CN103421341A - Method for increasing color value of capsicum haematochrome - Google Patents
Method for increasing color value of capsicum haematochrome Download PDFInfo
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- CN103421341A CN103421341A CN2012101639761A CN201210163976A CN103421341A CN 103421341 A CN103421341 A CN 103421341A CN 2012101639761 A CN2012101639761 A CN 2012101639761A CN 201210163976 A CN201210163976 A CN 201210163976A CN 103421341 A CN103421341 A CN 103421341A
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- capsanthin
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Abstract
The invention discloses a method for increasing color value of capsicum haematochrome. The method is as below: first dissolving capsicum haematochrome with acetone; adding a sodium hydroxide aqueous solution for saponification; then removing the slag and concentrating; dissolving the capsicum haematochrome obtained from concentration with 6# solvent naphtha; washing the mixture with brine; and finally concentrating to obtain refined capsicum haematochrome. The method first utilizes saponification to remove residual grease in capsicum haematochrome, then employs brine washing to remove other impurities in the capsicum haematochrome, so as to refine the capsicum haematochrome and increase purity and color interval of the capsicum haematochrome. The method can thoroughly remove impurity components in the capsicum haematochrome, so as to obviously improve quality of the capsicum haematochrome. After long term dispose, the capsicum haematochrome does not occur micelle deposition; and capsicum haematochrome stored at low temperature still has good fluidity, and has color value increased by 2-3 times and color value yield higher than 95%.
Description
Technical field
The present invention relates to a kind of process for purification of capsanthin, especially a kind of method that improves capsanthin look valency.
Background technology
Capsanthin is garnet paste liquid, main component has Capsorubin, capsorubin, zeaxanthin and carotene etc., it is the fat-soluble tetraterpenes compound of a class extracted from solanaceae plant pepper, it is strong coloring force not only, safety non-toxic, and there is very high nutritive value, be widely used in the industries such as food, medicine, makeup.
The conventional production method of capsanthin is first with organic solvent, from chilli, to extract the capsanthin crude product containing pungent, then, through taking off the processes such as peppery, de-residual, produce the capsanthin finished product.The pigment total yield of the method is high, but the look valency of product is lower, and foreign matter content is high, after the long-time placement of pigment, the micelle precipitation easily occurs, easily occurs solidification phenomenon during low-temp storage, and the pigment quality is unstable.
The patent of invention that application publication number is CN 101831198 A has been announced " a kind of preparation method of capsanthin ", it first obtains the pigment leach liquor with leaching agent extracting capsicum powder, the pigment leach liquor is concentrated, de-peppery again, finally adopt the method for chromatographic separation, obtain the capsanthin finished product.It utilizes chromatographic separation that capsanthin is purified, but the method treatment capacity of chromatographic separation is little, is difficult for large-scale production.
Patent of invention that application publication number is CN 101096327 A has been announced " a kind of take low-molecular-weight fatty acid remove the method for phosphatide in capsanthin as entrainment agent ", it first makes the capsanthin raw material with solvent method, take low-molecular-weight fatty acid as entrainment agent carries out supercritical carbon dioxide extraction to the capsanthin raw material again, make the capsanthin finished product.It utilizes the supercritical methanol technology capsanthin, but the cost compare that supercritical process is processed is high, and the scale operation operability is not strong.
In order to improve the quality of capsanthin, reduce the foreign matter content in capsanthin, obtain the better capsanthin of purity higher stability, urgently invention can be by the further refining method of capsanthin.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that is suitable for the raising capsanthin look valency of suitability for industrialized production, to obtain highly purified capsanthin.
For solving the problems of the technologies described above, the technical solution used in the present invention is: it is first by the capsanthin acetone solution, then adds the aqueous sodium hydroxide solution saponification, then removes slag rear concentrated; The concentrated capsanthin obtained is dissolved with the 6# solvent oil, then, with the salt solution washing, finally concentrate and obtain refining capsanthin.
The further processing step of the present invention is: dissolve capsanthin in acetone (1), obtains lysate;
(2) in lysate, add the aqueous sodium hydroxide solution that pigment weight 30～50%, concentration are 30～50wt% to carry out saponification, obtain mixed solution;
(3) above-mentioned mixed solution separation obtains supernatant liquor and slag phase; By supernatant concentration, obtain the refining work in-process of pigment;
(4) the refining work in-process of described pigment dissolve with the 6# solvent oil, then add pigment make with extra care the sodium chloride aqueous solution that 1～2 times of weight of work in-process, concentration are 3wt ‰ to be cleaned, and separation obtains 6# solvent oil reservoir and water layer;
(5) the concentrated solvent of removing of described 6# solvent oil reservoir, obtain refining capsanthin.
In step of the present invention (1), capsanthin is joined in the acetone of 3～5 times of pigment weight, stir 15～20min, obtain lysate.The purity requirement of described acetone is more than 95wt%.
Saponification in step of the present invention (2) is: after adding aqueous sodium hydroxide solution in lysate, at 25～30 ℃, stir 30～60min.
In step of the present invention (4), the refining work in-process of described pigment dissolve with the 6# solvent oil of 3～5 times of its weight; With sodium chloride aqueous solution, clean 2～3 times.
Slag in step of the present invention (3) is less than 0.3 with acetone rinsing to bits look valency; Rinse the acetone and supernatant liquor merging of slag after mutually, enter step (4).
The beneficial effect that adopts technique scheme to produce is: the present invention first utilizes saponification, removes residual grease in capsanthin, recycling salt solution washing (saltouing), other impurity in the removal capsanthin; Reach the purpose refining to capsanthin, thereby improved purity and the color range of capsanthin.
The present invention can thoroughly remove impurity component in capsanthin, the quality of capsanthin be improved significantly; After long-time the placement, capsanthin not there will be the micelle precipitation, and the mobility of low temperature storage capsanthin is still good, and the look valency can improve 2～3 times, and look valency yield is more than 95%.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment 1: the processing step of the method for this raising capsanthin look valency is as follows.
(1) dissolve: get capsanthin 300g, raw material look valency 100.2, add the acetone that 900g, purity are 96wt%, stirs 15min pigment is all dissolved, and obtains lysate.
(2) saponification: add the sodium hydroxide solution 150g that concentration is 40wt% in lysate, 25 ℃ are stirred 40min, obtain mixed solution.
(3) separate: by above-mentioned mixed solution centrifugation, obtain supernatant liquor and slag phase; By acetone rinsing slag phase until bits look valency is 0.25.
(4) concentrated: merge supernatant liquor and rinse the acetone of slag phase, concentrating under reduced pressure, obtain the refining work in-process 150g of pigment.
(5) washing: make with extra care the 6# solvent oil that adds 600g in work in-process to the 150g pigment, be stirred to whole dissolvings, add the sodium chloride aqueous solution that the 200g massfraction is 3 ‰, stir, then separate and obtain 6# solvent oil reservoir and water layer; Again add the sodium chloride aqueous solution that the 200g massfraction is 3 ‰ in 6# solvent oil reservoir, rear separation stirs.
(6) finished product: by 6# solvent oil reservoir reduction vaporization, obtain refining capsanthin finished product 114g.Finished product unit's look valency 250.6, look valency yield 95%.
Embodiment 2: the processing step of the method for this raising capsanthin look valency is as follows.
(1) get capsanthin 300g, raw material unit's look valency 60.8, add the acetone that 1000g, purity are 98wt%, stirs 20min pigment is all dissolved, and obtains lysate.
(2) add the sodium hydroxide solution 150g that concentration is 50wt%, 30 ℃ are stirred 50min, obtain mixed solution.
(3) above-mentioned mixed solution is centrifugal, obtain supernatant liquor and slag phase, with acetone rinsing slag to bits look valency, be 0.18.
(4) merge supernatant liquor and rinse the acetone of slag phase, concentrating under reduced pressure, obtain the refining work in-process 120g of pigment.
(5) make with extra care to the 120g pigment 6# solvent oil that adds 500g in work in-process, be stirred to whole dissolvings, the sodium chloride aqueous solution that is 3 ‰ with the 180g massfraction cleans 3 times, then separates and obtains 6# solvent oil reservoir and water layer.
(6), by 6# solvent oil reservoir reduction vaporization, obtain refining capsanthin finished product 96g.Finished product unit's look valency 182.3, look valency yield 96%.
Embodiment 3: the processing step of the method for this raising capsanthin look valency is as follows.
(1) dissolve: get capsanthin 300g, raw material look valency 76.4, add the acetone that 1500g, purity are 97wt%, stirs pigment is all dissolved, and obtains lysate.
(2) saponification: add the sodium hydroxide solution 100g that concentration is 30wt% in lysate, 27 ℃ are stirred 60min, obtain mixed solution.
(3) separate: by above-mentioned mixed solution centrifugation, obtain supernatant liquor and slag phase; By acetone rinsing slag phase until bits look valency is 0.20.
(4) concentrated: merge supernatant liquor and rinse the acetone of slag phase, concentrating under reduced pressure, obtain the refining work in-process 130g of pigment.
(5) washing: make with extra care the 6# solvent oil that adds 390g in work in-process to the 130g pigment, be stirred to whole dissolvings, add the sodium chloride aqueous solution that the 260g massfraction is 3 ‰, stir, then separate and obtain 6# solvent oil reservoir and water layer.
(6) finished product: by 6# solvent oil reservoir reduction vaporization, obtain refining capsanthin finished product 99g.Finished product unit's look valency 201.6, look valency yield 95%.
Embodiment 4: the processing step of the method for this raising capsanthin look valency is as follows.
(1) get capsanthin 300g, raw material unit's look valency 91.7, add the acetone that 1200g, purity are 98wt%, stirs pigment is all dissolved, and obtains lysate.
(2) add the sodium hydroxide solution 120g that concentration is 35wt%, 30 ℃ are stirred 30min, obtain mixed solution.
(3) above-mentioned mixed solution is centrifugal, obtain supernatant liquor and slag phase, with acetone rinsing slag to bits look valency, be 0.18.
(4) merge supernatant liquor and rinse the acetone of slag phase, concentrating under reduced pressure, obtain the refining work in-process 145g of pigment.
(5) make with extra care to the 145g pigment 6# solvent oil that adds 725g in work in-process, be stirred to whole dissolvings, the sodium chloride aqueous solution that is 3 ‰ with the 145g massfraction cleans 2 times, then separates and obtains 6# solvent oil reservoir and water layer.
(6), by 6# solvent oil reservoir reduction vaporization, obtain refining capsanthin finished product 103g.Finished product unit's look valency 227.5, look valency yield 96%.
Claims (8)
1. a method that improves capsanthin look valency is characterized in that: it is first by the capsanthin acetone solution, then adds the aqueous sodium hydroxide solution saponification, then removes slag rear concentrated; The concentrated capsanthin obtained is dissolved with the 6# solvent oil, then, with the salt solution washing, finally concentrate and obtain refining capsanthin.
2. a kind of method that improves capsanthin look valency according to claim 1, is characterized in that, the processing step of the method is: dissolve capsanthin in acetone (1), obtains lysate;
(2) in lysate, add the aqueous sodium hydroxide solution that pigment weight 30～50%, concentration are 30～50wt% to carry out saponification, obtain mixed solution;
(3) above-mentioned mixed solution separation obtains supernatant liquor and slag phase; By supernatant concentration, obtain the refining work in-process of pigment;
(4) the refining work in-process of described pigment dissolve with the 6# solvent oil, then add pigment make with extra care the sodium chloride aqueous solution that 1～2 times of weight of work in-process, concentration are 3wt ‰ to be cleaned, and separation obtains 6# solvent oil reservoir and water layer;
(5) the concentrated solvent of removing of described 6# solvent oil reservoir, obtain refining capsanthin.
3. a kind of method that improves capsanthin look valency according to claim 2, is characterized in that: in described step (1), capsanthin is joined in the acetone of 3～5 times of pigment weight, stir 15～20min, obtain lysate.
4. a kind of method that improves capsanthin look valency according to claim 3, it is characterized in that: the purity requirement of described acetone is more than 95wt%.
5. a kind of method that improves capsanthin look valency according to claim 2, is characterized in that, the saponification in described step (2) is: after adding aqueous sodium hydroxide solution in lysate, at 25～30 ℃, stir 30～60min.
6. a kind of method that improves capsanthin look valency according to claim 2 is characterized in that: in described step (4), and the 6# solvent oil dissolving of 3～5 times of its weight for the refining work in-process of described pigment.
7. a kind of method that improves capsanthin look valency according to claim 2, is characterized in that: in described step (4), with sodium chloride aqueous solution, clean 2～3 times.
8. improve the method for capsanthin look valency according to described any one of claim 2-7, it is characterized in that: the slag in described step (3) is less than 0.3 with acetone rinsing to bits look valency; Rinse the acetone and supernatant liquor merging of slag after mutually, enter step (4).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642276A (en) * | 2013-12-24 | 2014-03-19 | 云南宏绿辣素有限公司 | Preparation method of high-concentration capsanthin |
| CN103642269A (en) * | 2013-12-27 | 2014-03-19 | 中椒英潮辣业发展有限公司 | Process for extracting paprika red pigment through enzymolysis |
| CN104059379A (en) * | 2014-06-20 | 2014-09-24 | 新疆隆平高科红安种业有限责任公司 | Degumming method for red chilly extract |
| CN106590025A (en) * | 2016-11-29 | 2017-04-26 | 云南瑞宝生物科技股份有限公司 | Method for preparing high color value capsicum red pigment from capsicum extract |
| CN106752072A (en) * | 2016-12-05 | 2017-05-31 | 晨光生物科技集团股份有限公司 | A kind of High color values capsanthin continuous production processes |
| CN109370252A (en) * | 2018-11-23 | 2019-02-22 | 晨光生物科技集团股份有限公司 | A kind of refining methd of capsicum red pigment slag |
| CN113583471A (en) * | 2021-09-17 | 2021-11-02 | 云南博瑞生物科技有限公司 | Method for industrially producing high-quality capsanthin |
| CN114806214A (en) * | 2022-05-17 | 2022-07-29 | 晨光生物科技集团股份有限公司 | Preparation method of capsanthin with different color tones |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642276A (en) * | 2013-12-24 | 2014-03-19 | 云南宏绿辣素有限公司 | Preparation method of high-concentration capsanthin |
| CN103642269A (en) * | 2013-12-27 | 2014-03-19 | 中椒英潮辣业发展有限公司 | Process for extracting paprika red pigment through enzymolysis |
| CN104059379A (en) * | 2014-06-20 | 2014-09-24 | 新疆隆平高科红安种业有限责任公司 | Degumming method for red chilly extract |
| CN106590025A (en) * | 2016-11-29 | 2017-04-26 | 云南瑞宝生物科技股份有限公司 | Method for preparing high color value capsicum red pigment from capsicum extract |
| CN106752072A (en) * | 2016-12-05 | 2017-05-31 | 晨光生物科技集团股份有限公司 | A kind of High color values capsanthin continuous production processes |
| 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 |
| CN109370252A (en) * | 2018-11-23 | 2019-02-22 | 晨光生物科技集团股份有限公司 | A kind of refining methd of capsicum red pigment slag |
| CN109370252B (en) * | 2018-11-23 | 2020-02-21 | 晨光生物科技集团股份有限公司 | Refining method of capsanthin pigment residue |
| CN113583471A (en) * | 2021-09-17 | 2021-11-02 | 云南博瑞生物科技有限公司 | Method for industrially producing high-quality capsanthin |
| CN113583471B (en) * | 2021-09-17 | 2023-04-07 | 云南博瑞生物科技有限公司 | Method for industrially producing high-quality capsanthin |
| CN114806214A (en) * | 2022-05-17 | 2022-07-29 | 晨光生物科技集团股份有限公司 | Preparation method of capsanthin with different color tones |
| CN114806214B (en) * | 2022-05-17 | 2024-01-30 | 晨光生物科技集团股份有限公司 | Preparation method of capsanthin with different colors |
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