CN101831198A - Preparation method of capsanthin - Google Patents
Preparation method of capsanthin Download PDFInfo
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- CN101831198A CN101831198A CN 201010190564 CN201010190564A CN101831198A CN 101831198 A CN101831198 A CN 101831198A CN 201010190564 CN201010190564 CN 201010190564 CN 201010190564 A CN201010190564 A CN 201010190564A CN 101831198 A CN101831198 A CN 101831198A
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Abstract
The invention provides a preparation method of capsanthin, which comprises the following steps of: a) mixing chili powder and a leaching agent in a continuous extractor to obtain a pigment extract; b) performing vacuum concentration on the pigment extract to obtain pigment concentrated solution; and c) removing the sharp taste of the pigment concentrated solution and then performing chromatographic separation to obtain the capsanthin. The preparation method of the capsanthin uses the continuous extractor to ensure that the capsanthin is extracted more sufficiently and the extraction process can be operated continuously, so the preparation method is suitable for industrial preparation of the capsanthin. Besides, the preparation method of the capsanthin also uses a chromatographic separation technique to separate orange and yellow pigments such as beta-carotene, zeaxanthin and the like out from the capsanthin so as to improve the concentration of red pigments in the capsanthin and improve the absorbance ratio of the capsanthin.
Description
Technical field
The present invention relates to the foodstuff additive field, be specifically related to a kind of preparation method of capsanthin.
Background technology
The composition that capsanthin is made up of multiple natural pigment, its composition are Capsorubin (Capsanthin), capsorubin (Capsorubin), β-Hu Luobusu, zeaxanthin (Zeaxanthin) and latent capsanthin (Cryptocapsin).Capsanthin is not only bright-colored, nontoxic, and has oxidation resistant effect, is widely used in food-processing and makeup and makes the field.
The preparation technology of traditional capsanthin is: capsicum is pulverized obtain the capsicum powder earlier, by the capsanthin in the solvent extraction capsicum powder, obtain the pigment leach liquor, and then removing pungent in the described pigment leach liquor by ethanol, sodium hydroxide solution equal solvent, the solution concentration that will remove at last after the pungent obtains capsanthin.
The capsanthin of prior art for preparing contains a large amount of β-Hu Luobusus, and orange and xanthein such as zeaxanthin reduced the absorption ratio of capsanthin, and the color of the low more explanation capsanthin of the absorption ratio of capsanthin levels off to more orange-yellow.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation method of capsanthin, prepares absorption ratio greater than 1.00 capsanthin.
In order to overcome the above problems, the invention provides a kind of preparation method of capsanthin, comprising: a) capsicum powder and leaching agent are mixed in the continous way leacher, obtain the pigment leach liquor;
B) described pigment leach liquor is carried out vacuum concentration, obtain pigment concentrate;
C) carry out chromatographic separation after described pigment concentrate is deviate from pungent, obtain capsanthin.
Preferred step c) is specially:
C1) pigment concentrate that step b) is obtained and alcoholic solvent are 1: 2～6 to mix according to volume ratio, slough the pungent of described concentrated solution;
C2) with step c1) pigment concentrate of deviating from pungent that obtains carries out silica gel column chromatography, with the described silicagel column of sherwood oil drip washing, obtains the sherwood oil leacheate earlier, uses the described silicagel column of acetone drip washing again, obtains the acetone leacheate;
C3) with step c2) the acetone leacheate that obtains concentrates, and obtains capsanthin.
Preferably, described pigment leaching agent is the alkane that contains 4～7 carbon.
Preferably, described continous way leacher is: flat rotary extractor, loop type extractor, satellite-type leacher or track type leacher.
Preferably, the pressure of described vacuum concentration be-0.03MPa～-0.05MPa.
Preferably, described sherwood oil and silicagel column are 2～4: 1 by volume.
Preferably, described acetone and silicagel column are 2～4: 1 by volume.
Preferably, the flow velocity of described sherwood oil drip washing is 0.3～1 column volume/h.
Preferably, the flow velocity of described acetone drip washing is 0.3～1 column volume/h.
Preferably, described alcoholic solvent is the alcoholic solvent that contains 2～4 carbon.
The invention provides a kind of preparation method of capsanthin, comprising: a) capsicum powder and leaching agent are mixed in the continous way leacher, obtain the pigment leach liquor; B) described pigment leach liquor is carried out vacuum concentration, obtain pigment concentrate; C) carry out chromatographic separation after described pigment concentrate is deviate from pungent, obtain capsanthin.The preparation method of capsanthin provided by the invention has used the continous way leacher, and it is more abundant to make that capsanthin leaches, but and the leaching process operate continuously, be fit to the preparation of industrialization of capsanthin.The preparation method of capsanthin provided by the invention has also used the chromatographic separation technology in addition, orange and xanthein such as β-Hu Luobusu and zeaxanthin is separated from capsanthin, improve the red pigments concentration in the capsanthin, improved the absorption ratio of capsanthin.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiments of the invention are described, but should be appreciated that just restriction of these descriptions for further specifying the features and advantages of the present invention rather than patent of the present invention being required.
The topmost performance index of capsanthin are that the look valency is that absorbancy and tone are absorption ratio A470nm/A454nm.Described absorption ratio is meant the ratio of the absorbancy of capsanthin under the radiation of visible light of absorbancy under the 470nm radiation of visible light and 454nm.The color of capsanthin levels off to pure red more, and absorption ratio is big more.Because Capsorubin and capsorubin in the capsanthin are red pigments, β-Hu Luobusu and zeaxanthin are orange pigment and xanthein, so the concentration ratio of red pigments and xanthein is big more in the capsanthin, capsanthin levels off to pure red more, absorption ratio is big, otherwise then capsanthin levels off to yellow, and absorption ratio is little.Generally the absorption ratio of capsanthin is 0.94～1.00, the method purpose for preparing capsanthin provided by the invention is exactly in order to improve the concentration of red pigments in the capsanthin, orange pigment and xanthein are separated from capsanthin, improved the absorption ratio of capsanthin.
The invention provides a kind of preparation method of capsanthin, comprising:
A) capsicum powder and leaching agent are mixed in the continous way leacher, obtain the pigment leach liquor;
B) described pigment leach liquor is carried out vacuum concentration, obtain pigment concentrate;
C) carry out chromatographic separation after described pigment concentrate is deviate from pungent, obtain capsanthin.
According to the present invention, at first that capsicum is dry under 30 ℃～50 ℃, remove the moisture in the capsicum; Then chillies is pulverized, obtained the capsicum powder.The present invention preferably uses the capsicum skin of red pepper to prepare powder as main raw material, in addition can also be with the operation of extracting capsanthin again after the granulation of capsicum powder.The capsicum powder is delivered into the inside of continous way leacher by the auger on continous way leacher top, in course of conveying, the leaching agent and the capsicum powder uniform mixing of the pre-jet pipe ejection of the solvent that is connected with auger, obtain mixed slurry, described mixed slurry enters the inside of continous way leacher, leaching agent is separated the pigment in the capsicum powder, obtain the pigment leach liquor, described pigment leach liquor flows out by the leach liquor collector of continous way leacher.
Flat rotary extractor, loop type extractor, satellite-type leacher or track type leacher that continous way leacher used herein can be known for the field personnel, the present invention preferably uses flat rotary extractor, the leaching agent that the present invention uses is the alkane that contains 4～7 carbon atoms, preferably uses normal hexane.The spray temperature of described normal hexane can be 40 ℃～50 ℃, and spray flux can be 1000L/h～1500L/h.
According to the present invention, described pigment leach liquor is carried out vacuum concentration operation, the pressure of described vacuum concentration is preferably-0.03MPa～-0.05MPa, obtain pigment concentrate, the present invention does not do qualification to employed spissated equipment.Pigment concentrate and alcoholic solvent are preferably 1: 2～6, more preferably 1: 3～5 mixing according to volume ratio.Mixed solution is stirred 0.5h～4 down at 40 ℃～60 ℃, leave standstill the back layering, the upper strata is an alcoholic solvent, and lower floor is a pigment concentrate.Alcoholic solvent can extract the peppery element of capsaicine, dihydro in the pigment concentrate, fall the material that the peppery element of dihydro etc. produces pungent.After sloughing spicy substance, remove the alcoholic solvent on upper strata,, obtain sloughing the pigment concentrate of spicy substance lower floor's solution concentration.Described alcoholic solvent can be the alcoholic solvent of 2～4 carbon well known in the art, and as ethanol, propyl alcohol, butanols, Virahol etc., the present invention preferably uses ethanol to slough the material that produces pungent.
The pigment concentrate of sloughing spicy substance is carried out chromatographic separation.Contain Capsorubin, capsorubin, β-Hu Luobusu and zeaxanthin etc. in the described pigment concentrate of sloughing spicy substance.According to the present invention, the stationary phase that described chromatographic separation is used can be as silica gel, also can be aluminum oxide, magnesium oxide.The present invention preferably uses silica gel as stationary phase, and the specification of the silica gel that the present invention uses includes but not limited to 100-200 order, 200-300 order, and described silica gel and the described pigment concentrate of sloughing pungent are preferably 5～15: 1 by volume.
According to the present invention, the detailed process of chromatographic separation is: the pigment concentrate that will slough spicy substance earlier injects silicagel column, use sherwood oil drip washing on silicagel column earlier, obtain the sherwood oil leacheate, contain orange and xantheins such as β-Hu Luobusu and zeaxanthin in the described sherwood oil leacheate.Use acetone drip washing on silicagel column then, obtain the acetone leacheate, contain red pigments such as Capsorubin and capsorubin in the acetone leacheate.Sherwood oil and silica gel are preferably 2～4 according to volume ratio: 1, and acetone and silica gel are preferably 2～4 according to volume ratio: 1, the rate of flow in rinse of sherwood oil and acetone all is preferably 0.3～1 column volume/h.Described acetone leacheate is concentrated, spissated mode can be vacuum concentration again, also can be for normal pressure concentrate, and the present invention preferably uses vacuum concentration, and pressure is preferably-0.03MPa～-0.05MPa.The wine-colored oily liquids that obtains after concentrating is capsanthin.
Below set forth technical scheme of the present invention by specific embodiment.
Embodiment 1:
Get Xinjiang red pepper skin 2000kg, pulverize also and obtain the pigment leach liquor with the continuous leacher lixiviate of hoirzontally rotating after the granulation, will get pigment concentrate 120kg behind the leach liquor vacuum concentration again, the pressure of vacuum concentration is-0.03MPa.Ethanol 500kg with 70% mixes with described pigment concentrate and sloughs pungent, obtains sloughing the pigment concentrate 78kg of pungent.The pigment concentrate of sloughing pungent is placed silicagel column top, carry out the silica gel column chromatography lock out operation.With the sherwood oil drip washing silicagel column of 4000L, the flow velocity of drip washing is 0.3 column volume/h, obtains the sherwood oil leacheate earlier.Re-use acetone 4000L drip washing silicagel column, the flow velocity of drip washing is 0.3 column volume/h, obtains the acetone leacheate.Described acetone leacheate vacuum concentration is obtained capsanthin 71kg.
Capsanthin to embodiment 1 preparation detects, and absorbancy, arsenic content, lead content, total organic solvent residual quantity, hexane residual quantity, capsaicin content detect according to the method for GB 10783-2008; Absorption ratio is by formula A
470nm/ A
454nmCalculate, wherein A
470nmAnd A
454nmBe respectively the absorbancy by spectrophotometric determination, absorption ratio is the ratio of same solution absorbance when wavelength is 470nm and 454nm.Detected result is shown in embodiment in the table 11.
Embodiment 2:
Get Shandong red pepper skin 2000kg, pulverize also and obtain the pigment leach liquor with the continuous leacher lixiviate of hoirzontally rotating after the granulation, will get pigment concentrate 108kg behind the leach liquor vacuum concentration again, the pressure of vacuum concentration is-0.03MPa.Ethanol 450kg with 70% mixes with described pigment concentrate and sloughs pungent, obtains sloughing the pigment concentrate 60kg of pungent.The pigment concentrate of sloughing pungent is placed silicagel column top, carry out the silica gel column chromatography lock out operation.With the sherwood oil drip washing silicagel column of 4500L, the flow velocity of drip washing is 0.3 column volume/h, obtains the sherwood oil leacheate earlier.Re-use acetone 2500L drip washing silicagel column, the flow velocity of drip washing is 0.3 column volume/h, obtains the acetone leacheate.Described acetone leacheate vacuum concentration is obtained capsanthin 53kg.
Capsanthin to embodiment 2 preparations detects, and absorbancy, arsenic content, lead content, total organic solvent residual quantity, hexane residual quantity, capsaicin content detect according to the method for GB 10783-2008; Absorption ratio is by formula A
470nm/ A
454nmCalculate, wherein A
470nmAnd A
454nmBe respectively the absorbancy by spectrophotometric determination, absorption ratio is the ratio of same solution absorbance when wavelength is 470nm and 454nm.Detected result is shown in embodiment in the table 12.
Comparative example 1:
Obtain pigment leach liquor 130kg with the continuous leacher lixiviate of hoirzontally rotating after getting Xinjiang red pepper skin 2000kg pulverizing and granulation.Elder generation removes pungent with 70% ethanol 550kg, behind the vacuum removal solvent, obtains capsanthin finished product 79.5kg again.Capsanthin to the comparative example preparation detects, and detected result is shown in comparative example in the table 1.
The capsanthin performance comparison of table 1 embodiment 1～2 and comparative example preparation
According to table 1 as can be seen, the absorption ratio of the capsanthin of embodiment 1 and embodiment 2 preparations illustrates the concentration height of the red pigments of the capsanthin that embodiment 1 and embodiment 2 prepare all greater than 1 and greater than the capsanthin that comparative example prepares.
By the contrast of embodiment 1～2 and comparative example detected result, illustrate that preparation method of the present invention can large-scale industrial production.The present invention has also used the silica gel column chromatography separation in addition, has removed most orange pigment and xanthein in the capsanthin, and the concentration of red pigments is improved, and absorption ratio improves.
More than the preparation method of a kind of capsanthin provided by the invention is described in detail; having used specific case herein sets forth principle of the present invention and embodiment; the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; should be understood that; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention; can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (10)
1. the preparation method of a capsanthin is characterized in that, comprising:
A) capsicum powder and leaching agent are mixed in the continous way leacher, leach, obtain the pigment leach liquor;
B) described pigment leach liquor is carried out vacuum concentration, obtain pigment concentrate;
C) carry out chromatographic separation after described pigment concentrate is deviate from pungent, obtain capsanthin.
2. preparation method according to claim 1 is characterized in that step c) is specially:
C 1) pigment concentrate that step b) is obtained and alcoholic solvent be 1: 2～6 to mix according to volume ratio, sloughs the pungent of described pigment concentrate;
C2) with step c1) pigment concentrate of deviating from pungent that obtains carries out silica gel column chromatography and separates, and with the described silicagel column of sherwood oil drip washing, obtains the sherwood oil leacheate earlier, uses the described silicagel column of acetone drip washing again, obtains the acetone leacheate;
C3) with step c2) the acetone leacheate that obtains concentrates, and obtains capsanthin.
3. preparation method according to claim 1 is characterized in that, described pigment leaching agent is the alkane that contains 4～7 carbon.
4. preparation method according to claim 1 is characterized in that, described continous way leacher is: flat rotary extractor, loop type extractor, satellite-type leacher or track type leacher.
5. preparation method according to claim 1 is characterized in that, the pressure of described vacuum concentration is-and 0.03MPa～-0.05MPa.
6. preparation method according to claim 2 is characterized in that, described sherwood oil and silicagel column are 2～4: 1 by volume.
7. preparation method according to claim 2 is characterized in that, described acetone and silicagel column are 2～4: 1 by volume.
8. preparation method according to claim 2 is characterized in that, the flow velocity of described sherwood oil drip washing is 0.3～1 column volume/h.
9. preparation method according to claim 2 is characterized in that, the flow velocity of described acetone drip washing is 0.3～1 column volume/h.
10. preparation method according to claim 2 is characterized in that, described alcoholic solvent is the alcoholic solvent that contains 2～4 carbon.
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| CN2010101905648A CN101831198B (en) | 2010-05-27 | 2010-05-27 | Preparation method of capsanthin |
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| CN2010101905648A CN101831198B (en) | 2010-05-27 | 2010-05-27 | Preparation method of capsanthin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830096A (en) * | 2015-04-21 | 2015-08-12 | 河北东之星生物科技股份有限公司 | Method for preparation of high light absorption ratio capsorubin |
| CN105647227A (en) * | 2015-12-30 | 2016-06-08 | 河南中大恒源生物科技股份有限公司 | Method for separating red pigment from yellow pigment of paprika red pigment |
| CN112945879A (en) * | 2021-02-07 | 2021-06-11 | 四川省农业科学院园艺研究所 | Synergistic detection method for color value of capsaicin and capsorubin |
| CN110590630B (en) * | 2019-09-29 | 2021-07-13 | 山东天音生物科技有限公司 | Method for separating and purifying zeaxanthin from capsanthin |
| CN114279992A (en) * | 2021-12-30 | 2022-04-05 | 广电计量检测（成都）有限公司 | Method for extracting and detecting yellow pigment in Huanggongfang pepper |
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|---|---|---|---|---|
| CN1392201A (en) * | 2002-07-18 | 2003-01-22 | 中山大学 | Extracting and purifying method for natural capsanthin pigment |
| CN101139467A (en) * | 2006-09-07 | 2008-03-12 | 河北晨光天然色素有限公司 | Process for abstracting both paprika oleoresin and paprika capsicum from pimiento |
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2010
- 2010-05-27 CN CN2010101905648A patent/CN101831198B/en active Active
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 |
| CN101139467A (en) * | 2006-09-07 | 2008-03-12 | 河北晨光天然色素有限公司 | Process for abstracting both paprika oleoresin and paprika capsicum from pimiento |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830096A (en) * | 2015-04-21 | 2015-08-12 | 河北东之星生物科技股份有限公司 | Method for preparation of high light absorption ratio capsorubin |
| CN104830096B (en) * | 2015-04-21 | 2016-10-12 | 河北东之星生物科技股份有限公司 | A kind of method preparing high absorption ratio capsorubin |
| CN105647227A (en) * | 2015-12-30 | 2016-06-08 | 河南中大恒源生物科技股份有限公司 | Method for separating red pigment from yellow pigment of paprika red pigment |
| CN110590630B (en) * | 2019-09-29 | 2021-07-13 | 山东天音生物科技有限公司 | Method for separating and purifying zeaxanthin from capsanthin |
| CN112945879A (en) * | 2021-02-07 | 2021-06-11 | 四川省农业科学院园艺研究所 | Synergistic detection method for color value of capsaicin and capsorubin |
| CN114279992A (en) * | 2021-12-30 | 2022-04-05 | 广电计量检测（成都）有限公司 | Method for extracting and detecting yellow pigment in Huanggongfang pepper |
| CN114279992B (en) * | 2021-12-30 | 2024-03-22 | 广电计量检测（成都）有限公司 | Extraction and detection method of yellow pigment in yellow Gong Jiao |
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| CN101831198B (en) | 2012-05-02 |
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