CN1110622A - Technology for extracting capsaicine from dry chilli - Google Patents
Technology for extracting capsaicine from dry chilli Download PDFInfo
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- CN1110622A CN1110622A CN94104403A CN94104403A CN1110622A CN 1110622 A CN1110622 A CN 1110622A CN 94104403 A CN94104403 A CN 94104403A CN 94104403 A CN94104403 A CN 94104403A CN 1110622 A CN1110622 A CN 1110622A
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- capsaicine
- ether
- chilli
- ethanol
- benzinum
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Abstract
The process for preparing capsaicine from dry chilli powder features use of alcohol, ether and ligarine as extractant, diluted alkalilye for dissolving, hydrochloric acid for regulating pH value to 7-10, and organic solvent such as alcohol, ether, n-butane or ligarine for purification after extracting three times. Its advantages include simple technology (only phase splitting 4 times), high quality of product and easily available raw materials.
Description
The present invention relates to preparation technology's method of capsaicine.
Capsaicine is an important indicator weighing capsicum quality and definite breed difference, and it is not only important flavouring, more importantly is as nontoxic tear bombnoun, treatment stomach trouble and leukaemia, has very high economic worth.
Since this century many scholar's research have been arranged and have extracted the method for capsaicine by capsicum, they general process route all be to adopt organic solvent from chilli, to extract grease, from grease, isolate capsaicine again.Nelson(J.Ind.Eng.Chem.2,419,1910) shared 11 phase-splittings just obtain capsaicine, and condition harshness, complex steps, productive rate are lower; Todd(Food Technol.12,468,1958) use acetic acid, chloroform extracting, activated carbon decolorizing only provides reference for quantitative analysis; Karawya[Analyst(London) 92,581,1967] etc. the human column chromatography replaces many extractions of Nelson, though aspect simplifying the procedures, obtain breaking through, consuming time oversize; Hungarian patent (No.157919) is an extractant with chlorohydrocarbon, but because halogenated hydrocarbons has the teratogenesis mutagenesis to human body, and do not further developed; People such as Neil L.Sass [Food.Chem.25(6), 1419(1977)] a kind of modification method is proposed, be that raw material passes through repeatedly extractions such as numerous and diverse acetone, ether with fresh green capsicum, avoid using active carbon and halogenated hydrocarbons, and obtain capsaicine.Also there are a lot of people to attempt synthetic capsaicine in addition, but not success as yet up to now, and synthetic analog is not only poisonous, and its pungent degree differs greatly.
The purpose of this invention is to provide a kind of process, utilize this technology only just can obtain capsaicine with four phase-splittings by chilli extraction capsaicine.Raw material of the present invention is easy to get, and technology is simple, and is with low cost, the product quality height.
The present invention is at first with ethanol extraction, concentrated with the chilli powder, again with the alkali treatment of concentrate process, extracted with diethyl ether, separation, petroleum ether extraction, pass through the organic solvent purifying at last again, can obtain pure capsaicine product, the organic reagent that uses in the whole technology can reclaim and use repeatedly.
The weight proportion of chilli and various extractants is among the present invention: ethanol: ether: benzinum: chilli=5～10: 1.5～3: 0.5～1: 1.
Now specific embodiments of the present invention are described below:
The chilli powder is thrown in extractor, with 50～80% ethanol, preferably utilize 70% edible ethanol to be extractant, with the agitator stirring ethanol is fully mixed with chilli powder, ethanol and chilli powder are in 5～10: 1 ratio is mixed, and extraction is soaked and is not less than 5 hours under 30～70 ℃ of temperature, must be dissolved with the extract of capsaicine then through press filtration, filter residue can extract capsicum red pigment by usual method, finishes phase-splitting for the first time.Then extract is carried out evaporation and concentration, 78～85 ℃ of control evaporating temperatures, and reclaim ethanol with condenser, the gained concentrate is moved into the alkali dissolving tank, add 3～15% sodium hydroxide solutions to dissolving fully, concentrate and alkali lye leave standstill, tell the alkali lye phase in 1: 2～5 ratios, transfer pH=7-10 with acid solution, finish phase-splitting for the second time.Aqueous slkali is moved in the extractor, is extractant with ether, extracts in ether and alkali lye 1～5: 1 ratio, leaves standstill, and tells the ether phase, finishes phase-splitting for the third time.Ether evaporated mutually and reclaim ether, the gained concentrate moves in the extractor, is extractant with benzinum, extracts in benzinum and concentrate 8～15: 1 ratio, leaves standstill and tells the benzinum phase, finishes the 4th phase-splitting.With benzinum phase evaporation and concentration, and reclaim benzinum.
At last with concentrate with organic solvent purifying such as ether, ethanol, benzinum or normal butanes, and the capsaicine crystallization.
The present invention can obtain the capsaicine product through four phase-splittings, and raw material is easy to get, and technology is simple, and is easy to operate, and the product quality height is easy to suitability for industrialized production.
Below by example method of manufacturing technology of the present invention is described further, agents useful for same is AR among the present invention.
Example 1
Chilli powder 80Kg is dropped in the extractor, add 70% ethanol 700Kg, fully mix, make the chilli powder complete wetting, quiet bubble is 5 hours under 50 ℃ of temperature, stirs frequently therebetween, with air compressor ethanol extract is extruded through filter plate then, leave standstill 1 hour after, extract is moved in the evaporimeter, evaporate, and condensation recovery ethanol, evaporator temperature remains on 75～80 ℃, the gained concentrate is moved in the molten knockout drum of alkali, add 5%NaOH, fully stirring and dissolving, tell water, transfer pH=9, move into the extracted with diethyl ether jar with 1: 1 hydrochloric acid, add diethyl ether fully mix after, leave standstill, after the separation ether extraction liquid, in evaporimeter, carry out evaporation and concentration in 50-55 ℃, reclaim ether, concentrate is added benzinum, in extraction kettle, extract, leave standstill, isolate the benzinum phase, equally through evaporation and concentration, reclaim benzinum, obtain concentrate.This concentrate is carried out purification process with 4000 milliliters of ether again, get capsaicine product 40g.
Example 2
Handle chilli powder 100Kg, operating procedure is with example 1, and last concentrate carries out purification process with normal butane, can get capsaicine product 49g.
Example 3
Handle chilli powder 150Kg, operating procedure is with example 1, and last concentrate adds ethanol and carries out purifying, can get capsaicine product 77g.
Claims (6)
1, a kind of is the method for feedstock production capsaicine with the chilli, and it comprises uses ethanol, ether and benzinum as extractant, it is characterized in that its operating procedure is:
(1) ethanol of the chilli powder being put into 50-80% in reactor soaked extraction more than 5 hours under 30-70 ℃ of temperature;
(2) isolated immersion extract evaporation and concentration under 78～85 ℃ of temperature, concentrate add sig water dissolves fully, leaves standstill, and the alkali lye phase of separation is transferred pH=7～10 with acid solution;
(3) alkali lye moves in the extractor, adds ether, fully hybrid extraction;
(4) with ether extraction liquid in evaporimeter under 50～55 ℃ of temperature evaporation and concentration reclaim ether, concentrate adds petroleum ether extraction;
(5) again with benzinum phase evaporation and concentration, reclaim benzinum, last, concentrate is purifying in organic solvent, promptly gets product.
2,, it is characterized in that the weight proportion of chilli and extractant is according to the said method for preparing capsaicine of claim 1
Ethanol: chilli=5～10: 1
Ether: chilli=1.5～3: 1
Benzinum: chilli=0.5～1: 1.
3,, it is characterized in that said ethanol is 70% edible ethanol according to the said method for preparing capsaicine of claim 1.
4,, it is characterized in that said diluted alkaline is the sodium hydroxide solution of 5-15% according to the said method for preparing capsaicine of claim 1.
5,, it is characterized in that said acid is 1: 1 hydrochloric acid according to the said method for preparing capsaicine of claim 1.
6,, it is characterized in that said organic solvent is ethanol, ether, benzinum or normal butane according to the said method for preparing capsaicine of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94104403A CN1037242C (en) | 1994-04-22 | 1994-04-22 | Technology for extracting capsaicine from dry chilli |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94104403A CN1037242C (en) | 1994-04-22 | 1994-04-22 | Technology for extracting capsaicine from dry chilli |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1110622A true CN1110622A (en) | 1995-10-25 |
| CN1037242C CN1037242C (en) | 1998-02-04 |
Family
ID=5031561
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94104403A Expired - Fee Related CN1037242C (en) | 1994-04-22 | 1994-04-22 | Technology for extracting capsaicine from dry chilli |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1037242C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094310C (en) * | 1999-04-30 | 2002-11-20 | 郑树芹 | Preparation method of assistant for pesticide plant source |
| CN100406432C (en) * | 2005-01-18 | 2008-07-30 | 天津科技大学 | Process of extracting capsicine crystal from chili |
| CN100512806C (en) * | 2003-04-14 | 2009-07-15 | Lts勒曼治疗系统股份公司 | Therapeutic patch with polysiloxane matrix comprising capsaicin |
| CN102516110A (en) * | 2011-12-07 | 2012-06-27 | 天津大学 | High-purity capsaicin compound refining crystallization method |
| CN108041322A (en) * | 2017-12-06 | 2018-05-18 | 常州朋悦纺织品有限公司 | A kind of duck feed and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5753404A (en) * | 1980-09-17 | 1982-03-30 | Kao Corp | External preparation for skin obtained by blending plant extract |
| CN1019126B (en) * | 1989-04-17 | 1992-11-18 | 周洪喜 | Process for extracting capsic pigment and capsaicine |
| CN1059742A (en) * | 1990-09-11 | 1992-03-25 | 周建功 | Extract capsochrome and peppery plain processing method by capsicum |
| CN1053803A (en) * | 1991-03-18 | 1991-08-14 | 贵阳市云岩区农副业生产基地 | The production method of natural chilli pigment |
| US5728507A (en) * | 1996-02-20 | 1998-03-17 | Motorola, Inc. | Method for planarizing a semiconductor layer |
-
1994
- 1994-04-22 CN CN94104403A patent/CN1037242C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094310C (en) * | 1999-04-30 | 2002-11-20 | 郑树芹 | Preparation method of assistant for pesticide plant source |
| CN100512806C (en) * | 2003-04-14 | 2009-07-15 | Lts勒曼治疗系统股份公司 | Therapeutic patch with polysiloxane matrix comprising capsaicin |
| CN101601664B (en) * | 2003-04-14 | 2012-05-23 | Lts勒曼治疗系统股份公司 | Therapeutic patch comprising capsaicin and method for preparing the same |
| CN100406432C (en) * | 2005-01-18 | 2008-07-30 | 天津科技大学 | Process of extracting capsicine crystal from chili |
| CN102516110A (en) * | 2011-12-07 | 2012-06-27 | 天津大学 | High-purity capsaicin compound refining crystallization method |
| CN102516110B (en) * | 2011-12-07 | 2014-04-23 | 天津大学 | High-purity capsaicin compound refining crystallization method |
| CN108041322A (en) * | 2017-12-06 | 2018-05-18 | 常州朋悦纺织品有限公司 | A kind of duck feed and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1037242C (en) | 1998-02-04 |
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