CN107746091A - A kind of method for reducing camphor content in borneol water - Google Patents
A kind of method for reducing camphor content in borneol water Download PDFInfo
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- CN107746091A CN107746091A CN201711083647.5A CN201711083647A CN107746091A CN 107746091 A CN107746091 A CN 107746091A CN 201711083647 A CN201711083647 A CN 201711083647A CN 107746091 A CN107746091 A CN 107746091A
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- borneol
- water
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- camphor
- reducing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of method for reducing camphor content in borneol water, the described method comprises the following steps：(1) post separation filler is filled into post, then by borneol sample waterborne；(2) the borneol water that borneol aqueous effluent is reduced camphor content is collected, the present invention is safe, camphor content substantially reduces in borneol water after being handled by this method, unhappiness, there is irritating smell to significantly reduce so that borneol water has broader practice prospect and higher application value.
Description
Technical field
The invention belongs to Separation of Natural Products field, is related to a kind of method for reducing camphor content in borneol water.
Background technology
The method that natural borneol (d-Bomeol) is extracted from borneol camphor tree, more using steam distillation-cooling crystallization method, analysis
Aqueous after crystalline substance is also up to more than 21 kinds of composition containing a small amount of borneol etc..Aqueous (hereinafter referred to as " borneol water ") after crystallization,
Due to containing a small amount of camphor and containing some unhappy or penetrating odors, limiting the application of borneol water to a certain degree.Steam
Substantial amounts of borneol water after evaporating, it is impossible to reasonably utilized, cause the waste of resource.
The basic research to borneol water does not almost have at present, and CN101422416B has also simply expanded borneol water and led in daily use chemicals
The base application in domain.Camphor has certain side effect to human central nervous system, and FDA has very strict limitation to it.
The structure of camphor and natural borneol (d-Bomeol, hereinafter referred to as borneol) is closely similar, and the two only has a function
The difference of group, the former functional group is carbonyl, and the latter functional group is hydroxyl.From functional group's polarity, the two polarity is that natural borneol is big
In camphor.Camphor solubility 0.12g/100mL (25 DEG C) in water, natural borneol in water do not dissolve (be less than 0.1g/100mL,
18℃).According to " similar to mix " principle, under aqueous systems environment, from solubility angle, the two polarity is that camphor is more than natural ice
Piece.The reason for causing above contradiction is probably that camphor in aqueous, exists with a kind of more complicated structure, and natural borneol
More it is present in relatively simple structure (such as free state, ionic state) in the aqueous solution.
Due to the difference of the existence of camphor, borneol under water environment, therefore consider do not adding any chemical composition
On the premise of, using some safe high polymer materials or special space structural material, to reach separating natural borneol
It is the method for needing to research and develop at present with the purpose of camphor.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of side for reducing camphor content in borneol water
Method.
To reach this goal of the invention, the present invention uses following technical scheme：
The present invention provides a kind of method for reducing camphor content in borneol water, the described method comprises the following steps：
(1) post separation filler is filled into post, then by borneol sample waterborne；
(2) the borneol water that borneol aqueous effluent is reduced camphor content is collected.
In the present invention, the materials such as borneol, camphor are mainly contained in borneol water.The polarity of camphor and borneol is poor in borneol water
Different and functional group has differences.When camphor and borneol are in aqueous systems, camphor exists with a kind of increasingly complex structure, and imperial
The structure of brain is relatively simple, due to such architectural difference, using the method in above-mentioned steps of the present invention, can effectively reduce dragon
The content of camphor in brain water, reaches preferable separating effect.Also, the content of borneol is without obvious in the borneol water after separation
Change, unhappy, penetrating odor significantly reduce, and this causes the application value of borneol water further to improve.
Preferably, post separation filler described in step (1) is non-polar macroporous resin or acidulous cation resin.
In the present invention, non-polar macroporous resin or acidic cationic resin are safe, for camphor in borneol water and
The separation of natural borneol has very good effect.
Preferably, the non-polar macroporous resin is that Diaion HP21, Diaion HP20 or Amberlite XAD-4 appoint
Meaning is a kind of.
Preferably, the acidulous cation resin is resin D113.
Preferably, also include adjusting column equilibration after dress post in step (1).
Preferably, the regulation column equilibration is that water soaks and rinses post separation filler.
Preferably, counter-cylinder product 1mL post separation filler, the volume that borneol water described in step (1) loads for 7~
16mL, such as can be 7mL, 9mL, 12mL, 14mL or 16mL.
In the present invention, post separation filler with borneol water by setting specific volume ratio, imitate by the separation to reach optimal
Fruit.
Preferably, the flow velocity of step (2) the borneol water is 1.5~2.5 times of column volumes, such as can be 1.5 per hour
Again, 1.7 times, 1.9 times, 2.2 times, 2.4 times or 2.5 times.
Preferably, methods described also includes post cleaning.
Preferably, the post cleaning is to be eluted adsorbed camphor using eluant, eluent.
In the present invention, also include eluting a small amount of borneol with other impurities when post cleans, while eluting camphor,
Including 1,8- Cineoles, linalool, 4- terpinenols and first position terpinol.
Preferably, the eluant, eluent is sodium chloride or ethanol.
Preferably, the concentration of the sodium chloride is 4~8%, such as can be 4%, 5%, 6%, 7% or 8%.
Preferably, the concentration of the ethanol be 85~90%, such as can be 85%, 86%, 87%, 88%, 89% or
90%.
Preferably, the flow velocity of the sodium chloride and ethanol is 2 times of column volumes per hour.
Relative to prior art, the invention has the advantages that：
The method that camphor content in borneol water is reduced by the present invention, the content of camphor can be effectively reduced, by borneol water
Middle camphor separates with natural borneol, and holistic approach is safe, unhappy in borneol water, notable with irritating smell
Reduce so that borneol water has broader practice prospect and higher application value.
Brief description of the drawings
Fig. 1 is the gas chromatogram of borneol water stoste in the present invention.
Fig. 2 is the borneol water gas chromatogram of embodiment 1 after purification.
Fig. 3 is the borneol water gas chromatogram of embodiment 2 after purification.
Fig. 4 is the mass spectrogram of the camphor detected in the present invention in embodiment 1.
Fig. 5 is the mass spectrogram of the d-Bomeol detected in the present invention in embodiment 1.
Embodiment
Technical scheme is further illustrated below by embodiment.Those skilled in the art should be bright
, the embodiment be only to aid in understand the present invention, be not construed as to the present invention concrete restriction.
Embodiment 1
The present embodiment reduces the content of camphor in borneol water by the following method：
40mL acidulous cation resin D113 are taken, pillar is balanced with appropriate purified water, rinses resin.Then by borneol water
320mL loadings.2 times of column volumes of flow velocity per hour, collect loading efflux, and carry out GC detections；Terminate to collect loading efflux,
80mL 5% sodium chloride solution is taken, 2 times of column volumes of flow velocity carry out post cleaning per hour.After end, balanced with appropriate purified water,
Preparation separates next time.
Embodiment 2
The present embodiment reduces the content of camphor in borneol water by the following method：
40mL resin Diaion HP21 are taken, pillar is balanced with appropriate purified water, rinses resin.Then by borneol water 640mL
Loading.2.5 times of column volumes of flow velocity per hour, collect loading efflux, and carry out GC detections；Terminate to collect loading efflux, take
40mL 90% ethanol solution, 2 times of column volumes of flow velocity carry out post cleaning per hour.After end, balanced, prepared with appropriate purified water
Separate next time.
Embodiment 3
The present embodiment reduces the content of camphor in borneol water by the following method：
40mL resin Diaion HP20 are taken, pillar is balanced with appropriate purified water, rinses resin.Then by borneol water 280mL
Loading.1.5 times of column volumes of flow velocity per hour, collect loading efflux, and carry out GC detections；Terminate to collect loading efflux, take
80mL 90% ethanol solution, 2 times of column volumes of flow velocity carry out post cleaning per hour.After end, balanced, prepared with appropriate purified water
Separate next time.
Comparative example 1
1g sephadex lh-20s, with purified water complete swelling, the gel after swelling is then added to 150mL borneol
In water.Conical flask is rocked every 10min once, after 60min, takes solution GC to test and analyze.
Comparative example 2
15mL borneol water is taken, is separated with Millipore ultra-filtration centrifuge tubes.Molecular cut off 3K, rotating speed 12000r/min, from
Heart 15min, obtain centrifugal permeation liquid, sampling GC detection and analysis.
Above example 1-3 and comparative example 1-2 uses same batch borneol water, and the solution after separation is carried out into GC detections
Analysis.
GC assay methods are as follows：
Agilent 7820A gas chromatographs, Agilent 19091J-413:1HP-5 5%Phenyl methyl
Siloxan 30m*320um*0.25um capillary columns, heating schedule (70 DEG C of initial temperature, with 5 DEG C/min heating rate, rise
To 220 DEG C, and keep 5min).
Measurement result such as table 1 below：
Table 1
In terms of above table data, the d-Bomeol area ratio highest of embodiment 1.Area ratio is higher, purification efficiency
Better.From the point of view of the yield and area ratio of comprehensive d-Bomeol, the separating effect of embodiment 1 is ideal.Relative to other points
It is also ideal using acidulous cation resin separation method from method, and it can be concluded that is separated using resin
Method, the method that separating effect is also better than sephadex and Millipore ultrafiltration centrifugation.
By embodiment 1 and borneol water stoste, GC-MS detections are carried out, analyze the relative amount change of ingredient.Measure knot
Fruit such as table 2 below：
Table 2
| Borneol water stoste (%) | Embodiment 1 (%) | |
| 1.8- Cineole | 2.04 | 0.10 |
| Camphor | 4.54 | 1.54 |
| Linalool | 0.61 | 0.19 |
| 4- terpinenols | 0.75 | 0.29 |
| First position terpinol | 1.89 | 1.28 |
| Borneol | 19.84 | 17.05 |
As can be seen from the above table, borneol/camphor ratio is increased to 11.07 camphors and borneol to a certain degree from the 4.37 of stoste
The upper purifying that is separated.Content the biggest drop of 1, 8-Cineole, camphor, compared to stoste, 95%, 75% is reduced respectively, is caused
The change of fragrance.
Applicant states that the present invention illustrates that a kind of of the present invention reduces camphor content in borneol water by above-described embodiment
Method, but the invention is not limited in above-mentioned processing step, that is, do not mean that the present invention has to rely on above-mentioned processing step
It can implement.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to raw material selected by the present invention
The addition of equivalence replacement and auxiliary element, selection of concrete mode etc., all fall within protection scope of the present invention and open scope it
It is interior.
Claims (10)
- A kind of 1. method for reducing camphor content in borneol water, it is characterised in that the described method comprises the following steps：(1) post separation filler is filled into post, then by borneol sample waterborne；(2) the borneol water that borneol aqueous effluent is reduced camphor content is collected.
- 2. the method according to claim 1 for reducing camphor content in borneol water, it is characterised in that described in step (1) Post separation filler is non-polar macroporous resin or acidulous cation resin.
- 3. the method according to claim 2 for reducing camphor content in borneol water, it is characterised in that described nonpolar macroporous Resin is any one in Diaion HP21, Diaion HP20 or Amberlite XAD-4；Preferably, the acidulous cation resin is resin D113.
- 4. the method for reducing camphor content in borneol water according to claim any one of 1-3, it is characterised in that step (1) also include adjusting column equilibration after dress post in；Preferably, the regulation column equilibration is that water soaks and rinses post separation filler.
- 5. the method for reducing camphor content in borneol water according to claim any one of 1-4, it is characterised in that with respect to post Volume 1mL post separation filler, the volume that borneol water described in step (1) loads is 7~16mL.
- 6. the method for reducing camphor content in borneol water according to claim any one of 1-5, it is characterised in that step (2) flow velocity of the borneol water is 1.5~2.5 times of column volumes per hour.
- 7. the method for reducing camphor content in borneol water according to claim any one of 1-6, it is characterised in that the side Method also includes post and cleaned.
- 8. the method according to claim 7 for reducing camphor content in borneol water, it is characterised in that the post cleaning is to make Adsorbed camphor is eluted with eluant, eluent.
- 9. the method according to claim 8 for reducing camphor content in borneol water, it is characterised in that the eluant, eluent is chlorine Change sodium or ethanol；Preferably, the concentration of the sodium chloride is 4~8%；Preferably, the concentration of the ethanol is 85~90%.
- 10. the method according to claim 9 for reducing camphor content in borneol water, it is characterised in that the eluant, eluent Flow velocity is 2 times of column volumes per hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711083647.5A CN107746091B (en) | 2017-11-07 | 2017-11-07 | Method for reducing camphor content in borneol water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711083647.5A CN107746091B (en) | 2017-11-07 | 2017-11-07 | Method for reducing camphor content in borneol water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107746091A true CN107746091A (en) | 2018-03-02 |
| CN107746091B CN107746091B (en) | 2020-04-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711083647.5A Active CN107746091B (en) | 2017-11-07 | 2017-11-07 | Method for reducing camphor content in borneol water |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020153245A1 (en) * | 2001-02-14 | 2002-10-24 | Henuset Yves Michel | Flow-through eletrochemical reactor for wastewater treatment |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN103755527A (en) * | 2014-02-01 | 2014-04-30 | 闻永举 | Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract |
| CN205759871U (en) * | 2016-05-31 | 2016-12-07 | 浙江云涛生物技术股份有限公司 | A kind of left-handed resin tower with d-camphorsulfonic acid of the most quickly recovery |
-
2017
- 2017-11-07 CN CN201711083647.5A patent/CN107746091B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020153245A1 (en) * | 2001-02-14 | 2002-10-24 | Henuset Yves Michel | Flow-through eletrochemical reactor for wastewater treatment |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN103755527A (en) * | 2014-02-01 | 2014-04-30 | 闻永举 | Method for preparing high-purity borneol from lauraceae extract or blumea balsamifera extract |
| CN205759871U (en) * | 2016-05-31 | 2016-12-07 | 浙江云涛生物技术股份有限公司 | A kind of left-handed resin tower with d-camphorsulfonic acid of the most quickly recovery |
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| CN107746091B (en) | 2020-04-17 |
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