CN1186314C - Microwave once process for extracting capsaicin and pigment - Google Patents
Microwave once process for extracting capsaicin and pigment Download PDFInfo
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- CN1186314C CN1186314C CNB021314675A CN02131467A CN1186314C CN 1186314 C CN1186314 C CN 1186314C CN B021314675 A CNB021314675 A CN B021314675A CN 02131467 A CN02131467 A CN 02131467A CN 1186314 C CN1186314 C CN 1186314C
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- capsaicine
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- red pepper
- organic solvent
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- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The present invention discloses a method for extracting capsaicin from dried red hot peppers with alkali liquor in a microwave radiation field, separating and purifying the capsaicin once by a polarity macroporous resin column, and obtaining pigment from filtration residues with acetone, alcohol, etc. according to a literature technology. Compared with an organic solvent method, the present invention has the advantages that extraction time is shortened by scores of times, investment for equipment and floor space are reduced, energy consumption is little, and the alkali liquor can be recovered for reuse. The method is an environmental protection technical method. When the method is applied to industrial production, the benefit is obvious.
Description
The present invention relates to a kind of natural active matter leaching method, particularly in ripe capsicum, obtain the method for capsaicine and food dye continuously with the microwave buck.
Existing technical literature such as Chinese patent " extract the novel process of capsanthin and capsaicine in red pepper " and " extracting method of capsochrome and capsaicine " and document " screening of capsaicine extracting method " northwest pharmaceutical journal 1996.11 (2) is used all is first with ethanol or acetone and other organic solvent extracting.Find all that in our simulation test the aftertreatment separation circuit is complicated and be difficult for dividing clean.The present invention has improved the first step extracting, utilizes capsaicine to dissolve in the buck and the water insoluble character of pigment, at first with containing NaOH or the KOH buck proposes peppery element.Separation is with look fully and not, is placed in the microwave field when extracting and handles, and extracting has speeded up tens times.Filtering bits are obtained pigment by the known technology of literature method again.Isolating capsicum is young takes out or material such as processing oils, not in this patent scope.
Capsaicine has another name called capsicine, illustrious name (Capsaicin).It is the main composition that produces pungent in the capsicum.Its molecular structure is one and holds dimethyl nine carbochain methoxyl groups to phenol that the 8th a last amide group is a kind of plant acid amides.65 ℃ of fusing points dissolve in organic solvent and the buck.Modern studies show that it has of great value physiologically active.Strong and persistent anti-inflammatory analgesic action is arranged, and making dressing has significant curative effect to chronic rheumatic arthritis, zoster, neurodynia, and psoriasis, baldness are also had therapeutic action, and is again the major ingredient of making the tearing property defensive weapon.Present in the world price per kilogram is more than 5,000 dollars.This just has exploitation to be worth very much.
Another kind of material in the capsicum is natural food colour Capsorubin and Capsanthin (Cap-sorubin and Capsanthin), and the both is the oil soluble toxicological harmless pigment of multiple ketene.Domestic have quite a lot of manufacturer production, and its valency also can reach one kilogram in thousands of units.But mostly capsaicine is carried as refuse or byproduct based on the factory that produces pigment in many producers, the low and quality of yield can not reach export standard.This also be we to study improve technology, to obtain the invention reason of bigger comprehensive benefit.
Our comprehensive extractive processing method be earlier the drying and ripening red pepper of choosing is broken in rotating knife formula beating crusher＜fragment of 3mm, filter out young grain do in addition other composition exploitation with or sell.Again that fragmentation is good capsicum is packed in the Glass Containers.Adding the NaOH of 0.2～1.8Mol or KOH solution soaking is placed on after saturating and accepts microwave radiation in the microwave radiation field and handle.System total mass and microwave energy have been calculated with 0.5～5 watt/milliliter Power Processing.Investigating method heats up system temperature with the control temperature rise and is not more than 50 ℃, after disposing solution is filtered, filtrate is used for further extracting capsaicine, and filter residue continues processing and extracts pigment, boils off solvent and promptly can be used as the sale of commodity capsochrome with conventional organic solvent (ethyl acetate, hexane, acetone, ethanol etc.).
Solution after more than filtering is earlier with acid (Hcl, H
2SO
4, HCOOH and acetic acid) transfer between PH11～8, (concrete model is XAD-7, NKA-9 by polar macroporous adsorption resin then, D145, D160, S-8, NKA-II, HPD-800 etc.) post fully is adsorbed on the resin capsaicine, goes up new post when pungent appears in effluent liquid again.Treating that the saturated back of post absorption capsaicine is cleaned behind the post with organic solvent such as ethyl acetate, ethanol, benzene, hexane, ether, acetone, trichloromethane etc. with pure water gives wash-out.Again elutriant is reduced pressure to steam and stay, promptly get purer capsaicine except that after desolvating.As also not reaching requirement, again product is dissolved in ethanol or the acetone, filter and get elaboration with activated carbon decolorizing, recrystallize.
Present method buck be it seems the more of usefulness, but the buck that gets off from adsorption column, and available strong basic ion exchange resin is removed acid group, can continue again to use after adjusting PH＞12, and this has just greatly alleviated the environmental pollution of buck.The subsequent technique organic solvent will reclaim again, sees that thus processing method of the present invention also is comparatively favourable and feasible to the protection environment.
We set up testing method earlier before doing test, and we are according to the Sodium Nitrite on the classical documents---the Sodium orthomolybdate colorimetry.At the 420nm wavelength measurement, typical curve A=2.880m (mg)+0.0076, r=0.999.Test capsaicin content: % in the different location chilli of buying behind the establishment method respectively
Nanyang, Sichuan, Zhecheng, Henan
0.55 1.39 0.87
Getting Nanyang produces red pepper and is placed in the cutter formula rotation powder beating device and smashes to 3mm.About 260 grams that get screen out the capsicum son, and are standby.
Preparation 2%NaOH solution (about 0.5Mol) is got 400ml and is placed in the 500ml Florence flask, claim 25 gram be above-mentioned to go young red chilly powder to put into, soaking and stirring is not placed on and opens in the microwave oven on the 500W shelves to there being bubble, about three minutes of time, cold filtration is put in taking-up, collection filtrate is put into another 500 milliliters of Erlenmeyer flasks, filter residue adds a little 0.5MolNaOH again and soaks, and is merged filtrate after the filtration, transfers PH to 11 lower slightly with Hcl.Last two φ 2cm * 20cm resin columns, a dress NKA-9 (Nankai University's product) adorns commercially available XAD-7 for one and divides two halves to drip upper prop the above-mentioned alkali lye that contains capsaicine.Adding back observation effluent liquid has not had pungent, and each crosses post with the cold aquae destillata of 50ml again.Use 95% ethanol after washing instead and dripped the post desorb, merge two groups of elutriants and be placed on and heat in the rotatory evaporator about 45 ℃, open off-gas pump to ethanol and steam in a large number.Until do, take off the eggplant bottle, the capsaicine, the color that are bonded on bottle wall with the careful scraping of little spoon are white or little Huang.On analytical balance, weigh 149mg, calculated yield is 67%.
The above capsaicine that obtains recrystallization in a large amount of ethyl acetate is obtained thin platelike crystal, the oven dry of finding time in vacuum drier.Taking away to record on ultraviolet scanner at 210 millimicrons has small one and large one absorption peak with the 254nm place, with the literature value basically identical.Get some again and recording infrared light praseodymium absorption peak on the IR-FT instrument: methoxyl group on the 2890 and 1455 corresponding phenyl ring, 1651cm with pellet technique
-1Corresponding secondary amide base, 1274 corresponding to aryl ethers, and 1381 corresponding to the end sec.-propyl, and 1419 corresponding to methylene radical ketone, and 2930 corresponding to alkane.What confirm that we obtain with this is capsaicine.(referring to accompanying drawing)
Illustrate by other two embodiment more below:
Example one:
Get Zhecheng, commercially available Henan and produce chilli 300 grams, smash the son.Claim 25 gram green pepper powder to be positioned in the 500ml flask, 400 milliliters of NaOH solution that add 0.25Mol (about 1%), be dipped into and stir no bubble, be placed in the microwave oven with 500 watts of power in addition the width of cloth according to 160 seconds, put cold after-filtration, filter residue add again 100ml0.5MolKOH once more in microwave oven with the power width of cloth according to 100 seconds, cold filtration, merge filtrate twice, add acetic acid and transfer PH to 11, last AB-8 resin column absorption, back 95% ethanol elution, on rotatory evaporator, extremely do with 250ml pyriform flask reduction vaporization, scrape product, weigh 98.3mg, calculated yield ≈ 72%.
Example two:
Get high-load Sichuan capsicum and beat powder and go the son, get 25 grams, method is done on the photograph.Leach liquor is used 1.2Mol KOH instead, and secondary leaches the 1.8Mol NaOH with the same amount, D160 resin column absorption on the merging filtrate.Use eluent ethyl acetate, on rotatory evaporator, be decompressed to 45 ℃ of boilings, evaporate to dryness in 250ml pears type bottle, scrape get the product capsaicine weigh 265mg, calculated yield gets 76.2%.
Reach two examples in sum, its yield total all about in the of 70%, trace it to its cause.We think that one is because container is little, each output several grams of a zero point, be difficult to receive clean, and product to spread area out big, be skim, the part of can volatilizing; Two come our experimental technique that the imperfection place is still arranged, as the macroporous adsorbent resin pre-treatment of purchasing is not ideal enough.All can influence yield.Guess and amplify pilot scale on several hectograms during kilogram, yield also can improve.
With regard to the estimation of present yield, the per kilogram product needs the raw material capsicum at 100～250Kg, and with the matter of fundamental importance, the per kilogram product cost valencys such as solvent loss, depreciation that add are also below 20,000 yuan.That is to say that take out with 5,000 dollars of/kilogram calculations, rate of gross profit is greater than 50%.In addition the pigment product that reclaims has been close to net profit.Therefore this technology has market potential.
Claims (3)
1. method of in red pepper, extracting capsaicine and pigment, it is characterized in that earlier paprika powder being broken to particle less than 3mm, filter out young grain, the red pepper grain is placed container, the sodium hydroxide or the potassium hydroxide that add 0.2～1.8 volumetric molar concentration of 16 times of amounts, soak evenly to be placed in the microwave field and penetrate Power Processing with 0.5～5.0 watt every milliliter the width of cloth, the control temperature rise is not more than 50 ℃, filtrate last polar macroporous resin column after transferring pH value of handling after-filtration adsorbs, the post flushing is crossed with pure water in saturated back, carry out wash-out with organic solvent afterwards, elutriant evaporated under reduced pressure solvent obtains capsaicine; Filter residue is used acetone again, hexane, and ethyl acetate or ethanol stripping, evaporate to dryness promptly gets pigment.
2. the method for in red pepper, extracting capsaicine and pigment as claimed in claim 1, what it is characterized in that wherein said accent pH value uses is hydrochloric acid, sulfuric acid, formic acid or acetate, PH is between 8-11.
3. the method for extracting capsaicine and pigment in red pepper described in claim 1 is characterized in that wherein said wash-out refers to ethyl acetate, ethanol, trichloromethane or acetone with organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021314675A CN1186314C (en) | 2002-10-16 | 2002-10-16 | Microwave once process for extracting capsaicin and pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021314675A CN1186314C (en) | 2002-10-16 | 2002-10-16 | Microwave once process for extracting capsaicin and pigment |
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| CN1445212A CN1445212A (en) | 2003-10-01 |
| CN1186314C true CN1186314C (en) | 2005-01-26 |
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| CNB021314675A Expired - Fee Related CN1186314C (en) | 2002-10-16 | 2002-10-16 | Microwave once process for extracting capsaicin and pigment |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102058083B (en) * | 2010-11-09 | 2012-12-19 | 老河口华松科技有限责任公司 | Method for preparing water-soluble chili fine powder by chili skin |
| CN102127448B (en) * | 2010-12-22 | 2013-04-24 | 晨光生物科技集团股份有限公司 | Method for extracting oxidation-resistant substance from capsicum residues |
| CN102516802A (en) * | 2011-12-12 | 2012-06-27 | 山东凯斯达机械制造有限公司 | Method for extracting capsicum red pigment and capsaicin |
| CN103798133B (en) * | 2014-01-23 | 2016-03-09 | 青岛农业大学 | High and the selection of capsicum genetic stability inbred line not easy to fade of a kind of haematochrome content |
| CN104003897A (en) * | 2014-06-19 | 2014-08-27 | 南京麦思德餐饮管理有限公司 | Method for preparing capsaicin |
| 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 |
| CN106966917A (en) * | 2017-03-08 | 2017-07-21 | 黄冈师范学院 | Extraction separation method, capsorubin, the capsaicine of raw material of hot pepper |
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2002
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