CN1226276C - Extraction of natural capsaicine - Google Patents
Extraction of natural capsaicine Download PDFInfo
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- CN1226276C CN1226276C CN 03109061 CN03109061A CN1226276C CN 1226276 C CN1226276 C CN 1226276C CN 03109061 CN03109061 CN 03109061 CN 03109061 A CN03109061 A CN 03109061A CN 1226276 C CN1226276 C CN 1226276C
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Abstract
The present invention relates to a method for preparing capsaicine, particularly to a method for extracting natural capsaicine by adopting cayenne pepper or pepper extract which is a side product after orange red coloring matters are extracted from peppers. The present invention adopts alcohol, ether, acetone, petroleum ether, ethyl acetate, ethyl acetate, etc. as lixiviating extracting agents. Separation accelerating agents are added, which leads phase separation to be quickly completed without generation of a third phase. Saponifying active agents are adopted, which leads a saponifying reaction to be quickly completed under the low temperature (28 DEG C to 35 DEG C). Purifying agents are used, which leads crystals of natural capsaicine to be stable. The present invention has the advantages of simple equipment, easy operation, easy acquirement of raw material, short production period, little loss, quality assurance, low cost and high profit. More than 99 % of main components of capsaicine can be obtained. The serialization large scale production of pure products of the natural capsaicine can be realized.
Description
Technical field
The present invention relates to the preparation of capsicine, is raw material with red chilly powder or the byproduct chilli extract that extracted behind the orange red pigment by capsicum particularly, extracts the method for natural capsicine.
Technical background
The extracting method of at present relevant natural capsicine comprises: 1) solvent-extraction process.Use the organic solvent extraction oleo resin capsicum, from grease, isolating capsicine, many companions of these class methods condition harshness, step is loaded down with trivial details, and what have also needs the fractionation by adsorption post, and process cycle is long, only is that extract or trial-production in a small amount in the laboratory mostly.As Nelson method (J.Ind.Eng.Chem.2,419, (1910)) and Karawya method [Analyst (London), 92581 (1967)] and Neil.L.Sass method [Food.Chem.25 (6), 1419 (1977)].2) co_2 supercritical fluid extraction method, this processing method also must be used solvent method, repeatedly handles and just can obtain the pure product of capsicine.For example Fekaya method [Jpn.Kokai Tokyo Koho JP01,280,052 (1989)] is the entrainment agent co_2 supercritical fluid extraction with ethanol, only can separate obtaining 80% capsicine.Chinese patent ZL94104403.3 discloses the extracting method of capsicine, and it is to be that raw material has just obtained the pure product of capsicine with solvent method through four phase-splittings with the chilli, has simplified technology, has realized industrialization, productive rate 1.5-2/10000.But still exist the time that is separated long, and third phase appears, and its alkali purification temp height loses problems such as bigger.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of improved natural capsicine can overcome the deficiencies in the prior art.The present invention can reach rapidly and is separated when keeping technology easy, and no third produces mutually, and saponification temperature is reduced greatly.So both reduce facility investment, shortened the production cycle, improved productive rate again; Use scavenging agent simultaneously, can guarantee capsicine crystallization-stable and quality product, can obtain the capsicine main component and reach more than 99%.Present device is simple, processing ease, and raw material is easy to get, and cost is low, and the profit height can be realized the pure product of serialization scale operation natural capsicine.
The present invention uses chilli extract to be raw material, carries out low-temperature saponification with the alkaline solution that is added with promoting agent, through being added with fast organic solvent sharp separation from agent, obtains the pure product of natural capsicine through the scavenging agent processing again.The present invention can be a raw material with red chilly powder, at first uses the organic solvent lixiviate, through concentrate concentrated solution, carry out above-mentioned technological operation again, produce the pure product of natural capsicine, organic solvent will reclaim repeatedly and use in the whole technology.
The present invention includes with red chilly powder or chilli extract is raw material, and as extraction agent, said capsicine main component is with organic solvent:
Capsicine 57.88～58.97%
Dihydrocapsaicin 36.80～37.89%
Take off Dihydrocapsaicin 0.60%～0.61%
Class capsicine 3.12%
Its operation steps is:
1) in the lixiviate cylinder red chilly powder is put in the organic solvent I, stirs, extracted 1～4 hour under 25 ℃～30 ℃ temperature, isolated vat liquor through evaporation concentration, reclaims organic solvent I, obtains concentrated solution I;
2) concentrated solution I or chilli extract are put in the saponification still, use the sodium hydroxide solution that is added with the saponification promoting agent, stirring reaction is transferred pH 6～10 with acid solution after 1～2 hour again under 28 ℃～35 ℃ temperature, obtains neutralizer;
3) neutralizer is moved among the extractor I, add fastly from agent and organic solvent II, extracted 30 minutes to 120 minutes in 23 ℃～28 ℃ temperature, left standstill 10～30 minutes, tell organic phase, evaporation concentration reclaims organic phase II, concentrated solution II;
4) concentrated solution II is moved into extractor II, add organic solvent II I, extract 30 minutes by 90 minutes in 60 ℃～75 ℃, tell organic phase;
5) organic phase is moved in the cleaner, add scavenging agent, under 25 ℃～30 ℃ temperature, mix and stirred 10～30 minutes, left standstill 5～20 minutes, tell organic phase III;
6) with organic phase III evaporation concentration, reclaim organic solvent II I, concentrated solution is moved in the crystallizer, crystallization in organic solvent I V promptly gets the pure product of natural capsicine;
Wherein, said organic solvent I is 60%～95% ethanol, acetone, ethyl acetate, methyl acetate, normal hexane or ether.
Said organic solvent II is ether, methyl acetate, ethyl acetate or sherwood oil.
Said organic solvent II I is sherwood oil, ether or normal hexane.
Said organic solvent I V is sherwood oil, normal butane, ether or normal hexane.
Said red chilly powder or chilli extract and used volume of organic solvent/weight ratio are:
Organic solvent I: red chilly powder=3～5: 1
Organic solvent II: red chilly powder=1～2: 1
Organic solvent II: chilli extract=2～4: 1
Organic solvent II I: red chilly powder=0.5～1.5: 1
Organic solvent II I: chilli extract=1.5～3: 1.
Said saponification promoting agent is sodium ricinoleate and the rare anhydrous sodium sulphate of sodium oleate of trace and the aqueous solution of salt that contains trace:
Sodium ricinoleate 0.01～0.1%
Sodium oleate 0.01～0.2%
Salt 1～3%
Sodium sulfate (anhydrous) 2～6%
Water surplus.
Said speed is the acid solution of anhydrous sodium sulphate and borax or anhydrous sodium sulphate and trolamine from agent:
I speed is from agent: borax 2～8%
Concentrated hydrochloric acid 0.1～0.3%
Sodium sulfate (anhydrous) 3～10%
Water surplus, and
II speed is from agent: trolamine 0.4～1.5%
Concentrated hydrochloric acid 0.1～0.15%
Sodium sulfate (anhydrous) 3～8%
Water surplus.
Said scavenging agent consists of:
I scavenging agent: citric acid 1～5%
Sodium phosphate dibasic 0.4～0.8%
Water surplus, or
II scavenging agent: citric acid 1～10%
Sodium phosphate dibasic 0.1～0.5%
Water surplus.
Said saponification promoting agent, fastly be from agent, scavenging agent consumption (weight ratio):
Red chilly powder: saponification promoting agent=100: 0.1～0.8
Chilli extract: saponification promoting agent=100: 0.1～5
Red chilly powder: fast from agent=100: 0.1～0.6
Chilli extract: fast from agent=100: 0.8～3
Red chilly powder: scavenging agent=100: 20～60
Chilli extract: scavenging agent=100: 200～400.
Specific embodiments of the present invention is described below:
The raw material chilli extract is dropped in the saponification cylinder, add 4～12% sodium hydroxide solutions that contain promoting agent, chilli extract and sodium hydroxide solution are in 1: 2.5～4.5 ratios, 28 ℃～35 ℃ following stirring reactions 1～2 hour, transfer pH6～10 with acid, it is squeezed into the extraction cylinder, add fast from agent and ethyl acetate, chilli extract and ethyl acetate extract in 1: 2～4 ratios (weight/volume), left standstill 10～30 minutes, and isolated the ethyl acetate phase, ethyl acetate is reclaimed in evaporation, the gained concentrated solution drops into extraction liquid, add sherwood oil, chilli extract and sherwood oil extract in 1: 1.5～3 ratios, tell the sherwood oil phase, add scavenging agent, chilli extract and scavenging agent carry out purifying treatment in 1: 2～4 ratios, at last with the sherwood oil phase evaporation concentration after the purifying treatment, reclaim sherwood oil, the crystallization in normal butane of the concentrated solution of gained promptly gets the pure product of natural capsicine.
If raw material is a red chilly powder, at first red chilly powder is dropped in the lixiviate cylinder, use the normal hexane lixiviate, red chilly powder and normal hexane are in the lixiviate 1～4 hour under 25～30 ℃ of temperature of 1: 3～5 ratios (weight/volume), with the vat liquor evaporation concentration, reclaim normal hexane then, after the acquisition concentrated solution, press aforesaid operations again, final production goes out the pure product of natural capsicine.
The invention belongs to the preparation technology who extracts the pure product of natural capsicine by red chilly powder or chilli extract industry.Adopt ethanol, ether, acetone, sherwood oil, ethyl acetate or ethyl acetate etc. to be the lixiviate extraction agent, add fastly from agent, making is separated finishes rapidly and no third produces mutually.In the extracting and separating step, phase-splitting need be left standstill 6-20 hour in the prior art, and the present invention only need be left standstill 10-30 minute.Adopt the saponification promoting agent, saponification reaction is finished at low temperatures fast.The use of scavenging agent, the natural capsicine crystallization is more stable.This processing method is simple, and operational condition is easy to control, and is with short production cycle, and loss is few, guarantees quality product, can obtain the capsicine main component and reach more than 99%, productive rate 3.4-4/10000 (red chilly powder meter), productive rate 3.4-4/1000 (chilli extract meter).
Embodiment
Below by embodiment the present invention is described further.
Embodiment 1
Take by weighing chilli extract 50Kg and drop into adding promoting agent 60g in the saponification cylinder, rise moving the stirring, add 150kg 5% sodium hydroxide solution again, in 29 ℃ of down reactions 80 minutes, after adding concentrated hydrochloric acid then and adjusting system PH=8.5, drop into extraction cylinder I, add I speed from 150 liters of agent 400g and ether, in 25 ℃ of extractions 30 minutes, to leave standstill 15 minutes, analyse clearly at the interface, isolate the ether phase, reclaim ether in the evaporating kettle evaporation, gained concentrated solution input extraction cylinder II adds 100 liters of sherwood oils, in 70 ℃ of extractions 45 minutes, the sherwood oil that to tell adds I scavenging agent 150kg in cleaner, purifying treatment 30 minutes left standstill 20 minutes, the sherwood oil phase evaporation concentration that to isolate, reclaim sherwood oil, the crystallization in normal hexane of gained concentrated solution gets the pure product 160g of natural capsicine.Productive rate 3.2/1000.
Through high pressure liquid chromatographic analysis, capsicine content:
Capsicine 57.88%
Dihydrocapsaicin 37.89%
Take off Dihydrocapsaicin 0.61%
Class capsicine 3.12%.
Embodiment 2
Taking by weighing red chilly powder 400kg drops in the lixiviate cylinder, add 1200 liters of ethanol, in 28 ℃ of following lixiviates 90 minutes, then with the vat liquor evaporation concentration, reclaim ethanol, the gained concentrated solution drops in the saponification cylinder, continue operation, technology is with embodiment 1, and the inventory of adding is respectively: saponification promoting agent 450g, 8% sodium hydroxide solution 120kg, II speed is from 480 liters of agent 400g and ethyl acetate, leave standstill 20 fens master slave interfaces and analyse clearly, no third phase, 220 liters of hexanes, I scavenging agent 160kg obtains the pure product 150g of natural capsicine.Productive rate 3.75/10000.
Through high pressure liquid chromatographic analysis, capsicine content:
Capsicine 58.97%
Dihydrocapsaicin 36.80%
Take off Dihydrocapsaicin 0.60%
Class capsicine 3.12%.
Embodiment 3
Take by weighing chilli extract 70kg, drop in the saponification cylinder, operating procedure is with embodiment 1, its material add-on is respectively: saponification promoting agent 90g, and 6% sodium hydroxide solution 160kg, II speed is from 200 liters of agent 600g and methyl acetates, leave standstill 20 fens master slave interfaces and analyse clearly, no third produces mutually; 150 liters of sherwood oils, II scavenging agent 300kg obtains the pure product 245g of natural capsicine.Productive rate 3.5/1000.
Through high pressure liquid chromatographic analysis, capsicine content:
Capsicine 57.88%
Dihydrocapsaicin 37.89%
Take off Dihydrocapsaicin 0.61%
Class capsicine 3.12%.
Embodiment 4
Take by weighing red chilly powder 300kg and drop in the lixiviate cylinder, add 1000 liters in acetone, in 35 ℃ of stirring and leaching 120 minutes, with the vat liquor evaporation, reclaim acetone, the gained concentrated solution drops in the saponification cylinder, continues operating procedure with embodiment 1, adds inventory and is respectively:
Saponification promoting agent 380g
4% sodium hydroxide solution 150kg
II speed is from agent 350g and 340 liters of ether (left standstill 20 minutes, analyse clearly at the interface, and no third produces mutually)
150 liters of sherwood oils
II scavenging agent 140kg
Get the pure product 125g of natural capsicine, productive rate 4.16/10000.
Through high pressure liquid chromatographic analysis, capsicine content:
Capsicine 57.88%
Dihydrocapsaicin 37.89%
Take off Dihydrocapsaicin 0.61%
Class capsicine 3.12%.
Claims (5)
1, a kind of extracting method of natural capsicine, it comprises that with red chilly powder or chilli extract be raw material, as extraction agent, said capsicine main component is with organic solvent:
Capsicine 57.88～58.97%
Dihydrocapsaicin 36.80～37.89%
Take off Dihydrocapsaicin 0.60%～0.61%
Class capsicine 3.12%
The operation steps that it is characterized in that it is:
1) put into red chilly powder and organic solvent I in the lixiviate container, stir, extracted 1～4 hour under 25 ℃～30 ℃ temperature, isolate vat liquor, evaporation concentration reclaims organic solvent I, obtains concentrated solution I;
2) concentrated solution I or chilli extract are put in the saponification still, add the sodium hydroxide solution that contains the saponification promoting agent, stirring reaction is transferred pH6～10 with acid solution after 1～2 hour again under 28 ℃～35 ℃ temperature, obtains neutralizer;
3) neutralizer is moved among the extractor I, add fastly from agent and organic solvent II, extracted 30 minutes to 120 minutes in 23 ℃～28 ℃ temperature, left standstill 10～30 minutes, tell organic phase, evaporation concentration reclaims organic phase II, concentrated solution II;
4) concentrated solution II is moved into extractor II, add organic solvent II I, extract 30 minutes by 90 minutes in 60 ℃～75 ℃, tell organic phase;
5) organic phase is moved in the cleaner, add scavenging agent, under 25 ℃～30 ℃ temperature, mix and stirred 10～30 minutes, left standstill 5～20 minutes, tell organic phase III;
6) with organic phase III evaporation concentration, reclaim organic solvent II I, concentrated solution is moved in the crystallizer, crystallization in organic solvent I V promptly gets the pure product of natural capsicine;
Said organic solvent I is 60%～95% ethanol, acetone, ethyl acetate, methyl acetate, normal hexane or ether;
Said organic solvent II is an ether, or methyl acetate, or ethyl acetate, or sherwood oil;
Said organic solvent II I is sherwood oil, ether or normal hexane;
Said organic solvent I V is sherwood oil, normal butane, ether or normal hexane;
Said scavenging agent is the aqueous solution of citric acid and Sodium phosphate dibasic, and weight consists of:
I scavenging agent: citric acid 1～5%
Sodium phosphate dibasic 0.4～0.8%
Water surplus, or
II scavenging agent: citric acid 1～10%
Sodium phosphate dibasic 0.1～0.5%
Water surplus;
Said speed is the acidic aqueous solution of anhydrous sodium sulphate and borax or anhydrous sodium sulphate and trolamine from agent, and weight consists of:
I speed is from agent: borax 2～8%
Concentrated hydrochloric acid 0.1～0.3%
Anhydrous sodium sulphate 3～10%
Water surplus, or
II speed is from agent: trolamine 0.4～1.5%
Concentrated hydrochloric acid 0.1～0.15%
Anhydrous sodium sulphate 3～8%
Water surplus;
Said saponification promoting agent is sodium ricinoleate and the rare anhydrous sodium sulphate of sodium oleate of trace and the aqueous solution of salt that contains trace, and weight consists of:
Sodium ricinoleate 0.01～0.1%
Sodium oleate 0.01～0.2%
Salt 1～3%
Anhydrous sodium sulphate 2～6%
Water surplus.
2,, it is characterized in that said red chilly powder or chilli extract and used volume of organic solvent/weight ratio are according to the extracting method of the said natural capsicine of claim 1:
Organic solvent I: red chilly powder=3～5: 1
Organic solvent II: red chilly powder=1～2: 1
Organic solvent II: chilli extract=2～4: 1
Organic solvent II I: red chilly powder=0.5～1.5: 1
Organic solvent II I: chilli extract=1.5～3: 1.
3,, it is characterized in that said concentration of sodium hydroxide solution is 4%～12% according to the pure product method of the said preparation natural capsicine of claim 1.
4,, it is characterized in that said acid solution is a concentrated hydrochloric acid according to the extracting method of the said natural capsicine of claim 1.
5,, it is characterized in that said saponification promoting agent, fast weight ratio from agent, scavenging agent consumption are according to the extracting method of the said natural capsicine of claim 1:
Red chilly powder: saponification promoting agent=100: 0.1～0.8
Chilli extract: saponification promoting agent=100: 0.1～5
Red chilly powder: fast from agent=100: 0.1～0.6
Chilli extract: fast from agent=100: 0.8～3
Red chilly powder: scavenging agent=100: 20～60
Chilli extract: scavenging agent=100: 200～400.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03109061 CN1226276C (en) | 2003-04-03 | 2003-04-03 | Extraction of natural capsaicine |
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|---|---|---|---|
| CN 03109061 CN1226276C (en) | 2003-04-03 | 2003-04-03 | Extraction of natural capsaicine |
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| CN1226276C true CN1226276C (en) | 2005-11-09 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344608C (en) * | 2004-06-25 | 2007-10-24 | 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 |
| CN100406432C (en) * | 2005-01-18 | 2008-07-30 | 天津科技大学 | Process of extracting capsicine crystal from chili |
| CN1318391C (en) * | 2005-07-08 | 2007-05-30 | 上海雷辣婆食品有限公司 | Method of extracting capsaicin and capsaithin from red pepper |
| CN100516027C (en) * | 2006-04-28 | 2009-07-22 | 中国科学院过程工程研究所 | Method for purifying capsicine compound from capsicol resin by using ammoniacal liquor |
| CN101225052B (en) * | 2007-12-21 | 2012-03-21 | 王海棠 | Process for extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude product from red pepper |
| CN101744207B (en) * | 2010-02-25 | 2013-09-11 | 周顺 | Method for preparing high-pungency chilli extract |
| CN102492307B (en) * | 2011-12-08 | 2014-05-21 | 晨光生物科技集团股份有限公司 | Hydration degumming method for hot pepper extract |
| CN103936612B (en) * | 2014-04-28 | 2017-01-11 | 福建正味生物科技有限公司 | Preparation method of capsaicin compound |
| CN108850994A (en) * | 2018-06-25 | 2018-11-23 | 南昌大学 | A kind of spicy powder, preparation method thereof |
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2003
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