CN101940289A - Method for separating discolored chili extract from chili pigment in crude products of chili extract - Google Patents
Method for separating discolored chili extract from chili pigment in crude products of chili extract Download PDFInfo
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- CN101940289A CN101940289A CN2010102462613A CN201010246261A CN101940289A CN 101940289 A CN101940289 A CN 101940289A CN 2010102462613 A CN2010102462613 A CN 2010102462613A CN 201010246261 A CN201010246261 A CN 201010246261A CN 101940289 A CN101940289 A CN 101940289A
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Abstract
The invention provides a method for separating discolored chili extract from chili pigment in crude products of chili extract, which relates to a process for separating discolored chili extract from chili pigment. The method comprises the following steps: (1) soaking macroporous molecular adsorption resin by ethanol; (2) fully dissolving the crude products of chili extract by the ethanol; (3) injecting the chili extract solution into a chromatography column in which the molecular adsorption resin is filled, and standing; (4) enabling the solution to flow out of the chromatography column; (5) leaching by clear water; (6) eluting the chromatography column by the ethanol solution; (7) mixing the eluent and the ethanol effluent liquid, and carrying out decompression concentration to obtain the discolored chili extract; (8) eluting the chromatography column by normal hexane; and (9) collecting the eluent in the step (8), and carrying out decompression concentration to obtain the chili pigment without pungency. The invention overcomes the defects in the process of producing the discolored chili extract by activated carbon and diatomite, realizes the large-scale industrialized production of the discolored chili extract, can recycle the chili pigment to refine high-grade chili pigment, and is a cleaning project with low energy consumption and high efficiency.
Description
Technical field
The present invention relates to a kind of chemical technology, be specifically related to a kind of technology of separating decolouring chilli extract and capsochrome.
Background technology
Produce in the process of decolouring chilli extract at present, adopt activated carbon and diatomite is that adsorbent separates pigment more.But the chromatograph post that above two kinds of adsorbents are made can not reclaim pigment, and mass transfer rate is slow, and column efficiency is poor, and the rate of recovery is low, and solvent consumption is big, is difficult to realize large-scale industrialization production, and adsorbent can not reclaim use, greatly contaminated environment.
Adopt in the method for chromatographic column refining chilli pigment, Chinese patent CN1392201A utilizes in the macroporous absorbent resin separating pepper element, exists solvent consumption big, trivial operations, and yield is low, is not applied in the production of decolouring chilli extract.
Summary of the invention
The purpose of this invention is to provide the method for separating decolouring chilli extract and capsochrome in a kind of chilli extract crude product, the present invention overcomes the shortcoming with active carbon and diatomite production decolouring chilli extract, realize large-scale industrial production decolouring chilli extract and can reclaim capsochrome, making with extra care out high-quality capsochrome, is the cleaning project of low-consumption high-efficiency.
Separate the method for decolouring chilli extract and capsochrome in the chilli extract crude product of the present invention, operate according to following steps:
(1) with concentration 95% alcohol immersion macropore Molecular Adsorption resin, clean up in the chromatographic column of packing into standby with clear water then;
(2) be that 70%～90% ethanol fully dissolves the chilli extract crude product with concentration;
(3) chilli extract solution is injected the chromatographic column of the Molecular Adsorption resin of packing into, left standstill 2 hours～4 hours;
(4) by flow velocity 20 milliliters/minute～50 milliliters/minute allow solution flow out chromatographic column;
(5) with clear water drip washing chromatographic column, with 50 milliliters/minute～85 milliliters/minute flow velocity flows out chromatographic column, and will flow out liquid and discard;
(6) be in 50%～80% ethanolic solution elution chromatography post with concentration, and with 10 milliliters/minute～50 milliliters/minute flow velocity flow out chromatographic column, be eluted to and flow out liquid and do not have till the pungent;
(7) collect the eluent of (six) step and merge with above-mentioned (four) step ethanol stream fluid, decompression concentrates and obtains the chilli extract that decolours;
(8) with n-hexane elution chromatography post, with 10 milliliters/minute～50 milliliters/minute flow velocity flows out, and is close to colourless until flowing out liquid;
(9) collect eluent in the step (eight), decompression concentrates, and obtains not having the capsochrome of pungent.
Further, separate the method for decolouring chilli extract and capsochrome in the chilli extract crude product of the present invention, also have following characteristics, in (two) step, dissolve the chilli extract crude product of 1～5 gram in the ethanol of per 100 milliliters.
Used resin is a HPD-A macropore Molecular Adsorption resin.
The mass ratio of resin and chilli extract ethanolic solution is 1: 10 in (three) step.
Used chromatographic column specification is diameter 30cm * height 300cm.
Decompression concentrates in (seven) step or (nine) step, adopts the vacuum decker group, and heating-up temperature is 55 ℃, and vacuum is 0.1mpa.
The present invention is to produce the product of capsicum red pigment, the quality thickness, the dark brown chilli extract crude product of color is a raw material, with HPD-100A type macropore Molecular Adsorption resin is adsorbent, with 70%～90% ethanolic solution is solvent, absorption capsochrome and other impurity in chromatographic column flows out liquid and concentrates through decompression and obtains the chilli extract that decolours, and stays pigment in the post and concentrates after through the n-hexane wash-out and can obtain high-quality capsochrome.
It is of the present invention that to provide a kind of be adsorbent with macropore Molecular Adsorption resin, the method of from the chilli extract crude product, separating decolouring chilli extract and capsochrome, the mode of production can overcome the shortcoming with active carbon and diatomite production decolouring chilli extract, realize large-scale industrial production decolouring chilli extract and can reclaim capsochrome, making with extra care out high-quality capsochrome, is the cleaning project of low-consumption high-efficiency.
The present invention compared with prior art, can overcome present technology deficiency, the present invention takes macropore Molecular Adsorption resin to come adsorpting pigment, and capsochrome is separated with capsicim, obtains high-quality decolouring chilli extract and capsicum red pigment simultaneously, wash-out is easy, the efficient height, with short production cycle, overcome the shortcoming that active carbon can not reclaim pigment, resin can be regenerated to produce and be used, and reduces production costs greatly.
The specific embodiment
With illustrated embodiments the present invention is done detailed explanation below.
Embodiment one
The HPD-100A macropore Molecular Adsorption resin that adds 20kg in chromatographic column uses the ethanol (95%) of 50L to soak 2 hours, back clear water wash clean, triplicate.With the chilli extract crude product of the ethanol of 20L70%～90% dissolving, inject chromatographic column, absorption is 2 hours under the room temperature, puts into solution and collects with certain flow rate, with clear water drip washing chromatographic column, discards outflow liquid.Use 50% ethanolic solution elution chromatography post again, till outflow liquid does not have pungent.Merging twice and flow out liquid, is 0.06mpa with the vacuum pressure, 55 ℃ of temperature, and decompression concentrates, and reclaims ethanol, obtains the chilli extract that decolours.Use n-hexane elution chromatography post again, till outflow liquid was closely colourless, vacuum pressure was 0.08mpa, and temperature is 40 ℃, and decompression concentrates flows out liquid, and the recovery n-hexane obtains capsicum red pigment.
Embodiment two
(No. 1 chilli extract look valency is 10 with No. 1 chilli extract; Capsaicin content is 6.6%) 1kg is dissolved in the ethanolic solution of 40L90%, and chilli extract solution is injected chromatographic column, leaves standstill 3 hours, open the chromatographic column valve by chilli extract solution with 50 milliliters/minute flow out chromatographic column, and collect and flow out liquid.Solution flows out and finishes, with clear water drip washing chromatographic column, with 80 milliliters/minute outflow chromatographic column, drip washing is bordering on colourlessly to flowing out liquid, will flow out liquid and discard, the ethanol elution chromatographic column with 50%, and with 20 milliliters/minute outflow chromatographic column, being eluted to outflow liquid does not have till the pungent.Collect eluent and with the first time chilli extract ethanol collect liquid and merge, decompression concentrates, and reclaims ethanol, chilli extract 762.1g obtains decolouring.With n-hexane elution chromatography post again, with 20 milliliters/minute flow out chromatographic column, be bordering on colourlessly until flowing out liquid, collect eluent, decompression concentrates reclaims n-hexane, obtains not having the capsochrome 185g of capsicum look, press the detection of GB10783-2008 method, and its result is as follows:
Chilli extract look valency E
1% 1cm460nml
Capsaicin content: 8.4
The capsicim rate of recovery is: 96.9%
Capsochrome look valency E
1% 1cm460nm 50
The capsochrome rate of recovery is: 92.5%
Embodiment three
(No. 2 chilli extract look valency is 15 with No. 2 chilli extracts; Capsaicin content is 4.2%) 2kg is dissolved in 80% ethanolic solution of 60L, and chilli extract solution is injected chromatographic column, left standstill 4 hours.Open the chromatographic column valve by chilli extract solution with 40 milliliters/minute flow out chromatographic column, and collect and flow out liquid, wait solution to flow out and finish, with clear water drip washing chromatographic column and with 80 milliliters/minute flow out, drip washing is bordering on colourlessly to flowing out liquid, will flow out liquid and discard.With 70% ethanolic solution elution chromatography post, be eluted to and flow out liquid and do not have till the pungent, collect eluent and with the first time chilli extract ethanol collect liquid and merge, decompression, to concentrate the chilli extract that obtains decolouring be 1.02kg.With n-hexane elution chromatography post, to 30 milliliters/minute flow out chromatographic column, be bordering on colourlessly until flowing out liquid, collect the n-hexane eluent, decompression concentrates, and reclaims n-hexane, obtains capsicum red pigment 524.7g, press GB10783-2008 standard method detection, and the result is as follows:
Chilli extract look valency E
1% 1cm460nm=1
Capsaicin content: 8.2
The capsicim rate of recovery is: 98.1%
Capsochrome look valency E
1% 1cm460nm=55
The capsochrome rate of recovery is: 96.2%
Above embodiment is the more preferably specific embodiment a kind of of the present invention, the common variation that those skilled in the art carry out in the technical program scope and replace and should be included in protection scope of the present invention.
Claims (6)
1. separate the method for decolouring chilli extract and capsochrome in the chilli extract crude product, it is characterized in that, operate according to following steps:
(1) with concentration 95% alcohol immersion macropore Molecular Adsorption resin, clean up in the chromatographic column of packing into standby with clear water then;
(2) be that 70%～90% ethanol fully dissolves the chilli extract crude product with concentration;
(3) chilli extract solution is injected the chromatographic column of the Molecular Adsorption resin of packing into, left standstill 2 hours～4 hours;
(4) by flow velocity 20 milliliters/minute～50 milliliters/minute allow solution flow out chromatographic column;
(5) with clear water drip washing chromatographic column, with 50 milliliters/minute～85 milliliters/minute flow velocity flows out chromatographic column, and will flow out liquid and discard;
(6) be in 50%～80% ethanolic solution elution chromatography post with concentration, and with 10 milliliters/minute～50 milliliters/minute flow velocity flow out chromatographic column, be eluted to and flow out liquid and do not have till the pungent;
(7) collect the eluent of (six) step and merge with above-mentioned (four) step ethanol stream fluid, decompression concentrates and obtains the chilli extract that decolours;
(8) with n-hexane elution chromatography post, with 10 milliliters/minute～50 milliliters/minute flow velocity flows out, and is close to colourless until flowing out liquid;
(9) collect eluent in the step (eight), decompression concentrates, and obtains not having the capsochrome of pungent.
2. separate the method for decolouring chilli extract and capsochrome according to claim 1 in the chilli extract crude product, it is characterized in that, in (two) step, dissolve the chilli extract crude product of 1～5 gram in the ethanol of per 100 milliliters.
3. separate the method for decolouring chilli extract and capsochrome according to claim 1 in the chilli extract crude product, it is characterized in that used resin is a HPD-A macropore Molecular Adsorption resin.
4. as separating the method for decolouring chilli extract and capsochrome in the chilli extract crude product as described in the claim 2, it is characterized in that the mass ratio of resin and chilli extract ethanolic solution is 1: 10 in (three) step.
5. separate the method for decolouring chilli extract and capsochrome according to claim 1 in the chilli extract crude product, it is characterized in that used chromatographic column specification is diameter 30cm * height 300cm.
6. separate the method for decolouring chilli extract and capsochrome according to claim 1 in the chilli extract crude product, it is characterized in that, decompression concentrates in (seven) step or (nine) step, adopts the vacuum decker group, and heating-up temperature is 55 ℃, and vacuum is 0.1mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102462613A CN101940289B (en) | 2010-08-06 | 2010-08-06 | Method for separating discolored chili extract from chili pigment in crude products of chili extract |
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| CN2010102462613A CN101940289B (en) | 2010-08-06 | 2010-08-06 | Method for separating discolored chili extract from chili pigment in crude products of chili extract |
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| CN101940289B CN101940289B (en) | 2012-05-30 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102113661A (en) * | 2011-01-31 | 2011-07-06 | 新疆隆平高科弘安天然色素有限公司 | Method for recovering pungency substances in chilli powder crushing process |
| 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 |
| CN102715482A (en) * | 2012-06-19 | 2012-10-10 | 许秋雁 | Method for producing decolorized aqueous chilli extract |
| CN103351955A (en) * | 2013-07-17 | 2013-10-16 | 晨光生物科技集团股份有限公司 | Production method of colorless chilli extract |
| CN105505225A (en) * | 2015-12-29 | 2016-04-20 | 云南宏绿辣素有限公司 | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin |
| CN105566944A (en) * | 2015-12-28 | 2016-05-11 | 广西恒得润生物科技有限公司 | Method for separating decolorized chilli extract and chili pigments from chilli extract crude product |
| CN109874964A (en) * | 2018-12-27 | 2019-06-14 | 晨光生物科技集团股份有限公司 | A kind of production method and its decoloration chilli extract of the chilli extract that decolourizes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392201A (en) * | 2002-07-18 | 2003-01-22 | 中山大学 | Extracting and purifying method for natural capsanthin pigment |
| CN101333341A (en) * | 2008-06-30 | 2008-12-31 | 山东轻工业学院 | Technique of preparing capsanthin pigment |
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2010
- 2010-08-06 CN CN2010102462613A patent/CN101940289B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392201A (en) * | 2002-07-18 | 2003-01-22 | 中山大学 | Extracting and purifying method for natural capsanthin pigment |
| CN101333341A (en) * | 2008-06-30 | 2008-12-31 | 山东轻工业学院 | Technique of preparing capsanthin pigment |
Non-Patent Citations (2)
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| 《中国食品添加剂》 20021231 任召言等 辣椒精的精制及辣椒素的HPLC测定 75-76，86 1-6 , 第01期 2 * |
| 《贵州林业科技》 20011130 张彦雄等 辣椒碱类化合物及脱色辣椒精生产技术研究 1-8，18 1-6 第29卷, 第04期 2 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102113661A (en) * | 2011-01-31 | 2011-07-06 | 新疆隆平高科弘安天然色素有限公司 | Method for recovering pungency substances in chilli powder crushing process |
| 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 |
| CN102715482A (en) * | 2012-06-19 | 2012-10-10 | 许秋雁 | Method for producing decolorized aqueous chilli extract |
| CN103351955A (en) * | 2013-07-17 | 2013-10-16 | 晨光生物科技集团股份有限公司 | Production method of colorless chilli extract |
| CN103351955B (en) * | 2013-07-17 | 2015-02-25 | 晨光生物科技集团股份有限公司 | Production method of colorless chilli extract |
| CN105566944A (en) * | 2015-12-28 | 2016-05-11 | 广西恒得润生物科技有限公司 | Method for separating decolorized chilli extract and chili pigments from chilli extract crude product |
| CN105566944B (en) * | 2015-12-28 | 2018-03-02 | 广西恒得润生物科技有限公司 | The method that decolouring chilli extract and capsochrome are separated in chilli extract crude product |
| CN105505225A (en) * | 2015-12-29 | 2016-04-20 | 云南宏绿辣素有限公司 | Method for separating capsaicin and pigment in capsicum oleoresin with high capsaicin content and refining capsaicin |
| CN109874964A (en) * | 2018-12-27 | 2019-06-14 | 晨光生物科技集团股份有限公司 | A kind of production method and its decoloration chilli extract of the chilli extract that decolourizes |
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| CN101940289B (en) | 2012-05-30 |
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Application publication date: 20110112 Assignee: GUANGXI HENGDERUN BIOLOGICAL SCIENCE & TECHNOLOGY CO., LTD. Assignor: Yang Hongmei Contract record no.: 2013450000066 Denomination of invention: Method for separating discolored chili extract from chili pigment in crude products of chili extract Granted publication date: 20120530 License type: Exclusive License Record date: 20130807 |
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