CN101161636B - Method for purifying capsicine - Google Patents
Method for purifying capsicine Download PDFInfo
- Publication number
- CN101161636B CN101161636B CN2007101852776A CN200710185277A CN101161636B CN 101161636 B CN101161636 B CN 101161636B CN 2007101852776 A CN2007101852776 A CN 2007101852776A CN 200710185277 A CN200710185277 A CN 200710185277A CN 101161636 B CN101161636 B CN 101161636B
- Authority
- CN
- China
- Prior art keywords
- capsicine
- raw material
- capsaicin
- crystallization
- purification process
- 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.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method to prepare highly purified capsaicin with crude capsaicin as the raw material, which includes the following procedures that: firstly the raw material of crudecapsaicin is added with a refining agent, heated to 50 DEG C to 80 DEG C and stirred even, wherein the refining agent is a low-molecular polyol, such as glycol, propylene glycol, or glycerin, the mass of the refining agent is 0.5-2 times of that of the raw material of capsaicin, secondly water under 50 DEG C to 90 DEG C with the mass of 10-80 times of that of the raw material of crude capsaicin is added slowly into the mixture of capsaicin and the refining agent, which is obtained in step 1, and stirring is carried out continuously at the same time to decrease the temperature until the temperature decreases to 10 DEG C to 40 DEG C, then the mixture is poured into a crystallization container, and allowed for standing for crystallization, the environmental temperature of which is 5 DEG C to25 DEG C and, thirdly, after crystallization, the crystal is filtrated, added with water for rinsing, filtrated again, and dried in vacuum to obtain the white crystal product of capsaicin. The present invention has shortened technical process, decreased categories of organic solvent to be used, low fabrication cost and capability of environmental protection.
Description
Technical field
The present invention relates to a kind of is the method for feedstock production high-purity capsaicin with the capsaicine crude product.
Background technology
The contained sharp flavor composition of capsicum is called capsicine or claims capsaicine, and the capsaicine crystals of different purity is widely used in numerous areas such as military affairs, food, medicine, agricultural.Particularly as drug use, the clinical therapeutic efficacy of the property lost neurodynia, sacroiliitis, diabetic neuralgia and psoriatic etc. after the band shape kitchen disease has been obtained abundant affirmation, but capsicine must be purified and is the due drug action of high purity product competence exertion.At present, the method that is used for purifying capsaicin mainly contains: solvent extration, molecular distillation method, ion exchange method, column chromatography and macroporous adsorbent resin method etc., though can access the capsicine product of certain purity, all used a large amount of organic solvents, operation steps is also more loaded down with trivial details.It is long to exist the process time, and the organic solvent kind of use is many and can endanger environment structure, industrial equipments is required high, and some solvent load is bigger and toxic, causes many difficulties to suitability for industrialized production, and gained capsicine purity is not high yet.
Summary of the invention:
In order to overcome the shortcoming of prior art, the invention provides a kind of purification process of capsicine, its technical process is short, and with an organic solvent kind is few, and production cost is low, environmental protection.
The present invention solves the technical scheme that its technical problem takes: comprise the following steps: 1, add finishing agent in the raw material capsaicine crude product, be heated to 50-80 ℃ and mix, described finishing agent is the low molecular polylol class, as ethylene glycol, propylene glycol or glycerol, the weight of described finishing agent is 0.5-2 times of raw material capsicine; 2, get the 10-80 water doubly of raw material capsaicine crude product weight, water temp is 50-90 ℃, when stirring, capsicine and finishing agent mixture that the 1st step was made slowly add, continue to stir and lower the temperature, stop after temperature is reduced to 10-40 ℃ stirring, pour in the crystallisation vessel, place crystallization, the crystalline envrionment temperature is 5-25 ℃; 3, after the crystallization fully, filter out xln, add the water washing xln, refilter, vacuum-drying, obtain snow-white capsaicine crystals product.
Used water is the deionized water after plastic resin treatment in the 2nd step.
Placing the crystalline time in the 2nd step is 2-5 days.
Filter the capsicine crystallization in the 3rd step with 300 order filtering nets.
Vacuum drying temperature is 5-60 ℃ in the 3rd step, and pressure is 0.08Mpa, and the time is 2-6 hour.
The present invention has following major advantage: 1, the present invention adopts a kind of finishing agent crystalline method in water, just can reach the target that increases substantially capsicine purity; 2, to have technology easy in the present invention, advantage such as with short production cycle; 3, used low, the low toxicity of finishing agent cost of the present invention does not use any organic solvent, does not have waste water, waste gas and waste sludge discharge substantially, the production technique cleaning; 4, the product purity height produced of the technology of the present invention, total alkali reaches more than 99% in the capsaicine crystals, meets the physical and chemical index requirement of 30 editions United States pharmacopoeia specifications, can be applicable in the pharmaceutical industries; 5, in the production process of the present invention, because not with an organic solvent, organic solvent-free is residual in the final capsicine product, is more suitable for using in pharmaceutical industries.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
In 1 liter of beaker, add crude product capsicine 100 grams, behind the adding 90 gram ethylene glycol, be heated to 78 ℃ and also stir, mix; The deionized water of getting 80 ℃ joins in 10 liters of stainless steel casks for 5 kilograms, slowly adds capsicine and ethylene glycol mixture in the stainless steel cask under the stirring of electric mixer; Remove 1 kilogram of ionized water again, divide and wash beaker for several times, washing lotion slowly joins in the mixed solution that is stirring; Under agitation be cooled to 30 ℃, stop agitator, stainless steel cask is put under 15-20 ℃ the envrionment temperature and carried out crystallization; Take out after 3 days, filter, add 2 kilograms of deionized water wash after-filtration again with 300 purpose filtering nets, under 25 ℃, 0.08Mpa vacuum degree condition, dry 4 hours, snow-white capsicine crystallization 81.20 grams in dry back, detect that total alkali is 99.3% in this capsicine.
Embodiment 2:
In 1 liter of beaker, add crude product capsicine 100 grams, behind the adding 90 gram propylene glycol, be heated to 70 ℃ and also stir, mix; The deionized water of getting 75 ℃ joins in 10 liters of stainless steel casks for 7 kilograms, slowly adds capsicine and propylene glycol mixture in the stainless steel cask under the stirring of electric mixer; Remove 1 kilogram of ionized water again, divide and wash beaker for several times, washing lotion slowly joins in the mixed solution that is stirring; Under agitation be cooled to 25 ℃, stop agitator, stainless steel cask is put under 5-10 ℃ the envrionment temperature and carried out crystallization; Take out after 3 days, filter, add 2 kilograms of deionized water wash after-filtration again with 300 purpose filtering nets, under 15 ℃, 0.08Mpa vacuum degree condition, dry 5 hours, snow-white capsicine crystallization 81.40 grams in dry back, detect that total alkali is 99.6% in this capsicine.
Claims (6)
1. the purification process of a capsicine, it is characterized in that: comprise the following steps: 1, in the raw material capsaicine crude product, add finishing agent, be heated to 50-80 ℃ and mix, described finishing agent is ethylene glycol, propylene glycol or glycerol, and the weight of described finishing agent is 0.5-2 times of raw material capsicine; 2, get the 10-80 water doubly of raw material capsaicine crude product weight, water temp is 50-90 ℃, when stirring, capsicine and finishing agent mixture that the 1st step was made slowly add, continue to stir and lower the temperature, stop after temperature is reduced to 10-40 ℃ stirring, pour in the crystallisation vessel, place crystallization, the crystalline envrionment temperature is 5-25 ℃; 3, after the crystallization fully, filter out xln, add the water washing xln, refilter, vacuum-drying, obtain snow-white capsaicine crystals product.
2. the purification process of capsicine according to claim 1 is characterized in that: water used in the 2nd step is the deionized water after plastic resin treatment.
3. the purification process of capsicine according to claim 1 is characterized in that: placing the crystalline time in the 2nd step is 2-5 days.
4. the purification process of capsicine according to claim 1 is characterized in that: filter the capsicine crystallization in the 3rd step with 300 order filtering nets.
5. the purification process of capsicine according to claim 1 is characterized in that: vacuum drying temperature is 5-60 ℃ in the 3rd step, and pressure is 0.08Mpa, and the time is 2-6 hour.
6. the purification process of capsicine according to claim 5, it is characterized in that: vacuum drying temperature is 15-25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101852776A CN101161636B (en) | 2007-11-21 | 2007-11-21 | Method for purifying capsicine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101852776A CN101161636B (en) | 2007-11-21 | 2007-11-21 | Method for purifying capsicine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101161636A CN101161636A (en) | 2008-04-16 |
| CN101161636B true CN101161636B (en) | 2010-06-02 |
Family
ID=39296626
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101852776A Active CN101161636B (en) | 2007-11-21 | 2007-11-21 | Method for purifying capsicine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101161636B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102140067A (en) * | 2011-01-31 | 2011-08-03 | 新疆隆平高科弘安天然色素有限公司 | Method for extracting and purifying high-purity capsaicine from capsicum oleoresin |
| CN102302461B (en) * | 2011-09-02 | 2013-04-17 | 海南锦瑞制药股份有限公司 | Dantrolene sodium freeze-dried powder injection for injection and preparation method thereof |
| CN103724220B (en) * | 2013-12-25 | 2016-03-23 | 晨光生物科技集团股份有限公司 | A kind of purification process of capsicine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1711908A (en) * | 2004-06-25 | 2005-12-28 | 杨凌宏峰生物科技开发有限公司 | Production of high-purity capsaicin crystal by ion exchange resin method |
| CN1970530A (en) * | 2006-11-28 | 2007-05-30 | 广西大学 | Method for separating and purifying capsaicin compound using membrane separation technology |
-
2007
- 2007-11-21 CN CN2007101852776A patent/CN101161636B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1711908A (en) * | 2004-06-25 | 2005-12-28 | 杨凌宏峰生物科技开发有限公司 | Production of high-purity capsaicin crystal by ion exchange resin method |
| CN1970530A (en) * | 2006-11-28 | 2007-05-30 | 广西大学 | Method for separating and purifying capsaicin compound using membrane separation technology |
Non-Patent Citations (2)
| Title |
|---|
| 周雯雯等.辣椒碱的提取精制和应用现状.生物质化学工程41 3.2007,41(3),56-58. |
| 周雯雯等.辣椒碱的提取精制和应用现状.生物质化学工程41 3.2007,41(3),56-58. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101161636A (en) | 2008-04-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20140039288A (en) | Aliphatic polyester polyols from cyclohexane oxidation byproduct streams as precursors for polyurethane and polyisocyanurate polymers | |
| CN101161636B (en) | Method for purifying capsicine | |
| CN103193622B (en) | Recovery method of glycolic acid in phenoxy carboxylic acid industrial wastewater | |
| CN1927854A (en) | Preparation method of potassium sodium dehydroandroan drographolide succinate, potassium sodium dehydroandroan drographolide succinate preparation and preparation method thereof | |
| KR101764477B1 (en) | Method for producing polyalkylene glycol derivative having amino group at end, with narrow molecular weight distribution | |
| CN105753718A (en) | Method for removing impurity 2,3,4,5-tetrahydropyridine in nylon salt and purified nylon salt | |
| CN101914098B (en) | Preparation method of Meropenem trihydrate crystals | |
| CN102030647A (en) | Clean production method for preparing liquid antioxidant | |
| CN104610385A (en) | Refining method of D-glucosamine hydrochloride | |
| CN109232707B (en) | Method for removing solvent residues of diammonium glycyrrhizinate bulk drug | |
| CN101863818B (en) | Method for preparing DL-proline | |
| CN1266109C (en) | Technique for prepring 3,4,5-trihydroxybenzoic acid methyl ester | |
| CN103374046A (en) | Method for preparing D-glucosamine hydrochloride | |
| CN102557980A (en) | Method for preparing high-purity capsaicine monomer by crystallization | |
| CN102718740B (en) | Trioxymethylene crystallization method | |
| CN108191727A (en) | A kind of synthetic method of the different Thiocyanato -2- of 4- (trifluoromethyl) benzonitrile | |
| CN103709039A (en) | Method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite | |
| CN103172839A (en) | Method for preparing high-molecular-weight polylactic acid through direct condensation polymerization | |
| CN102875476B (en) | Method for preparing metronidazole benzoate | |
| CN103804265B (en) | The synthesis of a kind of Sulpiride or its optical isomer and post-processing approach | |
| CN105797643A (en) | Method for preparing non-ionic polyurethane Gemini surfactant | |
| CN101928261A (en) | Method for producing 2,2'-dibenzothiazolyl disulfide by nitric acid one-step method | |
| CN103044282A (en) | Daminozide production method capable of reducing residual amount of UDMH (unsymmetric dimethyl hydrazine) | |
| CN101074241A (en) | Method for preparing acephate | |
| CN101289462B (en) | Process for preparing acephate from ethenone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |