CN101057660B - Technique method for producing capsicine crystal from capsicum oleoresin - Google Patents
Technique method for producing capsicine crystal from capsicum oleoresin Download PDFInfo
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- CN101057660B CN101057660B CN200710057470A CN200710057470A CN101057660B CN 101057660 B CN101057660 B CN 101057660B CN 200710057470 A CN200710057470 A CN 200710057470A CN 200710057470 A CN200710057470 A CN 200710057470A CN 101057660 B CN101057660 B CN 101057660B
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Abstract
The invention relates to a method for preparing capsicine crystal with red pepper, comprising following steps: extracting capsicine from red pepper with organic solution at 55-70 Deg. C, washing extract with complex cleaner composed of NaHCO3, NaOH and NaCl, separating and getting cleaned extract, purifying cleaned extract for 1-4 hours, crystallizing at temperature below 18 Deg. C and getting capsicine. The invention is characterized by simple process, easy operation, and high-purity product, wide suitability and easiness for large scale industrial production.
Description
Technical field
The present invention relates to produce the process of capsaicine crystals from chilli extract.It is the process of only producing high-purity capsaicine crystals with a kind of organic solvent and the washing of a kind of composite purifying agent from chilli extract.
Background technology
Because unique physiological function of natural capsicine has been widely used in a lot of fields such as food, medicine, military affairs, agricultural, chemical industry and vigorous and graceful cosmetic.Being summarized by the method for chilli extract extraction natural capsicine crystal at present has: ion-exchange, column chromatography, supercritical extraction and organic solvent extractionprocess, all there is the problem of different aspect in these methods when industrial implementation: (1) complex process, the heavy length of process route, (2) the solvent for use kind is many, consumption is big, (3) auxiliary equipment such as solvent recovery, rectifying is many, and investment is big.Therefore suitability for industrialized production all has certain difficulty.
Summary of the invention
The purpose of this invention is to provide a kind of process of producing capsaicine crystals, can overcome the deficiencies in the prior art from chilli extract.Only with a kind of organic solvent and a kind of composite purifying agent, thereby production craft step is simplified greatly in the whole technical process, easy operating is controlled.Whole technical process is simple, obtains the high-purity natural capsaicine crystals.Applicability is strong, is easy to large-scale industrial production.
Step of producing the process of capsaicine crystals from chilli extract provided by the invention comprises: capsaicine reflux extraction is separated from the chilli extract raw material with organic solvent under 55 ℃～70 ℃ temperature, use NaHCO then
3, the composite purifying agent formed of the aqueous solution of NaOH and NaCl carries out washing, purifying to extract, separates to such an extent that purify extract, carries out crystallization under the temperature below 18 ℃ again with the extract insulation purifying 1～4h that purifies at last, obtains capsaicine crystals.
A kind of process of producing capsaicine crystals provided by the invention from chilli extract, its process step comprises:
1) under 55 ℃～70 ℃ temperature, with n-hexane or No. 6 solvent naphtha solvent extraction chilli extracts, reflux extraction capsaicine, the stirring and refluxing extraction time is 30 minutes to 60 minutes, and centrifugation gets extract; The mass ratio of described n-hexane or No. 6 solvent naphthas and chilli extract is 4～8: 1.Reflux extraction liquid enters in the butterfly seperator with 11～16kg/min speed and separates.
2) under 40 ℃～50 ℃ temperature, extract and composite purifying agent fully mix and carry out agitator treating and purify 20 minutes to 40 minutes, are incubated 20-30 minute, and described composite purifying agent is by 2-6%NaHCO
3The aqueous solution 2-5%NaOH aqueous solution and the 4-8%NaCl aqueous solution are formed; Described NaHCO
3, the NaOH aqueous solution and the NaCl aqueous solution mass ratio be: 1: 0.8-1.5: 18-20.
3) centrifugation or leave standstill separation in 1-24 hour, the capsaicine extraction solution that must purify.The preferred butterfly centrifugal machine that uses carries out centrifugation.The washing, purifying extract enters in the butterfly seperator with 20～22kg/min speed and separates.
4) the capsaicine extraction solution after will purifying is in 25 ℃～35 ℃ insulation 1～4h down;
5) crystallization (preferred 5-15 ℃ is carried out crystallization) is carried out in cooling under the temperature below 18 ℃, filter, and drying obtains capsaicine crystals.
Described its total alkali of chilli extract raw material is more than 2% (quality).
Crystallization Separation obtains mother liquor after the capsaicine crystals recyclable organic solvent usefulness again after concentrated among the present invention, gained capsaicine crystals of the present invention, and through high-performance liquid chromatogram determination, total alkali reaches more than 96.8% (quality), wherein:
Capsaicine content 60.5%
Dihydrocapsaicin content 32.1%
Class capsaicine content 4.2%
Total alkali recovery is more than 88%.
With existing technology contrast, the present invention has following characteristics:
1) in the whole technical process only with a kind of organic solvent and a kind of composite purifying agent, thereby production technology is simplified greatly, easy operating is controlled.
2) crystallization control process obtains the high-purity natural capsaicine crystals behind the purifying.
3) whole technology is only passed through the simple separation step, has realized the suitability for industrialized production of natural capsicine crystal, and investment and production cost reduce greatly.
The specific embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1: the composite purifying agent preparation
Normal temperature takes by weighing sodium acid carbonate 0.42kg, drops in the dosing cylinder, adds 10kg water, starts stirring, gets 4%NaHCO fully after the dissolving
3The aqueous solution.
Take by weighing 0.4kg NaOH equally, add 10kg water, get the 4%NaOH aqueous solution.Take by weighing 10.8kg salt, add water 170kg, get the 6%NaCl aqueous solution.
With above-mentioned three kinds of solution in pill tank, stir miscible after, filtering back gained filtrate through filter is NaHCO
3, NaOH and NaCl the composite purifying agent formed of the aqueous solution.
Embodiment 2:
No. 6 solvent naphthas of 300kg are squeezed in the extraction cylinder, started and stir, chilli extract 50kg is squeezed into the extraction cylinder, 65 ℃ ± 2 ℃ reflux extractions 35 minutes that heat up under agitation enter the butterfly centrifugal machine and separate, and control charging rate 11kg/min separates obtaining extract.
Extract is squeezed into washing tank, heats up 40 ℃～45 ℃, starts stirring, squeeze into composite purifying agent 150kg with 20kg/min speed, after adding, the insulation washing is 30 minutes again, under agitation enter the butterfly centrifugal machine, control charging rate 28kg/min separates being purified extract.The extract of cleaning is inserted 28 ℃ ± 2 ℃, behind the insulation 3h, move in the crystallizer.Crystallizer placed carry out crystallization under 15 ℃.After crystallization was finished, natural filtration after the vacuum drying, obtained capsaicine crystals 540g.
Through high-performance liquid chromatogram determination, total alkali is 99.1%, wherein:
Capsaicine 60.7%
Dihydrocapsaicin 31.9%
Class capsaicine 4.5%
Total alkali recovery 90%.
Embodiment 3:
With 250kg n-hexane input extraction cylinder, stir adding chilli extract 50kg down, heat up 60 ℃ ± 2 ℃ reflux extractions after 30 minutes, enter in the butterfly seperator with 16kg/min speed and separate.The gained extract is in 40 ℃ ± 2 ℃ washing tanks, stir down, add composite purifying agent 120kg with 14～15kg/min, after adding, the insulation washing is after 25 minutes again, separate in the butterfly centrifugal machine with the 22kg/min charging rate, obtain to clean extract behind 30 ℃ ± 2 ℃ maintenance 2h, move in the crystallizer, crystallizer is placed carry out crystallization under 10 ℃, below operation obtains capsaicine crystals 420g with embodiment 2.Through high-performance liquid chromatogram determination, total alkali 96.1%, wherein:
Capsaicine 60.1%
Dihydrocapsaicin 32.3%
Class capsaicine 3.7%
Total alkali recovery 88.6%.
Claims (8)
1. process of producing capsaicine crystals from chilli extract, it is characterized in that: the step of this process comprises: capsaicine reflux extraction is separated from chilli extract with n-hexane or No. 6 solvent naphthas under 55 ℃～70 ℃ temperature, use NaHCO then
3, the composite purifying agent formed of NaOH and the NaCl aqueous solution carries out washing, purifying to extract, separates to such an extent that purify extract, carries out crystallization under the temperature below 18 ℃ again with the extract insulation purifying 1～4h that purifies at last, obtains capsaicine crystals.
2. process of producing capsaicine crystals from chilli extract is characterized in that the step of this process comprises:
1) under 55 ℃～70 ℃ temperature, with n-hexane or No. 6 solvent naphtha solvent extraction chilli extracts, stirring and refluxing extracting capsicum alkali, the stirring and refluxing extraction time is 30 minutes to 60 minutes, and centrifugation gets extract;
2) under 40 ℃～50 ℃ temperature, extract and composite purifying agent fully mix and carry out agitator treating and purify 20 minutes to 40 minutes, are incubated 20-30 minute, and described composite purifying agent is by 2-6%NaHCO
3The aqueous solution, the 2-5%NaOH aqueous solution and the 4-8%NaCl aqueous solution are formed;
3) centrifugation or leave standstill separation in 1-24 hour, the capsaicine extraction solution that must purify;
4) the capsaicine extraction solution after will purifying is in 25 ℃～35 ℃ insulation 1～4h down;
5) crystallization is carried out in cooling under the temperature below 18 ℃, filters, and drying obtains capsaicine crystals.
3. according to the described process of producing capsaicine crystals of claim 2, it is characterized in that the mass ratio of described n-hexane or No. 6 solvent naphthas and chilli extract is 4～8: 1 from chilli extract.
4. according to the described process of producing capsaicine crystals of claim 2, it is characterized in that step 2 from chilli extract) described NaHCO
3, the NaOH aqueous solution and the NaCl aqueous solution mass ratio be: 1: 0.8-1.5: 18-20.
5. according to the described process of producing capsaicine crystals of claim 2 from chilli extract, it is characterized in that described its total alkali of chilli extract raw material 2% to improve quality.
6. according to the described process of producing capsaicine crystals of claim 2, it is characterized in that described centrifugation is to use the butterfly centrifugal machine to carry out centrifugation from chilli extract.
7. according to the described process of producing capsaicine crystals from chilli extract of claim 2, it is characterized in that the described centrifugation of step 1) is to use the butterfly centrifugal machine to carry out centrifugation, extract enters in the butterfly seperator with 11～16kg/min speed and separates.
8. according to the described process of producing capsaicine crystals from chilli extract of claim 2, it is characterized in that: the described centrifugation of step 3) is to use the butterfly centrifugal machine to carry out centrifugation, and the extract of washing, purifying enters in the butterfly seperator with 20～22kg/min speed and separates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710057470A CN101057660B (en) | 2007-05-28 | 2007-05-28 | Technique method for producing capsicine crystal from capsicum oleoresin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710057470A CN101057660B (en) | 2007-05-28 | 2007-05-28 | Technique method for producing capsicine crystal from capsicum oleoresin |
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| Publication Number | Publication Date |
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| CN101057660A CN101057660A (en) | 2007-10-24 |
| CN101057660B true CN101057660B (en) | 2010-05-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516110B (en) * | 2011-12-07 | 2014-04-23 | 天津大学 | High-purity capsaicin compound refining crystallization method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1650747A (en) * | 2005-01-07 | 2005-08-10 | 河北晨光天然色素有限公司 | Industrial method for raising chilli extract Iuality |
| CN1680285A (en) * | 2005-01-07 | 2005-10-12 | 天津金钰生物科技有限公司 | Industrial production of natural capsaicin crystal by molecular distilling and washing method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1650747A (en) * | 2005-01-07 | 2005-08-10 | 河北晨光天然色素有限公司 | Industrial method for raising chilli extract Iuality |
| CN1680285A (en) * | 2005-01-07 | 2005-10-12 | 天津金钰生物科技有限公司 | Industrial production of natural capsaicin crystal by molecular distilling and washing method |
Non-Patent Citations (2)
| Title |
|---|
| 董静等.辣椒中辣椒碱和辣椒红色素的提取及应用.食品科技 2.2006,(2),60-62. |
| 董静等.辣椒中辣椒碱和辣椒红色素的提取及应用.食品科技 2.2006,(2),60-62. * |
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