CN105505225A - Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin - Google Patents
Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin Download PDFInfo
- Publication number
- CN105505225A CN105505225A CN201511006345.9A CN201511006345A CN105505225A CN 105505225 A CN105505225 A CN 105505225A CN 201511006345 A CN201511006345 A CN 201511006345A CN 105505225 A CN105505225 A CN 105505225A
- Authority
- CN
- China
- Prior art keywords
- capsaicin
- pigment
- content
- oleoresin capsicum
- refining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/02—Purification
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
Abstract
The invention discloses a method for separating capsaicin and pigment in capsicum oleoresin with a high capsaicin content and refining the capsaicin. The method comprises the following steps that (1) the capsicum oleoresin is added to a stirring pot, a solvent A and a solvent B are added respectively, the mixture is stirred fully and uniformly, and a centrifugal machine is enabled to perform liquid-liquid-solid separation by the aid of different solubility of two phases in the pigment and the capsaicin and the density difference of the two phases, so that the purpose of initial separation of the pigment and the capsaicin is realized, the capsaicin content is improved, and insoluble substances and impurities are removed; (2) the pigment and the capsaicin obtained in the step (1) are filtered respectively, the insoluble substances are further removed, the capsaicin content is improved further, and the two phases are concentrated respectively to obtain the capsicum oleoresin and capsanthin; (3) a chromatographic column is added to the capsicum oleoresin obtained in the step (2), capsaicin is absorbed and eluted, the pigment is removed, an eluant is collected, and the capsicum oleoresin with the low color value and the high capsaicin content is obtained through concentration. The method is good in separation effect, free of discharge of three wastes and environment-friendly.
Description
Technical field
The present invention relates to natural product extraction separation field, being specifically separated and method that Capsaicin is refining of Capsaicin and pigment in a kind of high Capsaicin content oleoresin capsicum.
Background technology
The application of current capsaicine widely, can as food pungent additive, medicine aspect is used for anti-inflammatory analgesic, the blood fat that reduces blood pressure, fat-reducing, detonation suppressor can be made in army and police aspect, agricultural aspect can as biological pesticide, expelling parasite desinsection, industrial aspect is the raw material making Gopher-protected wire cable.Extract from capsicum at present after obtaining thick product oleoresin capsicum, Capsaicin always is a difficult problem in the industry with being separated of pigment, and prior art is separated complete not, and still have pigment residue in oleoresin capsicum, complicated operation, yield is on the low side, and cost is higher.For formulation application widely, be badly in need of a kind of oleoresin capsicum of low look valency height Capsaicin content, for various preparation is supplied raw materials, but there is no good Capsaicin and pigment separated technical scheme at present, also do not reach the Capsaicin purification scheme of level of the present invention.
Summary of the invention
The object of the present invention is to provide being separated and method that Capsaicin is refining, to solve the problem proposed in above-mentioned background technology of Capsaicin and pigment in a kind of high Capsaicin content oleoresin capsicum.
For achieving the above object, the invention provides following technical scheme:
Being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum, comprises the following steps:
(1) oleoresin capsicum is added in stirred pot, add solvent orange 2 A and solvent B respectively, stir, utilize two relative pigments and the different solubilities of Capsaicin and the density difference of two-phase, whizzer is used to carry out liquid-liquid-solid separation, thus reach the object of pigment and Capsaicin initial gross separation, improve the content of Capsaicin, remove insolubles and impurity;
(2) pigment phase step (1) obtained and Capsaicin filter mutually respectively, and remove insolubles further, Capsaicin content is further enhanced, and concentrated two-phase obtains oleoresin capsicum and capsanthin respectively;
(3) oleoresin capsicum that step (2) obtains is added chromatography column, absorb-elute Capsaicin, removes pigment, collects elutriant, the concentrated oleoresin capsicum obtaining low look valency height Capsaicin content.
As the further scheme of the present invention: in described high Capsaicin oleoresin capsicum, Capsaicin content is greater than 20%.
As the present invention's further scheme: described solvent orange 2 A is the one in sherwood oil, ether, hexanaphthene, normal hexane, ethyl acetate.
As the present invention's further scheme: described solvent B is the one in methyl alcohol, ethanol, ethylene glycol, Virahol, propyl carbinol, pure water, buck.
As the present invention's further scheme: the material ratio of described solvent orange 2 A is 1:1-1:5, the material ratio of solvent B is 1:1-1:5, and the stirring velocity of solvent orange 2 A and solvent B and material is 20-150r/min, and temperature is 20-70 DEG C.
As the present invention's further scheme: described whizzer is the one in tubular-bowl centrifuge, horizontal screw centrifuge, cup type whizzer, disk centrifugal separator and wet cyclone, and centrifugal speed is 1000-50000r/min.
As the present invention's further scheme: the mode of filtering in step (2) is: the one in the filtration of bag type filtering, filter screen filtration, core, membrane sepn and natural subsidence.
As the present invention's further scheme: the filler of chromatography column described in step (3) is the one in silica gel, gel, aluminum oxide, ion exchange resin, macroporous adsorbent resin, diatomite and gac.
As the present invention's further scheme: described in step (3), chromatography column applied sample amount is the 2%-20% of column volume, filler is the 40%-80% of column volume.
As the present invention's further scheme: the eluent that chromatography column is used in step (3) first use in methyl alcohol, ethanol, ethylene glycol, Virahol one or several, use in sherwood oil, normal hexane, acetone, ethyl acetate, pure water afterwards one or several, the usage quantity of eluent is 1-100 times of column volume, and thickening temperature is 50-100 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: the present invention adopt double solvent extraction separation, good separating effect, eliminate impurity and insolubles.Eliminate impurity and insolubles further by filtering, product Capsaicin content is improved, column chromatography for separation effectively can remove the residual pigment in oleoresin capsicum, and then obtains the oleoresin capsicum of low look valency height Capsaicin content.The all energy recycles of whole process solvent, three-waste free discharge, protection of the environment is the production technique of clean and effective.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
By Capsaicin content 22.3%, the oleoresin capsicum 300Kg of look valency 25.2 joins in stirred pot, then adds the normal hexane of 600L and the ethanol of 600L, and 60r/min stirs 30min; Being transported in disk centrifugal separator by mixing solution completely, centrifugal speed 6000r/min, being separated and obtaining two liquid phases and impurity solid phase, remove impurity and insolubles, heavy phase is concentrated obtains oleoresin capsicum 112.44Kg, Capsaicin content 59.32%, look valency 2.1, the Capsaicin rate of recovery 99.7%; Light concentrating mutually obtains capsanthin 186.39Kg, look valency 38.9, pigment recovery rate 95.9%; By oleoresin capsicum dissolve with ethanol obtained above, then remove solid insoluble and impurity further with filtration; By remove solid insoluble and impurity oleoresin capsicum on chromatography column, adsorb 4 hours, with ethanol elution, collect ethanol eluate, the concentrated oleoresin capsicum 87.72Kg obtaining low look valency height Capsaicin content, Capsaicin content 76.3%, look valency 0.3, the Capsaicin rate of recovery 99.2%.
Embodiment 2
By Capsaicin content 25.1%, the oleoresin capsicum 350Kg of look valency 27.2 joins in stirred pot, then adds the sherwood oil of 700L and the methyl alcohol of 700L, and 60r/min stirs 30min; Be transported in disk centrifugal separator by mixing solution completely, centrifugal speed 6000r/min, separating liquid two-phase and solid, remove impurity and insolubles, heavy phase is concentrated obtains oleoresin capsicum 145.25Kg, Capsaicin content 60.12%, look valency 2.6, the Capsaicin rate of recovery 99.4%; Light concentrating mutually obtains pigment 203.21Kg, look valency 45.1, pigment recovery rate 96.3%; By oleoresin capsicum dissolve with ethanol obtained above, then remove solid insoluble and impurity further with filtration; By remove solid insoluble and impurity oleoresin capsicum on chromatography column, adsorb 4 hours, adsorb with ethanolysis, collect ethanol eluate, the concentrated oleoresin capsicum 117.78Kg obtaining low look valency height Capsaicin, Capsaicin content 73.7%, look valency 0.4, the Capsaicin rate of recovery 99.4%.
The present invention is the separating effect improving Capsaicin and pigment in crude product oleoresin capsicum, refines further, obtain the oleoresin capsicum of low look valency height Capsaicin content to Capsaicin, for relevant preparation is supplied raw materials.The present invention adopt double solvent extraction separation, good separating effect, eliminate impurity and insolubles.Eliminate impurity and insolubles further by filtering, product Capsaicin content is improved, column chromatography for separation effectively can remove the residual pigment in oleoresin capsicum, and then obtains the oleoresin capsicum of low look valency height Capsaicin content.The all energy recycles of whole process solvent, three-waste free discharge, protection of the environment is the production technique of clean and effective.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum, is characterized in that, comprise the following steps:
(1) oleoresin capsicum is added in stirred pot, add solvent orange 2 A and solvent B respectively, stir, utilize two relative pigments and the different solubilities of Capsaicin and the density difference of two-phase, whizzer is used to carry out liquid-liquid-solid separation, thus reach the object of pigment and Capsaicin initial gross separation, improve the content of Capsaicin, remove insolubles and impurity;
(2) pigment phase step (1) obtained and Capsaicin filter mutually respectively, and remove insolubles further, Capsaicin content is further enhanced, and concentrated two-phase obtains oleoresin capsicum and capsanthin respectively;
(3) oleoresin capsicum that step (2) obtains is added chromatography column, absorb-elute Capsaicin, removes pigment, collects elutriant, the concentrated oleoresin capsicum obtaining low look valency height Capsaicin content.
2. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, in described high Capsaicin oleoresin capsicum, Capsaicin content is greater than 20%.
3. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, described solvent orange 2 A is the one in sherwood oil, ether, hexanaphthene, normal hexane, ethyl acetate.
4. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, described solvent B is the one in methyl alcohol, ethanol, ethylene glycol, Virahol, propyl carbinol, pure water, buck.
5. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, the material ratio of described solvent orange 2 A is 1:1-1:5, the material ratio of solvent B is 1:1-1:5, the stirring velocity of solvent orange 2 A and solvent B and material is 20-150r/min, and temperature is 20-70 DEG C.
6. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, described whizzer is the one in tubular-bowl centrifuge, horizontal screw centrifuge, cup type whizzer, disk centrifugal separator and wet cyclone, and centrifugal speed is 1000-50000r/min.
7. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, the mode of filtering in step (2) is: the one in the filtration of bag type filtering, filter screen filtration, core, membrane sepn and natural subsidence.
8. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, the filler of chromatography column described in step (3) is the one in silica gel, gel, aluminum oxide, ion exchange resin, macroporous adsorbent resin, diatomite and gac.
9. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, described in step (3), chromatography column applied sample amount is the 2%-20% of column volume, and filler is the 40%-80% of column volume.
10. being separated and method that Capsaicin is refining of Capsaicin and pigment in high Capsaicin content oleoresin capsicum according to claim 1, it is characterized in that, the eluent that chromatography column is used in step (3) first use in methyl alcohol, ethanol, ethylene glycol, Virahol one or several, use in sherwood oil, normal hexane, acetone, ethyl acetate, pure water afterwards one or several, the usage quantity of eluent is 1-100 times of column volume, and thickening temperature is 50-100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511006345.9A CN105505225A (en) | 2015-12-29 | 2015-12-29 | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511006345.9A CN105505225A (en) | 2015-12-29 | 2015-12-29 | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105505225A true CN105505225A (en) | 2016-04-20 |
Family
ID=55713540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511006345.9A Pending CN105505225A (en) | 2015-12-29 | 2015-12-29 | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105505225A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106752072A (en) * | 2016-12-05 | 2017-05-31 | 晨光生物科技集团股份有限公司 | A kind of High color values capsanthin continuous production processes |
| CN107523090A (en) * | 2017-06-29 | 2017-12-29 | 河北邯兆生物科技有限公司 | A kind of method for improving, improving capsicum red pigment absorption ratio |
| CN107903826A (en) * | 2017-11-23 | 2018-04-13 | 青岛赛特香料有限公司 | A kind of method of purifying crude capsicum oleoresin |
| CN109180517A (en) * | 2018-10-11 | 2019-01-11 | 许昌学院 | A method of preparing high pure white solid capsaicine |
| CN110713733A (en) * | 2019-10-29 | 2020-01-21 | 四川常青调正食品有限责任公司 | Process for separating capsanthin from hot pepper |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724511A (en) * | 2005-07-08 | 2006-01-25 | 上海雷辣婆食品有限公司 | Method of extracting capsaicin and capsaithin from red pepper |
| CN101940289A (en) * | 2010-08-06 | 2011-01-12 | 杨红梅 | Method for separating discolored chili extract from chili pigment in crude products of chili extract |
| CN102746793A (en) * | 2012-07-31 | 2012-10-24 | 云南宏绿辣素有限公司 | Method for refining capsicum oleoresins |
-
2015
- 2015-12-29 CN CN201511006345.9A patent/CN105505225A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724511A (en) * | 2005-07-08 | 2006-01-25 | 上海雷辣婆食品有限公司 | Method of extracting capsaicin and capsaithin from red pepper |
| CN101940289A (en) * | 2010-08-06 | 2011-01-12 | 杨红梅 | Method for separating discolored chili extract from chili pigment in crude products of chili extract |
| CN102746793A (en) * | 2012-07-31 | 2012-10-24 | 云南宏绿辣素有限公司 | Method for refining capsicum oleoresins |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106752072A (en) * | 2016-12-05 | 2017-05-31 | 晨光生物科技集团股份有限公司 | A kind of High color values capsanthin continuous production processes |
| CN106752072B (en) * | 2016-12-05 | 2019-03-19 | 晨光生物科技集团股份有限公司 | A kind of High color values capsanthin continuous production processes |
| CN107523090A (en) * | 2017-06-29 | 2017-12-29 | 河北邯兆生物科技有限公司 | A kind of method for improving, improving capsicum red pigment absorption ratio |
| CN107903826A (en) * | 2017-11-23 | 2018-04-13 | 青岛赛特香料有限公司 | A kind of method of purifying crude capsicum oleoresin |
| CN109180517A (en) * | 2018-10-11 | 2019-01-11 | 许昌学院 | A method of preparing high pure white solid capsaicine |
| CN110713733A (en) * | 2019-10-29 | 2020-01-21 | 四川常青调正食品有限责任公司 | Process for separating capsanthin from hot pepper |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105505225A (en) | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin | |
| CN103073915A (en) | Process for extracting and separating capsanthin and capsaicin by using biological enzyme | |
| CN104741094B (en) | Composite resin containing polyamide resin and preparation method thereof | |
| CN107778277B (en) | Process for the recovery of squalene, vitamin E and/or sterols | |
| CN101721979B (en) | Method for preparing macroporous adsorbent resin special for separating valine | |
| CN111039914A (en) | Extraction and separation method of cannabinol | |
| CN105566142A (en) | Process for extracting chili with high capsaicin content | |
| CN108017530B (en) | Method for continuously separating coenzyme Q10 from mushroom dregs | |
| CN104974068A (en) | Ajoene preparation method | |
| CN102675108B (en) | Refining method of pyrethrin crude extract | |
| CN107118242A (en) | Preparation method of amygdalin | |
| CN102079883B (en) | Novel process for extracting capsanthin and chilli extract by composite solvent | |
| CN109651301A (en) | A kind of purification process of orlistat | |
| CN104072510A (en) | Method for extracting hamaudol from Phlojodicarpus sibiricus | |
| CN104448904A (en) | Method for extracting capsanthin and chili extract through compound solvent | |
| CN103012384B (en) | Method for extracting silymarin from silybum marianum | |
| KR101227156B1 (en) | Manufacturing method of xanthorrhizol having oral antibacterial | |
| CN111138400A (en) | Extraction and separation method of cannabichromene | |
| CN108299459B (en) | Method for extracting artemisinin by using polyethylene glycol solvent | |
| CN101974014B (en) | Manufacturing technology for extracting ginkalide A and C from root and bark of maidenhair tree | |
| CN104961765B (en) | A kind of preparation method of the phosphatide with phosphatidyl-ethanolamine as principal component | |
| CN102617699A (en) | Process for preparing nomilin monomer by industrial chromatography | |
| CN102973618B (en) | Method for extracting valerenic acid from valeriana fauriei | |
| CN102993247A (en) | Method for separating anthraquinone ingredient of semen cassiae by low-pressure and medium-pressure preparative column | |
| CN102091127B (en) | New technology for extracting Chinese magnoliavine fruit lignanoid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160420 |