1:9 by solid-liquid ratio
To 85 DEG C of extraction 2h, borneol crude oil is obtained；
(4) it is concentrated in vacuo: obtained borneol crude oil being concentrated in a vacuum, obtains borneol essential oil, borneol extraction of essential oil rate
It is 0.44% or so.
Embodiment 7
(1) the borneol camphortree leaf of harvesting is dried, makes its moisture content 10%；
(2) mechanical activation: the borneol camphortree leaf dried is added in agitating ball mill, mechanical in the case where revolving speed is 130r/min
3min is activated, powder is obtained；
(3) Soxhlet extraction: being that powder and organic solvent (petroleum ether is selected in present case), heating is added in 1:9 by solid-liquid ratio
To 85 DEG C of extraction 2h, borneol crude oil is obtained；
(4) it is concentrated in vacuo: obtained borneol crude oil being concentrated in a vacuum, obtains borneol essential oil, borneol extraction of essential oil rate
It is 0.45% or so.
The above content is the preferred embodiments of combination the invention to further detailed made by provided technical solution
Describe in detail bright, and it cannot be said that the invention specific implementation is confined to these above-mentioned explanations, technology affiliated for the invention
For the those of ordinary skill in field, without departing from the concept of the premise of the invention, several simple deductions can also be made
Or replacement, it all shall be regarded as belonging to the protection scope of the invention.
Claims (9)
1. a kind of soxhlet type method of borneol essential oil, which comprises the following steps: (1) take borneol camphortree leaf, dry
It is dry；(2) in agitating ball mill, the drying borneol camphortree leaf mechanical activation of step (1) is obtained into powder；(3) pressing solid-liquid ratio will
Powder is mixed with organic solvent, and heating carries out Soxhlet extraction, obtains borneol essential oil crude product；(4) borneol essential oil crude product is existed
It is concentrated in vacuum, obtains finished product borneol essential oil.
2. a kind of soxhlet type method of borneol essential oil as described in claim 1, it is characterised in that: in step (1), be dried to
Moisture content is 8-12%.
3. a kind of soxhlet type method of borneol essential oil as described in claim 1, it is characterised in that: in step (2), stir ball
The revolving speed 90-130r/min of grinding machine, the time of mechanical activation are 3-7min.
4. a kind of soxhlet type method of borneol essential oil as described in claim 1, it is characterised in that: in step (3), the rope
The organic solvent that family name extracts is petroleum ether, solid-liquid ratio 1:1-1:13, and preferably 1:7-1:11.
5. a kind of soxhlet type method of borneol essential oil as claimed in claim 4, it is characterised in that: in the Soxhlet extraction,
Solid-liquid ratio is 1:7-1:11.
6. a kind of soxhlet type method of borneol essential oil as described in any one in claim 1-5, it is characterised in that: step (3)
In, the Extracting temperature is 65-95 DEG C.
7. a kind of soxhlet type method of borneol essential oil as claimed in claim 6, it is characterised in that: the Extracting temperature is
75-85℃。
8. a kind of soxhlet type method of borneol essential oil as described in any one in claim 1-5, it is characterised in that: step (3)
In, the extraction time is selected as 0.5-4h.
9. a kind of soxhlet type method of borneol essential oil as claimed in claim 8, it is characterised in that: the extraction time is 2-
3.5h。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123853A (en) * | 2019-06-25 | 2019-08-16 | 湖北瑞晟农业科技有限责任公司 | A kind of extraction method of borneol camphor tree leaf crab apple tablet crude extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949035A (en) * | 2016-05-09 | 2016-09-21 | 南京明宽信息咨询中心 | Method for extraction of borneol from camphorwood branches and leaves and application |
| CN108484362A (en) * | 2018-05-16 | 2018-09-04 | 江南大学 | A method of improving natural borneol recovery rate |
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- 2019-04-10 CN CN201910283296.5A patent/CN109880694A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949035A (en) * | 2016-05-09 | 2016-09-21 | 南京明宽信息咨询中心 | Method for extraction of borneol from camphorwood branches and leaves and application |
| CN108484362A (en) * | 2018-05-16 | 2018-09-04 | 江南大学 | A method of improving natural borneol recovery rate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110123853A (en) * | 2019-06-25 | 2019-08-16 | 湖北瑞晟农业科技有限责任公司 | A kind of extraction method of borneol camphor tree leaf crab apple tablet crude extract |
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Application publication date: 20190614 |