CN106349028B - A method of extracting elemicin from pepper - Google Patents
A method of extracting elemicin from pepper Download PDFInfo
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- CN106349028B CN106349028B CN201610628810.0A CN201610628810A CN106349028B CN 106349028 B CN106349028 B CN 106349028B CN 201610628810 A CN201610628810 A CN 201610628810A CN 106349028 B CN106349028 B CN 106349028B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
The present invention is suitable for phytochemicals production preparation technical field, provides a kind of method that elemicin is extracted from pepper, the method is using pepper leaf as raw material, including processing step: pepper leaf being crushed, is first freezed, hot-water soak is then carried out；Extraction step: filtering takes filtered pepper leaf to carry out EtOH Sonicate extraction, obtains extract liquor；Elemicin obtaining step: filtering the extract liquor, and filtrate is taken to distill 1-2h at a temperature of 95-105 DEG C.A kind of method for extracting elemicin from pepper provided by the present invention destroys the cell wall of blade and cell membrane effectively, is conducive to the extraction of elemicin in subsequent extraction step before extraction first to pepper leaf by the way of first freezing and steeping hot water again.It after pepper leaf is handled, is handled using EtOH Sonicate extraction+distillation, has efficiently extracted the elemicin in pepper leaf, and recovery rate is high.
Description
Technical field
The invention belongs to phytochemicals production preparation technical field more particularly to a kind of sides that elemicin is extracted from pepper
Method.
Background technique
Elemicin, chemical formula are 5- allyl -1,2, and 3- trimethoxy-benzene is Novel anesthetic, and structural formula is as follows:
Although containing this kind of ingredient in many plants, because content is less is difficult to extract, and impurity is more and abandon.For
This, has researcher to attempt to carry out compound experiment to elemicin using chemically synthesized method, but in chemically synthesized method
Also containing benezene other impurities are had unavoidably, have larger danger to human body.
Pepper is a kind of plant that southern region of China is largely planted, at present people using it is more be pepper fruit,
And cauline leaf does not have further processing to use substantially.Correlative study shows to contain a certain amount of elemicin in pepper.If one can be studied
The method that kind can extract elemicin from pepper, not only increases the utility value of pepper, also provides one for the acquisition of elemicin
The completely new channel of kind.However, there is no such method in the art at present.
Summary of the invention
In order to solve the above technical problems, the method that the present invention provides a kind of to extract elemicin from pepper, it is intended to be olive
The acquisition of fragrant element provides a kind of new approach, while improving the resource utilization of pepper leaf.
The invention is realized in this way a method of elemicin is extracted from pepper, the method is original with pepper leaf
Material, comprising:
Processing step: pepper leaf being crushed, is first freezed, and then carries out hot-water soak；
Extraction step: filtering takes filtered pepper leaf to carry out EtOH Sonicate extraction, obtains extract liquor；
Elemicin obtaining step: filtering the extract liquor, and filtrate is taken to distill 1-2h at a temperature of 95-105 DEG C.
Compared with prior art, the present invention beneficial effect is: one kind provided by the present invention extracts elemi from pepper
The method of element obtains the cell wall of blade and cell membrane before extraction first to pepper leaf by the way of first freezing and steeping hot water again
It is destroyed to effective, is conducive to the extraction of elemicin in subsequent extraction step.After pepper leaf is handled, extracted using EtOH Sonicate
+ distillation processing is taken, has efficiently extracted the elemicin in pepper leaf, and recovery rate is high.
Detailed description of the invention
Fig. 1 is the flow diagram for the extraction step that the embodiment of the present invention 1 provides.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The method that the present invention provides a kind of from pepper extracts elemicin, the method using pepper leaf as raw material, including
Following steps:
Processing step: pepper leaf being crushed, is first freezed, and then carries out hot-water soak；
Extraction step: filtering takes filtered pepper leaf to carry out EtOH Sonicate extraction, obtains extract liquor；And
Elemicin obtaining step: filtering the extract liquor, and filtrate is taken to distill 1-2h at a temperature of 95-105 DEG C.
The present invention is in processing step, to pepper leaf by the way of first freezing and steeping hot water again, make blade cell wall and
Cell membrane is effectively destroyed, and the extraction of elemicin in extraction step is conducive to.
Specifically, the EtOH Sonicate extraction process are as follows:
Filtered pepper leaf is divided into first part, second part and third part by quality, every part carries out ethyl alcohol three times and surpasses
Sound extraction；
The EtOH Sonicate extraction process three times of first portion of pepper leaf are as follows:
First part of pepper leaf be soaked in in the ethyl alcohol for be three times in its quality progress first time ultrasonic extraction, filtering obtains the
Solid matter and first time extract liquor；
First time solid matter is soaked in the ethyl alcohol of its twice quality and carries out second of ultrasonic extraction, filters, obtains
Second of solid matter and second of extract liquor；
Second of solid matter is soaked in progress third time ultrasonic extraction in the ethyl alcohol of its twice quality, filtering obtains
Pepper leaf waste residue and third time extract liquor.
Specifically, the EtOH Sonicate extraction process three times of second portion of pepper leaf are as follows:
Second part of pepper leaf is soaked in progress first time ultrasonic extraction in the first time extract liquor, filtering obtains second
Part first time solid matter and second part of first time extract liquor；
Second part of first time solid matter is soaked in second of extract liquor and carries out second of ultrasonic extraction,
Filtering, obtains second part of second of solid matter and second part of second of extract liquor；
Second part of second of solid matter is soaked in progress third time ultrasonic extraction, mistake in the third time extract liquor
Filter, obtains pepper leaf waste residue and second part of third time extract liquor.
Specifically, the EtOH Sonicate extraction process three times of third part pepper leaf are as follows:
Third part pepper leaf is soaked in progress first time ultrasonic extraction in second part of first time extract liquor, is filtered,
Obtain third part first time solid matter and third part first time extract liquor；
Third part first time solid matter is soaked in described second part of second of extract liquor and surpass for the second time
Sound extraction, filtering obtain second of extract liquor of second of solid matter of third part and third part；
Second of solid matter of third part is soaked in second part of third time extract liquor and carries out third time ultrasound extraction
It takes, filters, obtain pepper leaf waste residue and third part third time extract liquor；
Merge third part first time extract liquor, second of extract liquor of third part, third part third time extract liquor, as
The extract liquor.
Specifically, extract liquor standing 48h can be subjected to subsequent filtration step.
Specifically, the frequency of the first time ultrasonic extraction is 0.05-0.5MHz (megahertz), time 0.5h；Described
The frequency of twice ultrasonic extraction is 6-15MHz, time 1-2h；The frequency of the third time ultrasonic extraction is 30-50MHz, when
Between be 1-2h.The first time of described second part and third part, second, the frequency of third time ultrasonic extraction and time are with first
Part is corresponding identical.
In extraction step, the extract liquor three times of first part of pepper leaf is respectively used to second portion of pepper of extraction by the present invention
Leaf is then used to third part.Relative motion using dynamic countercurrent extraction method+ultrasonication, between etoh solvent and pepper leaf
Make boundary layer updating decision between etoh solvent and material pepper leaf, the yield and extraction efficiency of effective component are all improved, such as adopt
With non-dynamic adverse current extraction method+non-ultrasonic extraction, at least want 10kg autumn old-age group pepper blade that could extract the olive of 10g or so
Fragrant element, and pass through extracting process of the invention, 3kg autumn old-age group pepper blade can extract the elemicin of 10g or more.
Specifically, the smashed diameter of pepper leaf is 1-5mm, preferably 2-3mm.
Specifically, the temperature of the freezing is 3 DEG C hereinafter, the time is 0.5-2h；It is preferred that -5 DEG C -0 DEG C of cryogenic temperature, the time
1-1.5h.The temperature of the hot-water soak is 70-100 DEG C, time 0.5-5h；80-90 DEG C of preferable temperature, time 0.5-2h.
Specifically, the elemicin obtaining step further includes addition ODS silica gel in the filtrate described in the forward direction of the distillation
(octadecylsilane chemically bonded silica).It is eluted after distillation with alcohol-water, elemicin is obtained after concentrate drying.The present invention also uses ODS
Silica gel column purification, the elemicin of available high-purity, silica gel are also recycling.
Preferably, the pepper leaf is autumn old-age group pepper blade, and aged pepper blade includes falling off from the upper nature of tree
Blade.Hydrolysis occurs for protein in aged pepper leaf, chlorophyll is lost, these variations promote ethyl alcohol to the elemi in pepper leaf
The extraction of element.
A kind of method for extracting elemicin from pepper provided by the invention, according to the molecular structure of elemicin from pepper
It is extracted in cauline leaf, easy to operate, device therefor is less, can be used for extracting elemicin in batches.Extracting method of the invention is suitable
In large-scale production, and yield is big, high production efficiency and energy saving.
Technical solution of the present invention is illustrated below in conjunction with specific embodiment.
Embodiment 1
A method of extracting elemicin from pepper, steps are as follows:
Processing step: selecting autumn old-age group pepper blade 3kg, pepper leaf crushed, and then freezes 2 hours for 2 DEG C；It takes
The pepper leaf crushed after freezing out, is put into the hot water tank equipped with 90 DEG C；
Extraction step: load weighted same 3 portions of peppers leaf powder is respectively put into 3 extractors of the first, second and third tank,
The ethyl alcohol of 3 times of solid weights is added into the first tank, ultrasonic wave extraction is impregnated 30 minutes, and extracting solution A1 is then set the second tank the
Primary to extract, solid slag continues to extract 1h with the EtOH Sonicate ripple of 2 times of volumes, and extracting solution A2 is placed in the second tank for mentioning for the second time
It taking, the first tank solid slag continues plus the EtOH Sonicate ripple of 2 times of volumes extracts 1h, and extracting solution A3 is placed in the second tank third time and extracts,
It finally obtains medical fluid C1, C2 and C3 to mix, stands 48h, then filter and extract liquor (referring to attached drawing 1) is made.
Elemicin obtaining step: filtering to obtain extract liquor, the stirring of ODS silica gel is added in extract liquor, distillation, then volatilization is dry
Ethyl alcohol and other impurities, then eluted with alcohol-water, it is concentrated and dried the elemicin purified, weighing its quality is 12g.
Embodiment 2
A method of extracting elemicin from pepper, steps are as follows:
Processing step: autumn old-age group pepper blade 3kg is selected, pepper leaf is crushed, then -5 DEG C of freezing 1-2 are small
When；The pepper leaf crushed after freezing is taken out, is put into the hot water tank equipped with 70-90 DEG C；
Extraction step: load weighted same 3 portions of peppers leaf powder is respectively put into 3 extractors of the first, second and third tank,
The ethyl alcohol of 3 times of solid weights is added into the first tank, ultrasonic wave extraction is impregnated 30 minutes, and extracting solution A1 is then set the second tank the
Primary to extract, solid slag continues to extract 1.5h with the EtOH Sonicate ripple of 2 times of volumes, and extracting solution A2 is placed in the second tank and is used for second
It extracts, the first tank solid slag continues plus the EtOH Sonicate ripple of 2 times of volumes extracts 1.5h, and extracting solution A3 is placed in the second tank third time and mentions
It takes, finally obtains medical fluid C1, C2 and C3 and mix, stand 48h, then filter and extract liquor (referring to attached drawing 1) is made.
Elemicin obtaining step: filtering to obtain extract liquor, the stirring of ODS silica gel is added in extract liquor, distillation, then volatilization is dry
Ethyl alcohol and other impurities, then eluted with alcohol-water, it is concentrated and dried the elemicin purified, weighing its quality is 15g.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of method for extracting elemicin from pepper, which is characterized in that the method is using pepper leaf as raw material, comprising:
Processing step: pepper leaf being crushed, is first freezed, and then carries out hot-water soak；
Extraction step: filtering takes filtered pepper leaf to carry out EtOH Sonicate extraction, obtains extract liquor；
Elemicin obtaining step: filtering the extract liquor, and filtrate is taken to distill 1-2h at a temperature of 95-105 DEG C；By filtered Hu
Green pepper leaf is divided into first part, second part and third part by quality, and every part carries out EtOH Sonicate three times and extracts；The first time ultrasound
The frequency of extraction is 0.05-0.5MHz, time 0.5h；The frequency of second of ultrasonic extraction is 6-15MHz, time 1-
2h；The frequency of the third time ultrasonic extraction is 30-50MHz, time 1-2h.
2. the method as described in claim 1, which is characterized in that the EtOH Sonicate extraction process are as follows:
The EtOH Sonicate extraction process three times of first portion of pepper leaf are as follows:
First part of pepper leaf is soaked in progress first time ultrasonic extraction in the ethyl alcohol of three times quality, filtering obtains first time solid
Substance and first time extract liquor；
First time solid matter is soaked in the ethyl alcohol of twice of mass and carries out second of ultrasonic extraction, is filtered, obtains second admittedly
Body substance and second of extract liquor；
Second of solid matter is soaked in progress third time ultrasonic extraction in the ethyl alcohol of twice of mass, it is useless to obtain pepper leaf for filtering
Slag and third time extract liquor.
3. method according to claim 2, which is characterized in that the EtOH Sonicate extraction process three times of second portion of pepper leaf
Are as follows:
Second part of pepper leaf is soaked in the first time extract liquor progress first time ultrasonic extraction, filtering obtains second part the
Solid matter and second part of first time extract liquor；
Second part of first time solid matter is soaked in second of extract liquor and carries out second of ultrasonic extraction, mistake
Filter, obtains second part of second of solid matter and second part of second of extract liquor；
Second part of second of solid matter is soaked in progress third time ultrasonic extraction in the third time extract liquor, filtering obtains
Pepper leaf waste residue and second part of third time extract liquor.
4. method as claimed in claim 3, which is characterized in that the EtOH Sonicate extraction process three times of third part pepper leaf
Are as follows:
Third part pepper leaf is soaked in second part of first time extract liquor progress first time ultrasonic extraction, filtering obtains the
Three parts of first time solid matters and third part first time extract liquor；
Third part first time solid matter is soaked in described second part of second of extract liquor and carries out second of ultrasound extraction
It takes, filters, obtain second of extract liquor of second of solid matter of third part and third part；
Second of solid matter of third part is soaked in progress third time ultrasonic extraction, mistake in second part of third time extract liquor
Filter, obtains pepper leaf waste residue and third part third time extract liquor；
Merge third part first time extract liquor, second of extract liquor of third part, third part third time extract liquor, it is as described
Extract liquor.
5. the method as described in claim 1, which is characterized in that the smashed diameter of pepper leaf is 1-5mm.
6. the method as described in claim 1, which is characterized in that the temperature of the freezing is 3 DEG C hereinafter, the time is 0.5-2h.
7. the method as described in claim 1, which is characterized in that the temperature of the hot-water soak is 70-100 DEG C, and the time is
0.5-5h。
8. the method as described in claim 1, which is characterized in that the elemicin obtaining step further includes before the distillation
ODS silica gel is added into the filtrate.
9. the method as described in claim 1, which is characterized in that the pepper leaf is autumn old-age group pepper blade.
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| CN201610628810.0A CN106349028B (en) | 2016-08-03 | 2016-08-03 | A method of extracting elemicin from pepper |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101352258A (en) * | 2008-09-04 | 2009-01-28 | 河南中烟工业公司 | Ligusticum sinense extract liquid and use thereof in tobacco |
| CN104706688A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院上海生命科学研究院湖州营养与健康产业创新中心 | Method for preparing effective parts of nutmeg total lignanoids |
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- 2016-08-03 CN CN201610628810.0A patent/CN106349028B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101352258A (en) * | 2008-09-04 | 2009-01-28 | 河南中烟工业公司 | Ligusticum sinense extract liquid and use thereof in tobacco |
| CN104706688A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院上海生命科学研究院湖州营养与健康产业创新中心 | Method for preparing effective parts of nutmeg total lignanoids |
Non-Patent Citations (1)
| Title |
|---|
| 许勇等.树胡椒繁殖后代叶油及成分的变化.《香料香精化妆品》.2002,(第3期),14-18. |
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