CN108341751A - A kind of extraction process of capsaicine - Google Patents
A kind of extraction process of capsaicine Download PDFInfo
- Publication number
- CN108341751A CN108341751A CN201810365122.9A CN201810365122A CN108341751A CN 108341751 A CN108341751 A CN 108341751A CN 201810365122 A CN201810365122 A CN 201810365122A CN 108341751 A CN108341751 A CN 108341751A
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- China
- Prior art keywords
- extraction
- capsaicine
- capsicum
- extract
- methanol
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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
-
- 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
Abstract
The present invention relates to a kind of extraction process 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, meets environmental requirement as extractant using supercritical methanol, extraction efficiency is high；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 extraction process 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 extraction process of capsaicine, and step includes：
1) it pre-processes：The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, dried after cleaning, deepfreeze 10~
20h, refrigerated storage temperature are -10~-40 DEG C；Capsicum after refrigeration is sent into for the lye of 9-9.5 in high pressure abrasive kettle with pH value
Grinding obtains capsicum slurry；
2) supercritical extract：The capsicum is starched and 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：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 lye is aqueous solution any in sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate；Grinding
Rate is 8000~9000r/min, and grinding temperature is 60~80 DEG C, and pressure is 10~15Mpa, and milling time is 1~3h.
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) it pre-processes：The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, dried after cleaning, deepfreeze 20h,
Refrigerated storage temperature is -10 DEG C；The potassium hydroxide solution that capsicum after refrigeration is 9 with pH value is sent into high pressure abrasive kettle and is ground, is obtained
It is starched to capsicum, grinding rate 8000r/min, grinding temperature is 80 DEG C, pressure 15Mpa, milling time 1h；
2) supercritical extract：The capsicum is starched and is imported in extraction kettle, enables overcritical device, supercritical methanol is with 20L/
The flow of h by compressor squeezes into extractor after being filtered, until reaching the pressure 35MPa of setting, extraction temperature is by extracting
The cycle water management of tank chuck is simultaneously stablized at 35 DEG C, while importing beeswax as entrainer, is 35 DEG C in extraction temperature, fluid pressure
Power is 35MPa, and under flow velocity 0.3ml/min, extraction 3h obtains extract, after extraction with supercritical methanol liquid reaches knockout drum decompression,
It is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption is absorbed
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) it pre-processes：The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, dried after cleaning, deepfreeze 10h,
Refrigerated storage temperature is -40 DEG C, and the sodium hydroxide solution that the capsicum after refrigeration is 9.5 with pH value is sent into high pressure abrasive kettle and is ground
Mill, obtains capsicum slurry, grinding rate 8500r/min, and grinding temperature is 75 DEG C, pressure 2Mpa, milling time 2h；
2) supercritical extract：The capsicum is starched and is imported in extraction kettle, enables overcritical device, supercritical methanol is with 20L/
The flow of h by compressor squeezes into extractor after being filtered, until reaching the pressure 25MPa of setting, extraction temperature is by extracting
The cycle water management of tank chuck is simultaneously stablized at 40 DEG C, while importing beeswax as entrainer, is 40 DEG C in extraction temperature, fluid pressure
Power is 25MPa, and under flow velocity 0.4ml/min, extraction 2h obtains extract liquor, after extraction with supercritical methanol liquid reaches knockout drum decompression,
It is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption is absorbed
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) it pre-processes：The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, dried after cleaning, deepfreeze 15h,
Refrigerated storage temperature is -25 DEG C；The sodium carbonate liquor that capsicum after refrigeration is 9 with pH value is sent into high pressure abrasive kettle and is ground, is obtained
It is starched to capsicum, grinding rate 8000r/min, grinding temperature is 80 DEG C, pressure 15Mpa, milling time 1h；
2) supercritical extract：The capsicum is starched and is imported in extraction kettle, enables overcritical device, supercritical methanol is with 20L/
The flow of h by compressor squeezes into extractor after being filtered, until reaching the pressure 20MPa of setting, extraction temperature is by extracting
The cycle water management of tank chuck is simultaneously stablized at 40 DEG C, while importing beeswax as entrainer, is 40 DEG C in extraction temperature, fluid pressure
Power is 20MPa, and under flow velocity 0.2ml/min, extraction 3h obtains extract liquor, after extraction with supercritical methanol liquid reaches knockout drum decompression,
It is detached with extract, the supercritical methanol is used into the compressor cycle, and extract methanol absorption is absorbed
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 extraction process of capsaicine, its step are as follows：
1) it pre-processes：The impurity inside capsicum is removed into capsicum remove seed, stalk, sorting, dried after cleaning, 10~20h of deepfreeze,
Refrigerated storage temperature is -10~-40 DEG C；Capsicum after refrigeration is sent into for the lye of 9-9.5 in high pressure abrasive kettle with pH value and is ground,
Obtain capsicum slurry；
2) supercritical extract：The capsicum is starched and is imported in extraction kettle, using supercritical methanol as extractant, beeswax is as folder
Band agent is 20~40 DEG C in extraction temperature, and 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 extraction process of capsaicine according to claim 1, the capsicum be moisture content 40~60% it is fresh peppery
Green pepper, and not necessary any drying process processing.
3. the extraction process of capsaicine according to claim 1, in the step 1), the lye is sodium hydroxide, hydrogen
Any aqueous solution in potassium oxide, sodium carbonate or potassium carbonate；Grinding rate is 8000~9000r/min, grinding temperature 60
~80 DEG C, pressure is 10~15Mpa, and milling time is 1~3h.
4. the extraction process of capsaicine according to claim 1, in the step 2), the extract separation process is：
After extraction with supercritical methanol liquid reaches knockout drum decompression, detached with extract, the supercritical methanol enters compressor cycle and makes
With by extract methanol absorption, be absorbed liquid.
5. the extraction process of capsaicine according to claim 1, in step 3), the macroreticular resin is AB-8, NKA, X-
5, the macroreticular resins such as NKA-9, S-8, and pre-processed before the use.
6. further including walking as follows according to the extraction process of Claims 1 to 5 any one of them capsaicine, in the step 2)
Suddenly, overcritical device is enabled, supercritical methanol squeezes into extractor after being filtered with the flow of 20L/h by compressor, until
Reach 20~40MPa of pressure of setting, extraction temperature is by the cycle water management and stabilization of extractor chuck at 20~40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810365122.9A CN108341751A (en) | 2018-04-18 | 2018-04-18 | A kind of extraction process of capsaicine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810365122.9A CN108341751A (en) | 2018-04-18 | 2018-04-18 | A kind of extraction process of capsaicine |
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| CN108341751A true CN108341751A (en) | 2018-07-31 |
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| CN201810365122.9A Pending CN108341751A (en) | 2018-04-18 | 2018-04-18 | A kind of extraction process of capsaicine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110663926A (en) * | 2019-10-29 | 2020-01-10 | 四川常青调正食品有限责任公司 | Preparation method and application of capsicum particles |
| CN111187177A (en) * | 2020-01-03 | 2020-05-22 | 海山都(上海)生物技术有限公司 | Method for preparing high-purity natural capsaicin monomer |
Citations (5)
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| CN103254092A (en) * | 2013-05-19 | 2013-08-21 | 常州亚当生物技术有限公司 | Production process of capsaicin |
| CN103739511A (en) * | 2013-12-20 | 2014-04-23 | 白城艾高食品有限公司 | Method for extracting capsaicin |
| CN104529806A (en) * | 2014-12-25 | 2015-04-22 | 晨光生物科技集团股份有限公司 | Method for preparing high-purity capsaicin |
| CN107118121A (en) * | 2017-05-31 | 2017-09-01 | 江苏师范大学 | A kind of method of capsaicine pre-treatment |
| CN107573255A (en) * | 2017-09-14 | 2018-01-12 | 中山大学 | A kind of method that capsaicine and dihydrocapsaicin are isolated and purified from pepper fruit |
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2018
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| CN103254092A (en) * | 2013-05-19 | 2013-08-21 | 常州亚当生物技术有限公司 | Production process of capsaicin |
| CN103739511A (en) * | 2013-12-20 | 2014-04-23 | 白城艾高食品有限公司 | Method for extracting capsaicin |
| CN104529806A (en) * | 2014-12-25 | 2015-04-22 | 晨光生物科技集团股份有限公司 | Method for preparing high-purity capsaicin |
| CN107118121A (en) * | 2017-05-31 | 2017-09-01 | 江苏师范大学 | A kind of method of capsaicine pre-treatment |
| CN107573255A (en) * | 2017-09-14 | 2018-01-12 | 中山大学 | A kind of method that capsaicine and dihydrocapsaicin are isolated and purified from pepper fruit |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110663926A (en) * | 2019-10-29 | 2020-01-10 | 四川常青调正食品有限责任公司 | Preparation method and application of capsicum particles |
| CN111187177A (en) * | 2020-01-03 | 2020-05-22 | 海山都(上海)生物技术有限公司 | Method for preparing high-purity natural capsaicin monomer |
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