CN108689873A - A kind of process for super-critical extracting of capsaicine - Google Patents
A kind of process for super-critical extracting of capsaicine Download PDFInfo
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- CN108689873A CN108689873A CN201810257865.4A CN201810257865A CN108689873A CN 108689873 A CN108689873 A CN 108689873A CN 201810257865 A CN201810257865 A CN 201810257865A CN 108689873 A CN108689873 A CN 108689873A
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- capsaicine
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- capsicum
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Organic Chemistry (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a kind of process for super-critical extracting of capsaicine, raw material is not required to dry directly use, and energy consumption is few, and extract yield is high, and security risk is low.Using enzymatic isolation method processing treated capsicum in extraction process, clasmatosis fully uses supercritical methanol to meet environmental requirement, extraction efficiency height as extractant;Beeswax can significantly improve the extraction content of capsaicine as entrainer.
Description
Technical field
The present invention relates to a kind of extraction process, more particularly to a kind of process for super-critical extracting of capsaicine.
Background technology
Pimiento is a kind of extremely common crops, and ingredient includes capsaicine, capsicum red pigment, protein, vitamin
With the nutriments such as amino acid.Wherein capsaicin compound is also referred to as capsaicine, is the main component of capsicum pungent, has extensive
Pharmacological activity.Research shows that the capsaicine of low concentration is commonly used for flavouring or additive, it is widely used in family and food work
Industry;And the capsaicine of high concentration has an analgesia, antipruritic, anti-inflammatory, sterilization, treats enterogastritis and the effects that leukemia, also weight-reducing and
The health-care efficacies such as relaxing tendons and activating collaterals.
Extractive technique about capsaicine has many reports, and main method includes organic solvent extraction, overcritical two
Carbon oxide fluid extraction, crystallisation etc..Such as Chinese invention patent (ZL200410054008), be gone out using extract by solvents it is peppery
Green pepper essence crude product, then chilli extract crude product is put into the extraction kettle in overcritical device, open extraction cycle circuit " extraction-separation
Device-extraction " is extracted, and is controlled CO2 pressure, be can be obtained the higher capsaicine of purity, but the method to equipment investment, safety and
Operate more demanding, production cost is also higher, is unfavorable for production application;Method is disclosed in patent document (ZL94104403.3)
Capsaicine is extracted from chilli extract by method for crystallising, the method is complex for operation step, and consumption of organic solvent is big, it is difficult to which popularization is answered
With.Therefore, active development is simple and easy to do, extracting method rapidly and efficiently is to produce the capsicum alkali product of high-purity, highly-water-soluble
Seem most important.
Invention content
The purpose of the present invention is to provide a kind of simple for process, toxic organic solvents are not used, are extracted using macroreticular resin
It is a kind of isolation technics easy to operate, recovery rate is high, is suitable for industrialized production uses.
The present invention provides a kind of process for super-critical extracting of capsaicine, and step includes:
1) enzymolysis processing:The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, a certain amount of ethyl alcohol is then added,
The pectase for being equivalent to capsicum weight 0.1%~0.3% and be equivalent to capsicum weight 0.9%~1.6% half is added after stirring evenly
Cellulase, enzymolysis processing for a period of time, obtains enzymolysis mixture at 25~40 DEG C;
2) supercritical extract:The enzymolysis mixture is imported in extraction kettle, using supercritical methanol as extractant, bee
Wax is 20~40 DEG C in extraction temperature as entrainer, and Fluid pressure is 20~40MPa, under 0.10~0.40ml/min of flow velocity,
1~3h of extraction obtains extract, and extract is absorbed liquid with methanol absorption;
3) macroporous resin enrichment:By macroporous resin column adsorption and enrichment in absorbing liquid, the aperture of big pore resin is 50~
80 angstroms, specific surface area is 600~700m2/ g, liquid flow control is in 2~5mL/min;
4) it elutes:It is eluted with the methanol of 3~10BV amounts, flow control is opened in 3~8mL/min after eluent flows out 1BV
Begin to collect eluent, concentrate drying obtains capsaicine.
Preferably, the capsicum described in step 1) is fresh chilli of the moisture content 40~60%, and not necessary any
Drying process processing.The solid-liquid ratio of capsicum and ethanol solution is 1:0.5~1:2.The hemicellulase is that can be planted constituting
The general name of the various enzymes of polysaccharide (except cellulose and pectin substance) hydrolyzable of object cell membrane;Pectase is from head mold
Extraction, so that intercellular pectic substance is degraded, cell is separated out of tissue.
In step 2), concrete operations are as follows:Overcritical device is enabled, supercritical methanol is with the flow of 20L/h through filter
Extractor is squeezed by compressor after filtering, until reach 20~40MPa of pressure of setting, extraction temperature by extractor chuck cycle
Water management is simultaneously stablized at 20~40 DEG C.
The extract separation process is:After supercritical methanol fluid extraction liquid reaches knockout drum decompression, with extract point
From the supercritical methanol fluid is used into the compressor cycle, and by extract methanol absorption, be absorbed liquid.
In step 3), the macroreticular resin is the macroreticular resins such as AB-8, NKA, X-5, NKA-9, S-8, and before the use
It is pre-processed.
Advantages of the present invention is as follows:
Using enzymatic isolation method processing treated capsicum in extraction process, clasmatosis is abundant, ensure that extraction efficiency;Using
Supercritical methanol meets environmental requirement as extractant, and extraction efficiency is high;Beeswax can significantly improve capsaicine as entrainer
Extraction content.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
[Embodiment 1]
1) enzymolysis processing:The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, a certain amount of ethyl alcohol is then added,
Addition is equivalent to the pectase of capsicum weight 0.1% and is equivalent to the hemicellulase of capsicum weight 0.9% after stirring evenly, at 40 DEG C
Enzymolysis processing for a period of time, obtains enzymolysis mixture;
2) supercritical extract:The enzymolysis mixture is imported in extraction kettle, enables overcritical device, supercritical methanol with
The flow of 20L/h by compressor squeezes into extractor after being filtered, until reach the pressure 35MPa of setting, extraction temperature by
The cycle water management of extractor chuck is simultaneously stablized at 35 DEG C, while importing beeswax as entrainer, is 35 DEG C in extraction temperature, stream
Body pressure is 35MPa, and under flow velocity 0.3ml/min, extraction 3h obtains extract, and extraction with supercritical methanol liquid reaches knockout drum decompression
Afterwards, it is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption obtains
Absorbing liquid.
3) macroporous resin enrichment:By AB-8 macroporous resin columns adsorption and enrichment in absorbing liquid, the aperture of big pore resin is
50 angstroms, specific surface area 600m2/ g, liquid flow control is in 5mL/min;
4) it elutes:It is eluted with the methanol of 5BV amounts, flow control is in 8mL/min, after eluent flows out 1BV, starts to collect and wash
De- liquid, concentrate drying obtain capsaicine.
[Embodiment 2]
1) enzymolysis processing:The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, a certain amount of ethyl alcohol is then added,
Addition is equivalent to the pectase of capsicum weight 0.3% and is equivalent to the hemicellulase of capsicum weight 1.2% after stirring evenly, at 35 DEG C
Enzymolysis processing for a period of time, obtains enzymolysis mixture;
2) supercritical extract:The enzymolysis mixture is imported in extraction kettle, enables overcritical device, supercritical methanol with
The flow of 20L/h by compressor squeezes into extractor after being filtered, until reach the pressure 25MPa of setting, extraction temperature by
The cycle water management of extractor chuck is simultaneously stablized at 40 DEG C, while importing beeswax as entrainer, is 40 DEG C in extraction temperature, stream
Body pressure is 25MPa, and under flow velocity 0.4ml/min, extraction 2h obtains extract liquor, and extraction with supercritical methanol liquid reaches knockout drum decompression
Afterwards, it is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption obtains
Absorbing liquid.
3) macroporous resin enrichment:By NKA-9 macroporous resin columns adsorption and enrichment in absorbing liquid, the aperture of big pore resin is
50 angstroms, specific surface area 600m2/ g, liquid flow control is in 5mL/min;
4) it elutes:It is eluted with the methanol of 5BV amounts, flow control is in 8mL/min, after eluent flows out 1BV, starts to collect and wash
De- liquid, concentrate drying obtain capsaicine.
[Embodiment 3]
1) enzymolysis processing:The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, a certain amount of ethyl alcohol is then added,
Addition is equivalent to the pectase of capsicum weight 0.2% and is equivalent to the hemicellulase of capsicum weight 1.5% after stirring evenly, at 25 DEG C
Enzymolysis processing for a period of time, obtains enzymolysis mixture;
2) supercritical extract:The enzymolysis mixture is imported in extraction kettle, enables overcritical device, supercritical methanol with
The flow of 20L/h by compressor squeezes into extractor after being filtered, until reach the pressure 20MPa of setting, extraction temperature by
The cycle water management of extractor chuck is simultaneously stablized at 40 DEG C, while importing beeswax as entrainer, is 40 DEG C in extraction temperature, stream
Body pressure is 20MPa, and under flow velocity 0.2ml/min, extraction 3h obtains extract liquor, and extraction with supercritical methanol liquid reaches knockout drum decompression
Afterwards, it is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption obtains
Absorbing liquid.
3) macroporous resin enrichment:Aperture by S-8 macroporous resin columns adsorption and enrichment in absorbing liquid, big pore resin is 50
Angstrom, specific surface area 600m2/ g, liquid flow control is in 5mL/min;
4) it elutes:It is eluted with the methanol of 5BV amounts, flow control is in 8mL/min, after eluent flows out 1BV, starts to collect and wash
De- liquid, concentrate drying obtain capsaicine.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (6)
1. a kind of process for super-critical extracting of capsaicine, its step are as follows:
1) enzymolysis processing:The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, a certain amount of ethyl alcohol is then added, stirs evenly
It is added afterwards and is equivalent to the pectase of capsicum weight 0.1%~0.3% and is equivalent to the hemicellulose of capsicum weight 0.9%~1.6%
Plain enzyme, enzymolysis processing for a period of time, obtains enzymolysis mixture at 25~40 DEG C;
2) supercritical extract:The enzymolysis mixture is imported in extraction kettle, using supercritical methanol as extractant, beeswax is made
It is 20~40 DEG C in extraction temperature for entrainer, Fluid pressure is 20~40MPa, under 0.10~0.40ml/min of flow velocity, extraction
1~3h obtains extract, and extract is absorbed liquid with methanol absorption;
3) macroporous resin enrichment:Aperture by macroporous resin column adsorption and enrichment in absorbing liquid, big pore resin is 50~80 angstroms,
Specific surface area is 600~700m2/ g, liquid flow control is in 2~5mL/min;
4) it elutes:It is eluted with the methanol of 3~10BV amounts, flow control starts to receive in 3~8mL/min after eluent flows out 1BV
Collect eluent, concentrate drying obtains capsaicine.
2. the process for super-critical extracting of capsaicine according to claim 1, the capsicum is moisture content 40~60%
Fresh chilli, and not necessary any drying process processing.
3. the process for super-critical extracting of capsaicine according to claim 1, in the step 1), capsicum and ethanol solution
Solid-liquid ratio is 1:0.5~1:2.
4. the process for super-critical extracting of capsaicine according to claim 1, in the step 2), the extract detached
Cheng Wei:After extraction with supercritical methanol liquid reaches knockout drum decompression, detached with extract, the supercritical methanol enters compressor and follows
Ring uses, and by extract methanol absorption, be absorbed liquid.
5. the process for super-critical extracting of capsaicine according to claim 1, in step 3), the macroreticular resin be AB-8,
The macroreticular resins such as NKA, X-5, NKA-9, S-8, and pre-processed before the use.
6. further include according to the process for super-critical extracting of Claims 1 to 5 any one of them capsaicine, in the step 2) as
Lower step, enables overcritical device, and supercritical methanol by compressor squeezes into extraction after being filtered with the flow of 20L/h
Tank, until reaching 20~40MPa of pressure of setting, extraction temperature is by the cycle water management and stabilization of extractor chuck 20~40
℃。
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| CN201810257865.4A CN108689873A (en) | 2018-03-27 | 2018-03-27 | A kind of process for super-critical extracting of capsaicine |
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| CN201810257865.4A CN108689873A (en) | 2018-03-27 | 2018-03-27 | A kind of process for super-critical extracting of capsaicine |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587321A (en) * | 2004-08-26 | 2005-03-02 | 上海交通大学 | Process for separating capsorubin and capsaicine from hot pepper |
| CN103739511A (en) * | 2013-12-20 | 2014-04-23 | 白城艾高食品有限公司 | Method for extracting capsaicin |
| CN104529805A (en) * | 2014-11-27 | 2015-04-22 | 安徽省万顺现代农业科技有限公司 | Method for extracting capsicine from capsicum |
| CN107661361A (en) * | 2017-11-17 | 2018-02-06 | 浙江工业大学上虞研究院有限公司 | A kind of process for super-critical extracting of ginko leaves flavone class compound |
-
2018
- 2018-03-27 CN CN201810257865.4A patent/CN108689873A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587321A (en) * | 2004-08-26 | 2005-03-02 | 上海交通大学 | Process for separating capsorubin and capsaicine from hot pepper |
| CN103739511A (en) * | 2013-12-20 | 2014-04-23 | 白城艾高食品有限公司 | Method for extracting capsaicin |
| CN104529805A (en) * | 2014-11-27 | 2015-04-22 | 安徽省万顺现代农业科技有限公司 | Method for extracting capsicine from capsicum |
| CN107661361A (en) * | 2017-11-17 | 2018-02-06 | 浙江工业大学上虞研究院有限公司 | A kind of process for super-critical extracting of ginko leaves flavone class compound |
Non-Patent Citations (2)
| Title |
|---|
| 吴梁森: "超临界乙醇萃取洗油中联苯的工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 李进军，等: "《绿色化学导论》", 31 August 2015, 武汉大学出版社 * |
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