CN102807770A - Method for preparing paprika red pigment by ultrasonic pre-treatment - Google Patents
Method for preparing paprika red pigment by ultrasonic pre-treatment Download PDFInfo
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- CN102807770A CN102807770A CN2012102659353A CN201210265935A CN102807770A CN 102807770 A CN102807770 A CN 102807770A CN 2012102659353 A CN2012102659353 A CN 2012102659353A CN 201210265935 A CN201210265935 A CN 201210265935A CN 102807770 A CN102807770 A CN 102807770A
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Abstract
The invention discloses a method for preparing paprika red pigment by ultrasonic pre-treatment. The method comprises the steps of: selecting red chillies from Chengdu, Sichuan, removing pedicles and seeds, drying, crushing, screening by a 40meshes of standard screen, so as to obtain dry chilli powder; adding acetone in the dry chilli powder, carrying out pre-treatment by ultrasonic wave; adding the pre-treated material in a Soxhlet extractor, leaching and extracting for 3h at the temperature being 50 DEG C, conducting filter separation and decompression concentration so as to obtain chilli oil resin; adding ethanol in the chilli oil resin, extracting to obtain paprika red pigment rough product; adding sodium hydroxide aqueous solution in the paprika red pigment rough product, then adding normal hexane, adjusting pH value to be 3 by hydrochloric acid, conducting centrifugal separation, decompressing concentrating and drying so as to obtain the paprika red pigment product. According to the method, the industrial mass production is realized, and the prepared paprika red pigment product has the characteristics of high extracting speed, high purity, and the like.
Description
Technical field
The invention belongs to the foodstuff additive field, particularly a kind of is the process method of feedstock production CAPSAICIN with the natural capsicum.
Background technology
At present, food dye is one of indispensable raw material in the foodstuffs industry, can be divided into synthetic colour and natural pigment, and wherein synthetic colour is restricted its Application Areas because of having certain toxicity and detrimentally affect; Natural pigment then has natural and healthy attribute, so its market demand is huge.CAPSAICIN is the orange red natural fat-soluble pigment of tetraterpenes that from capsicum, extracts, the multiple ketene in type of the belonging to Radix Dauci Sativae pigment, and its lovely luster, the look valency is high, strong coloring force, it is good to protect chromatic effect, can effectively prolong the shelf-lives of bionic food; And have nutritional health function, and had anti-cancer function by the modern science proof, be widely used in fields such as food, beverage, feed, health care medicine and makeup at present, be the best the most salable red pigment of generally acknowledging in the world at present.
Capsicum presents the rough structure of fibrous tissue of sheet after pulverizing, and pigment and other fat-soluble component are present in the fibrous tissue.The method that is used for the CAPSAICIN extraction at present mainly contains oil molten method, organic solvent method and supercutical fluid method, and wherein oil dissolves the shortcoming of method existence oil and pigment separation difficulty, is difficult to obtain dense thick pigment; The supercutical fluid method is because of complicated operation, apparatus expensive, the more high factor of cost, and the commercial exploitation difficulty is bigger; And though organic solvent method is simple to operate, not high to equipment requirements, extraction time is long, yield is low, and the required organic solvent amount of subsequent processes is big, is unfavorable for suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, with low cost, the preparation method of the CAPSAICIN that is easy to realize suitability for industrialized production.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of ultrasonic pretreatment prepares the method for CAPSAICIN, and it comprises the steps:
(1) material choice:
Selecting the place of production for use is that the little red sharp green pepper in Chengdu, Sichuan is a raw material, after plucking the base of a fruit and removing seed, places 60 ℃ of baking ovens to dry to constant weight, pulverizes the back and crosses 40 mesh standard sieves, obtains dry paprika;
(2) ultrasonic pretreatment:
In the dry paprika that step (1) obtains, add acetone, utilize UW to carry out pre-treatment 20～30min, ultrasonic power is 360W;
(3) Suo Shi extracts:
Material after step (2) processing is added in the apparatus,Soxhlet's, in 50 ℃ of lixiviate 3h, then through filtering separation, concentrating under reduced pressure, the acquisition oleoresin capsicum;
(4) extraction is taken off peppery:
In the oleoresin capsicum that step (3) obtains, add alcohol and extract, re-extract 4 times is got upper strata (alcohol layer), and evaporation concentration obtains the CAPSAICIN bullion;
(5) alkalization is refining:
In the CAPSAICIN bullion that step (4) obtains, add aqueous sodium hydroxide solution, then add normal hexane, use hydrochloric acid adjust pH to 3 subsequently, obtain the CAPSAICIN product through spinning, concentrating under reduced pressure and 60 ℃ of oven dry.
In the step (2), for every 1g chillies, the adding volume of acetone is 10mL.
In the step (3), in the Suo Shi leaching process, the siphon number of times is 25～30 times.
In the step (4), ethanol concn is 75% (v/v).
In the step (4), described alcohol volume is 10 times of oleoresin capsicum volume.
In the step (5), the concentration of aqueous sodium hydroxide solution is 0.02g/mL, and for every 1mL CAPSAICIN bullion, the volumetric usage of aqueous sodium hydroxide solution is 10mL.
In the step (5), for every 1mL CAPSAICIN bullion, the volumetric usage of normal hexane is 6～8mL.
The method that adopts the ultrasonic pretreatment material to extract CAPSAICIN is to utilize UW in solvent, to propagate " cavitation effect " that produces; The capsicum cell walls is further broken and red pigment etc. is discharged in the extraction agent; Greatly reduce the CAPSAICIN permeation cell like this and be dissolved into the resistance of organic solvent, the extraction rate of CAPSAICIN and extraction yield are improved greatly.Soxhlet extraction then is backflow and the siphon principle that utilizes solvent, makes CAPSAICIN continuously by solvent extraction, has improved the extraction efficiency of CAPSAICIN greatly.Therefore, through ultrasonic pretreatment and combine soxhlet extraction to extract the process method of CAPSAICIN, obviously shortened whole extraction time, consumption of organic solvent significantly reduces than traditional method, the yield of CAPSAICIN also improves a lot; So this method can significantly be improved the extraction process of CAPSAICIN, will help realizing suitability for industrialized production, accelerate the extraction and the development and use speed of CAPSAICIN.
The invention has the beneficial effects as follows:
(1) with after the capsicum oven dry, pulverizing, the process ultrasonic pretreatment also combines soxhlet extraction to extract CAPSAICIN, can significantly shorten extraction time, reduce the usage quantity of organic solvent, and technology is simple, processing ease.
(2) technology of the present invention is easy to realize industrial amplification production.
(3) the CAPSAICIN product of the present invention's preparation has characteristics such as extraction rate is fast, product purity height.
Embodiment
According to following embodiment, can understand the present invention better.Yet, those skilled in the art will readily understand that the described content of embodiment only is used to explain the present invention, and the present invention that should also can not limit in claims to be described in detail.
Embodiment 1:
(1) material choice:
Selecting the place of production for use is that the little red sharp green pepper in Chengdu, Sichuan is a raw material, after plucking the base of a fruit and removing seed, places 60 ℃ of baking ovens to dry to constant weight, pulverizes the back with kibbler and crosses 40 mesh standard sieves, obtains dry paprika;
(2) ultrasonic pretreatment:
Get 10g dry paprika that step (1) obtains in triangular flask, add 100mL acetone, sealing is placed in the ultrasonic cleaner, utilizes UW to carry out pre-treatment 20～30min, and ultrasonic power is 360W;
(3) Suo Shi extracts:
Material after step (2) processing is added in the apparatus,Soxhlet's, in 50 ℃ of lixiviate 3h (the siphon number of times is 25～30 times), then through filtering separation, concentrating under reduced pressure, the about 4mL of acquisition oleoresin capsicum;
(4) extraction is taken off peppery:
In the oleoresin capsicum that step (3) obtains, add 40mL 75% (v/v) alcohol and extract, re-extract 4 times is got upper strata (alcohol layer), and evaporation concentration obtains the about 3mL of CAPSAICIN bullion;
(5) alkalization is refining:
In the CAPSAICIN bullion that step (4) obtains, add 0.02g/mL 30mL aqueous sodium hydroxide solution; Then add the 20mL normal hexane; Using 1:1 (v/v) hydrochloric acid adjust pH to 3 subsequently, obtain the CAPSAICIN product through spinning, concentrating under reduced pressure and 60 ℃ of oven dry, is 203.6 through measuring its look valency; Extraction yield is 83%, and the CAPSAICIN of preparation is comparatively stablized (table 1 and table 2) to heat, light etc.
Table 1 temperature is to the influence of CAPSAICIN stability
Table 2 illumination is to the influence of CAPSAICIN stability
Comparative Examples 1:
(1) material choice:
Selecting the place of production for use is that the little red sharp green pepper in Chengdu, Sichuan is a raw material, after plucking the base of a fruit and removing seed, places 60 ℃ of baking ovens to dry to constant weight, pulverizes the back with kibbler and crosses 40 mesh standard sieves, obtains dry paprika;
(2) Suo Shi extracts:
Get 10g dry paprika that step (1) obtains in apparatus,Soxhlet's, add 100mL acetone, in 50 ℃ of lixiviate 3h (the siphon number of times is 25～30 times), separate through filtering then, concentrating under reduced pressure, obtain the about 4mL of oleoresin capsicum;
(3) extraction is taken off peppery:
In the oleoresin capsicum that step (3) obtains, add 40mL 75% (v/v) alcohol and extract, re-extract 4 times is got upper strata (alcohol layer), and evaporation concentration obtains the about 3mL of CAPSAICIN bullion;
(4) alkalization is refining:
In the CAPSAICIN bullion that step (4) obtains, add 0.02g/mL 30mL aqueous sodium hydroxide solution; Then add the 20mL normal hexane; Use 1:1 (v/v) hydrochloric acid adjust pH to 3 subsequently; Obtaining the CAPSAICIN product through spinning, concentrating under reduced pressure and 60 ℃ of oven dry, is 194.2 through measuring its look valency, and extraction yield is 73%.
Comparative Examples 2:
(1) material choice:
Selecting the place of production for use is that the little red sharp green pepper in Chengdu, Sichuan is a raw material, after plucking the base of a fruit and removing seed, places 60 ℃ of baking ovens to dry to constant weight, pulverizes the back with kibbler and crosses 40 mesh standard sieves, obtains dry paprika;
(2) ultrasonic pretreatment:
Get 10g dry paprika that step (1) obtains in triangular flask, add 100mL acetone, sealing is placed in the ultrasonic cleaner, utilizes UW to carry out pre-treatment 20～30min, and ultrasonic power is 360W;
(3) leave standstill extraction:
Material after step (2) processing is added in the triangular flask, in 50 ℃ of lixiviate 3h (every 10min shakes 1 time), then through filtering separation, concentrating under reduced pressure, the about 4mL of acquisition oleoresin capsicum;
(4) extraction is taken off peppery:
In the oleoresin capsicum that step (3) obtains, add 40mL 75% (v/v) alcohol and extract, re-extract 4 times is got upper strata (alcohol layer), and evaporation concentration obtains the about 3mL of CAPSAICIN bullion;
(5) alkalization is refining:
In the CAPSAICIN bullion that step (4) obtains, add 0.02g/mL 30mL aqueous sodium hydroxide solution; Then add the 20mL normal hexane; Use 1:1 (v/v) hydrochloric acid adjust pH to 3 subsequently; Obtaining the CAPSAICIN product through spinning, concentrating under reduced pressure and 60 ℃ of oven dry, is 112.4 through measuring its look valency, and extraction yield is 46%.
Claims (7)
1. a ultrasonic pretreatment prepares the method for CAPSAICIN, it is characterized in that it comprises the steps:
(1) material choice:
Selecting the place of production for use is that the little red sharp green pepper in Chengdu, Sichuan is a raw material, after plucking the base of a fruit and removing seed, places 60 ℃ of baking ovens to dry to constant weight, pulverizes the back and crosses 40 mesh standard sieves, obtains dry paprika;
(2) ultrasonic pretreatment:
In the dry paprika that step (1) obtains, add acetone, utilize UW to carry out pre-treatment 20～30min, ultrasonic power is 360W;
(3) Suo Shi extracts:
Material after step (2) processing is added in the apparatus,Soxhlet's, in 50 ℃ of lixiviate 3h, then through filtering separation, concentrating under reduced pressure, the acquisition oleoresin capsicum;
(4) extraction is taken off peppery:
In the oleoresin capsicum that step (3) obtains, add alcohol and extract, re-extract 4 times is got the upper strata, and evaporation concentration obtains the CAPSAICIN bullion;
(5) alkalization is refining:
In the CAPSAICIN bullion that step (4) obtains, add aqueous sodium hydroxide solution, then add normal hexane, use hydrochloric acid adjust pH to 3 subsequently, obtain the CAPSAICIN product through spinning, concentrating under reduced pressure and 60 ℃ of oven dry.
2. ultrasonic pretreatment according to claim 1 prepares the method for CAPSAICIN, it is characterized in that, in the step (2), for every 1g chillies, the adding volume of acetone is 10mL.
3. ultrasonic pretreatment according to claim 1 prepares the method for CAPSAICIN, it is characterized in that, in the step (3), in the Suo Shi leaching process, the siphon number of times is 25～30 times.
4. ultrasonic pretreatment according to claim 1 prepares the method for CAPSAICIN, it is characterized in that, in the step (4), ethanol concn is 75% (v/v).
5. ultrasonic pretreatment according to claim 4 prepares the method for CAPSAICIN, it is characterized in that, in the step (4), described alcohol volume is 10 times of oleoresin capsicum volume.
6. ultrasonic pretreatment according to claim 1 prepares the method for CAPSAICIN; It is characterized in that in the step (5), the concentration of aqueous sodium hydroxide solution is 0.02g/mL; For every 1mL CAPSAICIN bullion, the volumetric usage of aqueous sodium hydroxide solution is 10mL.
7. ultrasonic pretreatment according to claim 1 prepares the method for CAPSAICIN, it is characterized in that, in the step (5), for every 1mL CAPSAICIN bullion, the volumetric usage of normal hexane is 6～8mL.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103013179A (en) * | 2013-01-11 | 2013-04-03 | 邯郸市中进天然色素有限公司 | Method for enhancing extinction ratio of capsanthin pigment |
| CN103254093A (en) * | 2013-05-24 | 2013-08-21 | 杨博智 | Method for rapidly extracting capsaicin from pepper |
| CN103549239A (en) * | 2013-11-19 | 2014-02-05 | 四川省原子能研究院 | Color protection method for hot-chili-oil-containing food by irradiation processing |
| CN105038307A (en) * | 2015-07-23 | 2015-11-11 | 柳州易农科技有限公司 | Ultrasonic-assisted method for extracting watermelon haematochrome |
| CN106281651A (en) * | 2016-08-16 | 2017-01-04 | 张�杰 | A kind of chilli oil ultrasonic extraction device and preparation method |
| CN106350196A (en) * | 2016-08-16 | 2017-01-25 | 张�杰 | System and method for producing chili oil |
| CN115073279A (en) * | 2022-07-13 | 2022-09-20 | 遵义职业技术学院 | Extraction method of capsorubin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013179A (en) * | 2013-01-11 | 2013-04-03 | 邯郸市中进天然色素有限公司 | Method for enhancing extinction ratio of capsanthin pigment |
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| CN103549239A (en) * | 2013-11-19 | 2014-02-05 | 四川省原子能研究院 | Color protection method for hot-chili-oil-containing food by irradiation processing |
| CN103549239B (en) * | 2013-11-19 | 2015-02-11 | 四川省原子能研究院 | Color protection method for hot-chili-oil-containing food by irradiation processing |
| CN105038307A (en) * | 2015-07-23 | 2015-11-11 | 柳州易农科技有限公司 | Ultrasonic-assisted method for extracting watermelon haematochrome |
| CN106281651A (en) * | 2016-08-16 | 2017-01-04 | 张�杰 | A kind of chilli oil ultrasonic extraction device and preparation method |
| CN106350196A (en) * | 2016-08-16 | 2017-01-25 | 张�杰 | System and method for producing chili oil |
| CN115073279A (en) * | 2022-07-13 | 2022-09-20 | 遵义职业技术学院 | Extraction method of capsorubin |
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Application publication date: 20121205 |