Method for refining capsanthin and application thereof

Abstract

The invention relates to the technical field of extract refining, and particularly discloses a method for refining capsanthin and application of the capsanthin. The method for refining the paprika red pigment comprises the following steps: (1) sequentially carrying out secondary supercritical carbon dioxide extraction on the paprika red pigment to be refined, and collecting the paprika red pigment A from a separation kettle; the temperature of the secondary supercritical carbon dioxide extraction is 50-55 DEG C; the pressure of the first extraction is 15-20 Mpa, and the pressure of the second extraction is 25-30 Mpa; (2) heating the capsanthin A to 43 + / -3 DEG C, fully dissolving, cooling to 5 + / -2 DEG C, and heating to room temperature; or, after the temperature is reduced to 5 + / -2 DEG C, repeated heating and cooling treatment is conducted, the heating temperature of each time is lower than the heating temperature of the last time, the cooling temperature of each time is higher than the cooling temperature of the last time, and finally the temperature is increased to the room temperature; during heating and cooling treatment, heat preservation is performed for 0.5-1.5 hours after heating and cooling each time; and (3) separating and removing impurities. The pigment product with good stability and low-temperature fluidity can be obtained.

Description

Technical Field

[0001] The invention relates to the technical field of extract refining, in particular to a method for refining capsanthin and application thereof. Background Art

[0002] Capsanthin, commonly known as capsanthin, is a natural carotenoid ester complex extracted, separated and refined from the natural spice capsanthin. Capsanthin is usually a red liquid with stable performance and can be miscible with oils and fats in any proportion. Because it is natural and safe, easy to use, and the pigment content can be standardized and controlled, it has been widely used in various foods. Although capsanthin has a good coloring effect and is easy to use, it is easily affected by light, heat, and oxygen and is easy to fade. Especially in powder products, fading is a common problem. How to improve the stability of capsanthin has been widely and deeply studied by many scholars and manufacturers.

[0003] According to statistical analysis, the most mature and commonly used method is to add exogenous color-protecting ingredients to capsanthin. Commonly used color-protecting agents are mainly synthetic and natural antioxidants and other color-protecting ingredients, such as TBHQ, BHT, BHA, tea polyphenols, vitamin E, vitamin C, carnosic acid, etc. By adding exogenous color-protecting ingredients, the light, heat and oxygen stability of capsanthin can be greatly improved, and the shelf life of the product can be extended.

[0004] Although adding exogenous color preservatives is a relatively economical and feasible method to solve the stability of capsanthin, many commonly used antioxidant color preservatives are not allowed to be used in some special / high-demand scenarios. For example, some products do not allow the addition of any non-capsicum ingredients. Therefore, it is very necessary to research and develop a processing method that can improve the light, heat and oxygen stability of capsanthin in powder application scenarios and does not contain any exogenous color preservatives. Summary of the invention

[0005] One of the purposes of the present invention is to provide a method for maintaining the light and heat stability of capsanthin without adding exogenous color-protecting components.

[0006] The present invention provides a method for refining capsanthin, which comprises: (1) subjecting the capsanthin to be purified to a first supercritical carbon dioxide extraction, and after the impurities are discharged from the separation kettle, the pressure is increased to conduct a second supercritical carbon dioxide extraction, and the capsanthin A is collected from the separation kettle; The temperature of the first supercritical carbon dioxide extraction and the second supercritical carbon dioxide extraction is 50-55° C.; the pressure of the first supercritical carbon dioxide extraction is 15-20 MPa, and the pressure of the second supercritical carbon dioxide extraction is 25-30 MPa; (2) subjecting the capsanthin A to a temperature rise and fall treatment: First, the capsanthin A is heated to 43±3°C to be fully dissolved (without any particulate matter, and the whole is in a uniform black-red liquid state), then cooled to 5±2°C, and then heated to room temperature; or, after cooling to 5±2°C, the temperature is repeatedly raised and lowered, each time the temperature is lower than the previous temperature, and each time the temperature is lower than the previous temperature, and finally the temperature is raised to room temperature; during the temperature raising and lowering treatment, the temperature is kept for 0.5-1.5 hours after each heating and cooling; (3) Separate and remove impurities (solid or viscous impurity components).

[0007] The material composition of capsanthin is relatively complex, among which the main components that present color are a series of natural carotenoid substances such as capsanthin, capsanthin, and zeaxanthin. The content of natural pigments in capsanthin products is usually measured by color value, and the main specification circulating in the market is E150. Taking E150 specification capsanthin as an example, the weight of various natural carotenoids accounts for about 7-8%; the fatty acid esters with diglycerides and triglycerides as the main components account for about 85-90%. In addition, it also contains a lot of sugars, sugar esters, amides, and polyphenols. These ingredients account for a small proportion, but the present invention has found that they may have a relatively large impact on the storage and application stability of the pigment, and thus a method has been developed to prevent capsanthin from being easily affected by light, heat, and oxygen during application and fading and loss.

[0008] The present invention has been found in the industrial processing implementation process of capsanthin for many years through practice that a specific supercritical carbon dioxide extraction method can remove some components that are easy to cause the loss of capsanthin, and can also enrich the stability components in capsanthin, thereby improving the stability of capsanthin to a certain extent, but the degree of stability improvement still needs to be improved, and the capsanthin obtained by supercritical carbon dioxide extraction is low in price, and it is easy to solidify and agglomerate at low temperature. It is difficult to disperse evenly when mixing and applying on powder food, and it is easy to cause the appearance of pigment blocks, which is inconvenient to use. When the capsanthin obtained by supercritical impurity removal extraction and separation in a specific way is further subjected to temperature change treatment, the stability of capsanthin can be further improved, and the problem of easy solidification of pigment at low temperature and uneven mixing of powder is solved at the same time. The refined capsanthin obtained by the method can significantly improve the light, heat and oxygen stability of capsanthin when applied, and is convenient for application in powder scenes.

[0009] Specifically, the present invention first extracts the capsanthin raw paste (not diluted with oil) which is conventionally commercially available or prepared by conventional methods for the first time under a specific lower pressure with supercritical carbon dioxide. This step can not only retain the color value as much as possible, but also discharge the impurities that affect stability from the separation kettle as much as possible (the impurities can be treated as grease waste). After the impurity separation is completed, the pressure of the extraction kettle is increased for extraction and separation, so that the materials therein are subjected to a second supercritical carbon dioxide extraction at a specific higher pressure. At this time, the substances that contribute to stability are dissolved by supercritical carbon dioxide together with part of the capsanthin and brought into the separation kettle. After decompression separation, the capsanthin A with improved stability can be obtained, and the remaining materials in the extraction kettle are capsanthin products with slightly poor stability but higher color value and no taste. This step obtains two capsanthin products with different performances, realizes the comprehensive utilization of raw materials, and avoids waste.

[0010] The present invention obtains a capsanthin product (capsanthin A) with high yield and improved stability by setting specific secondary supercritical carbon dioxide extraction conditions, and further combines one or more stages of specific heating and cooling treatment processes, so that impurities in the capsanthin A can be further removed, substances that are beneficial to stability and substances that present color are further enriched, so that the stability and color value of the product are further improved, and the low-temperature fluidity of the product is also improved, which can be better used in subsequent applications.

[0011] In the method of the present invention, after the first sufficient dissolution, although the greater the temperature reduction, the more conducive it is to the precipitation of impurities, if the temperature is too low and causes the capsanthin A to solidify, even if the subsequent temperature is repeatedly raised and lowered, the effect of impurity separation will still be reduced and the product yield will be reduced.

[0012] In the present invention, room temperature refers to 24-26°C.

[0013] Preferably, the pressure of the first supercritical carbon dioxide extraction is 18-20 MPa, and the extraction time is 1 hour, and the pressure of the second supercritical carbon dioxide extraction is 28-30 MPa, and the extraction time is 4-6 hours.

[0014] In step (2) of the method of the present invention, during the temperature rise and fall treatment, the temperature rise and fall rates after sufficient dissolution are 0.09-0.11°C / min; the temperature rise and fall treatment is always carried out under stirring, and the stirring rate is 10-20 rpm.

[0015] The present invention finds that slowly increasing or decreasing the temperature helps to improve the stability of capsanthin A. If the temperature increase or decrease rate is too fast, although the purity of capsanthin A can be improved, the yield and stability of capsanthin A will be reduced.

[0016] In step (2) of the method of the present invention, the temperature is repeatedly raised and lowered 1 to 3 times.

[0017] In the method of the present invention, during the first supercritical carbon dioxide extraction and the second supercritical carbon dioxide extraction, the ratio of the mass of the capsanthin to be purified to the flow rate of carbon dioxide is 1: (10-15) kg: L / h (when 1 kg of raw material is put into the extraction kettle, the flow rate of carbon dioxide is 10-15 L / h); the time of the first supercritical carbon dioxide extraction is 1.0-1.5 h, and the time of the second supercritical carbon dioxide extraction is 4-6 h.

[0018] In the method of the present invention, the separation pressure of the separation kettle is 5-10 MPa, and the separation temperature is 30-40°C.

[0019] In step (3) of the method of the present invention, the method for separating and removing impurities is centrifugation or filtration.

[0020] For example, disc centrifugation can be used with a centrifugal speed of 3800-4200 rpm, and the light phase obtained by centrifugation is the refined capsanthin product.

[0021] In step (2) of the method of the present invention, when the temperature is repeatedly raised and lowered, each heating temperature is 5±1°C lower than the previous heating temperature, and each cooling temperature is 5±1°C higher than the previous cooling temperature.

[0022] That is, if the highest temperature of capsanthin A during the first dissolution is 45°C and then cooled to 5°C, the end point temperature of the second heating may be 45-5°C (40°C), and the end point of the cooling may be 5+5°C (10°C), and so on.

[0023] The present invention has found that the smaller the difference in the end point of each temperature increase and decrease, the more favorable it is for obtaining a product with high yield and high stability. However, for the sake of production efficiency, the present invention preferably sets the end point difference in the temperature for each temperature increase and decrease to 5±1°C, and the number of repeated temperature increase and decrease treatments is 2 times.

[0024] As a preferred embodiment, in step (2) of the method of the present invention, the capsanthin A is first heated to 43±3°C and stirred until fully dissolved, then cooled to 5±2°C at a rate of 0.09-0.11°C / min, stirred for 1.0-1.5h, and then heated to 40±2°C at a rate of 0.09-0.11°C / min, stirred for 20-30min, and then heated to 40±2°C at a rate of 0.09-0.11°C / min. in. The temperature was cooled to 10±2℃ at a rate of 0.09-0.11℃ / min. After stirring for 1.0-1.5h, the temperature was increased to 35±2℃ at a rate of 0.09-0.11℃ / min. After stirring for 20-30min, the temperature was cooled to 15±2℃ at a rate of 0.09-0.11℃ / min. After stirring for 1.0-1.5h, the temperature was increased to 23-25℃ at a rate of 0.09-0.11℃ / min. The temperature was increased for 1.0-1.5h.

[0025] The present invention also provides capsanthin, which is obtained by refining the above method.

[0026] The method of the present invention can obtain capsanthin with improved light, heat and oxygen stability, and has good low-temperature fluidity, and is suitable for coloring powdered foods (such as pickles, barbecue ingredients and other powdered composite seasonings).

[0027] The present invention also provides application of the above method in improving the stability and / or low-temperature fluidity of capsanthin.

[0028] The beneficial effects of the present invention are at least: The present invention provides for the first time a method for improving the light, heat and oxygen stability of capsanthin through a refining process. The capsanthin prepared by the refining method of the present invention can greatly improve the light, heat and oxygen stability of the capsanthin component without adding any exogenous color retaining agent, especially in powder application scenarios, the stability can be improved by more than 1 times, greatly extending the shelf life of the product. Moreover, the capsanthin prepared by the refining method of the present invention has good low-temperature fluidity and no condensate, and is suitable for application under low temperature conditions.

[0029] The process of refining capsanthin of the present invention is a physical separation method without extreme conditions. There is basically no loss of capsanthin pigment in the whole process. While preparing capsanthin pigment with good stability, the capsanthin pigment remaining in the extraction kettle after supercritical secondary treatment has no taste, can meet the use demand of high-end odorless capsanthin, and also realizes the added value of the product.

[0030] Furthermore, the method for refining capsanthin provided by the present invention has the advantages of short operation time and high efficiency, and is suitable for industrial large-scale production. DETAILED DESCRIPTION

[0031] The preferred embodiments of the present invention will be described in detail below in conjunction with examples. It should be understood that the following examples are provided only for the purpose of illustration and are not intended to limit the scope of the present invention. Those skilled in the art may make various modifications and substitutions to the present invention without departing from the purpose and spirit of the present invention.

[0032] The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, etc. used in the following examples are commercially available or prepared according to conventional methods in the art unless otherwise specified.

[0033] The capsanthin (raw material) to be refined used in the following examples and comparative examples is extracted by an organic solvent method. Specifically, the bell peppers dried or baked in Xinjiang are used as raw materials, and the seeded pepper skin is crushed, granulated, extracted and concentrated by a weak polar organic solvent to prepare a crude extract, and then degummed by hydration, and separated by low-carbon alcohol (including methanol, ethanol, isopropanol, etc., and ethanol with a safer and cost-effective ethanol is usually selected for the convenience of industrial implementation) to prepare capsanthin. The weak polar organic solvent is a subcritical butane or a single or mixed alkane of C6 (such as n-hexane, 2-methylpentane, 3-methylpentane, methylcyclopentane, cyclohexane, vegetable oil extraction solvent, etc.), or the weak polar organic solvent is a mixed solvent of a single or mixed alkane of C6 and acetone or ethyl acetate, and the alkane generally accounts for 85-95% of the mixed solvent.

[0034] Specifically, when preparing the capsanthin of Examples 1-8 and Comparative Examples 1-4, the weakly polar organic solvent used is a mixed solvent of vegetable oil extraction solvent / acetone = 90 / 10. After hydration and degumming, the capsanthin is separated by despicable removal with 78° ethanol to prepare the capsanthin. When preparing the capsanthin of Example 9, the weakly polar organic solvent used is subcritical butane. After hydration and degumming, the capsanthin is separated by despicable removal with 75° ethanol to prepare the capsanthin. Examples 1-7 and Example 9 use a raw material of pepper particles with a unit color value of 17.5 for extraction and preparation; Example 8 uses a raw material of pepper particles with a unit color value of 16.6 for preparation.

[0035] For the detection method of some color values ​​in the specific implementation mode of the present invention, please refer to GB 1886.34-2015.

[0036] Example 1 This embodiment provides a method for refining capsanthin, and the steps are as follows: (1) Take 1000.0g of capsanthin (color value is E240) and put it into a 5L supercritical carbon dioxide extraction kettle. Under the conditions of extraction temperature of 55℃, extraction pressure of 20MPa, separation pressure of 10MPa, separation temperature of 40℃, and carbon dioxide flow rate of 11L / h, after 1.0 hour of extraction and separation, 50.5g of the separated product was released from the separation kettle after the pressure was reduced (the color value of the separated product was E1.5 according to the national standard method for capsanthin (GB 1886.34-2015), and it can be treated as waste oil). Then, the extraction pressure of the extraction kettle was increased to 30MPa. Under the condition that other parameters were the same as the first extraction, the extraction and separation was continued for 5.0h, and the pressure was reduced to obtain 382.3g of capsanthin A from the separation kettle, with a color value of E167.6; 566.2g of odorless supercritical capsanthin was released from the extraction kettle, with a color value of E307.2.

[0037] (2) Take 350g of capsanthin A and put it into a 1000ml glass reactor. Turn on the temperature control system, heat it to 45℃ and stir for 1.0 hour. After the pigment is fully dissolved and the overall color remains uniform black and red, start the program cooling. After cooling to 5℃, keep it warm for 1.5 hours, then program heating to 40℃ and keep it warm and stir for 30 minutes. Then program cooling to 10℃ and keep it warm for 1.0 hour. Then program heating to 35℃ and keep it warm for 30 minutes. Then program cooling to 15℃ and keep it warm for 1.0 hour. Then program heating to 25℃ and keep it warm and stir for 1.0 hour. All program heating and cooling rates are 0.1℃ / min, and the stirring rate is 20 rpm. Afterwards, centrifugation was carried out at 4000 rpm for 10 min to obtain 324.6 g of centrifugal light phase capsanthin B with a color value of E179.3 and 25.4 g of centrifugal heavy phase impurities with a color value of E17.7. The color value yield of this treatment process was 99.22%, with very low loss.

[0038] Example 2 This embodiment provides a method for refining capsanthin, and the steps are as follows: Take 350g of the capsanthin A prepared according to the method of Example 1, put it into a 1000ml glass reactor, turn on the temperature control system, heat it to 45 ° C and stir for 1.0 hours, the pigment is fully dissolved, and the whole is kept uniformly black and red. Then, the program is turned on to cool it down, and after cooling to 5 ° C and keeping it for 1.5h, the program is heated to 25 ° C and kept stirring for 1.0h. All program heating and cooling rates are 0.1 ° C / min, and the stirring rate is 15 rpm. Afterwards, at 4000 rpm, centrifugation is performed for 10min to obtain centrifugal light phase capsanthin B 329.2g, the color value is E174.6, the centrifugal heavy phase impurities are 20.8g, the color value is E93.7, and the color value yield of the treatment process is 97.99%.

[0039] Example 3 This embodiment provides a method for refining capsanthin, and the steps are as follows: Take 350g of the capsanthin A prepared according to the method of Example 1, put it into a 1000ml glass reactor, turn on the temperature control system, heat it to 45 ° C and stir for 1.0 hours, the pigment is fully dissolved, and the overall uniform black and red color is maintained. Then, the program is turned on to cool down, cool to 5 ° C and keep it for 1.5 hours, then program it to 40 ° C and keep it for 30 minutes, then program it to cool down to 10 ° C and keep it for 1.0 hours, then program it to 25 ° C and keep it for 1.0 hours, all program heating and cooling rates are 0.1 ° C / min, and the stirring rate is 15 revs / min. Afterwards, at 4000 revs / min, centrifugation is performed for 10 minutes to obtain centrifugal light phase capsanthin B326.7g, the color value is E177.2, the centrifugal heavy phase impurities are 23.3g, and the color value is E46.6. The color value yield of the processing process is 98.69%.

[0040] Example 4 This embodiment provides a method for refining capsanthin, and the steps are as follows: Take 350g of capsanthin A prepared according to the method of Example 1, put it into a 1000ml glass reactor, turn on the temperature control system, heat it to 45°C and stir for 1.0 hour, the pigment is fully dissolved, and the whole color is kept uniformly black and red. Then, start the program cooling, cool it to 5°C, keep it warm for 1.5h, then program it to 40°C, keep it warm and stir for 30 minutes, then program it to cool to 10°C and keep it warm for 1.0h, then program it to heat it to 35°C and keep it warm for 30 minutes, then program it to cool to 15°C and keep it warm for 1.0h, then program it to heat it to 30°C and keep it warm for 30 minutes, then program it to cool to 20°C and keep it warm for 1.0h, then program it to heat it to 25°C and keep it warm for 1.0h, all program heating and cooling rates are 0.1°C / min, and the stirring rate is 10 rpm. Afterwards, centrifugation was carried out at 4000 rpm for 10 min to obtain 319.3 g of centrifugal light phase capsanthin B with a color value of E182.2 and 30.7 g of centrifugal heavy phase impurities with a color value of E13.3. The color value yield of this treatment process was 99.18%.

[0041] Example 5 This embodiment provides a method for refining capsanthin, and the steps are as follows: (1) Take 1000.0g of the capsanthin to be purified (color value E240) used in Example 1 and put it into a 5L supercritical carbon dioxide extraction kettle. Under the conditions of extraction temperature of 50°C, extraction pressure of 15MPa; separation pressure of 6MPa, separation temperature of 30°C, and carbon dioxide flow rate of 10L / h, after 1.0 hour of extraction and separation, 24.5g of the separated product (color value E1.2, which can be treated as waste oil) was released from the separation kettle by reducing the pressure. Then, the extraction pressure was increased to 25MPa. Under the condition that other parameters were the same as the first extraction, the extraction and separation was continued for 5.0h, and the pressure was reduced to obtain 400.9g of capsanthin A from the separation kettle, with a color value of E151.3; 571.2g of odorless supercritical capsanthin was released from the extraction kettle, with a color value of E310.5.

[0042] (2) Take 350g of capsanthin A and put it into a 1000ml glass crystallization reactor. Turn on the temperature control system, heat it to 45℃ and stir for 1.0 hour. After the pigment is fully dissolved and the overall color remains uniform black and red, start the program cooling. After cooling to 5℃, keep it warm for 1.5 hours, then program heating to 40℃ and keep it warm and stir for 30 minutes. Then program cooling to 10℃ and keep it warm for 1.0 hour. Then program heating to 35℃ and keep it warm for 30 minutes. Then program cooling to 15℃ and keep it warm for 1.0 hour. Then program heating to 25℃ and keep it warm and stir for 1.0 hour. All program heating and cooling rates are 0.1℃ / min, and the stirring rate is 20 rpm. Afterwards, centrifugation was carried out at 4000 rpm for 10 min to obtain 301.2 g of centrifugal light phase capsanthin B with a color value of E173.3 and 48.8 g of centrifugal heavy phase impurities with a color value of E15.3. The color value yield of this treatment process was 98.57%.

[0043] Example 6 (1) Take 1000.0g of capsanthin (color value is E240) and put it into a 5L supercritical carbon dioxide extraction kettle. Under the conditions of extraction temperature of 55℃, extraction pressure of 20MPa, separation pressure of 10MPa, separation temperature of 40℃, and carbon dioxide flow rate of 15L / h, after 1.0 hour of extraction and separation, 60.2g of the separated product was released from the separation kettle after the pressure was reduced (the color value of the separated product was E1.9 according to the national standard method for capsanthin (GB 1886.34-2015), and it can be treated as waste oil). Then, the extraction pressure of the extraction kettle was increased to 30MPa. Under the condition that other parameters were the same as the first extraction, the extraction and separation was continued for 5.0h, and the pressure was reduced to obtain 410.7g of capsanthin A from the separation kettle, with a color value of E171.2; 529.1g of odorless supercritical capsanthin was released from the extraction kettle, with a color value of E316.8.

[0044] (2) Take 350g of capsanthin A and put it into a 1000ml glass reactor. Turn on the temperature control system, heat it to 45℃ and stir for 1.0 hour. After the pigment is fully dissolved and the overall color remains uniform black and red, start the program cooling. After cooling to 5℃, keep it warm for 1.5 hours, then program heating to 40℃ and keep it warm and stir for 30 minutes. Then program cooling to 10℃ and keep it warm for 1.0 hour. Then program heating to 35℃ and keep it warm for 30 minutes. Then program cooling to 15℃ and keep it warm for 1.0 hour. Then program heating to 25℃ and keep it warm and stir for 1.0 hour. All program heating and cooling rates are 0.1℃ / min, and the stirring rate is 20 rpm. After that, centrifugation was performed at 4000 rpm for 10 min to obtain 325.5 g of centrifugal light phase capsanthin B with a color value of E182.6 and 24.5 g of centrifugal heavy phase impurities with a color value of E18.3. The color value yield of this treatment process was 99.19%. Example 7 This embodiment provides a method for refining capsanthin, and the steps are as follows: Take 350g of capsanthin A prepared according to the method of Example 1, put it into a 1000ml glass reactor, turn on the temperature control system, heat it to 46°C and stir for 1.0 hour, the pigment is fully dissolved, and the whole color is kept uniformly black and red. Then, start the program cooling, cool it to 4°C, keep it warm for 1.5h, then program it to 40°C, keep it warm and stir for 30 minutes, then program it to cool to 10°C and keep it warm for 1.0h, then program it to heat it to 34°C and keep it warm for 30 minutes, then program it to cool to 16°C and keep it warm for 1.0h, then program it to heat it to 25°C and keep it warm and stir for 1.0h, all program heating and cooling rates are 0.1°C / min, and the stirring rate is 20 rpm. Afterwards, centrifugation was carried out at 4000 rpm for 10 min to obtain 323.4 g of centrifugal light phase capsanthin B with a color value of E179.2 and 26.6 g of centrifugal heavy phase impurities with a color value of E33.3. The color value yield of this treatment process was 98.80%, with low loss.

[0045] Example 8 This embodiment provides a method for refining capsanthin, and the steps are as follows: (1) Take 1000.0g of capsanthin (color value is E200) and put it into a 5L supercritical carbon dioxide extraction kettle. Under the conditions of extraction temperature of 55℃, extraction pressure of 20MPa, separation pressure of 10MPa, separation temperature of 40℃, and carbon dioxide flow rate of 11L / h, after 1.0 hour of extraction and separation, 48.7g of separated product (color value is E1.4, which can be treated as waste oil) is released from the separation kettle by reducing the pressure. Then, the extraction pressure of the extraction kettle is increased to 30MPa. Under the condition that other parameters are the same as the first extraction, the extraction and separation is continued for 5.0h, and the pressure is reduced to obtain 376.6g of capsanthin A from the separation kettle, with a color value of E151.8; 573.9g of odorless supercritical capsanthin is released from the extraction kettle, with a color value of E246.3.

[0046] 350 g of capsanthin A was taken and prepared according to the method of step (2) of Example 1 to obtain 334.1 g of capsanthin B with a color value of E158.2. 15.9 g of centrifugal heavy phase impurities had a color value of E17.3. The color value yield of the treatment process was 99.48%, with very low loss.

[0047] Example 9 This embodiment provides a method for refining capsanthin, and the steps are as follows: (1) Take 1000.0g of capsanthin (color value is E252.5) ​​and put it into a 5L supercritical carbon dioxide extraction kettle. Under the conditions of extraction temperature of 55℃, extraction pressure of 20MPa, separation pressure of 10MPa, separation temperature of 40℃, and carbon dioxide flow rate of 11L / h, after 1.0 hour of extraction and separation, 53.8g of separated product (color value is E1.7, which can be treated as waste oil) is released from the separation kettle by reducing the pressure. Then, the extraction pressure of the extraction kettle is increased to 30MPa. Under the condition that other parameters are the same as the first extraction, the extraction and separation is continued for 5.0h, and the pressure is reduced to obtain 384.1g of capsanthin A from the separation kettle, with a color value of E173.6; 561.1g of odorless supercritical capsanthin is released from the extraction kettle, with a color value of E327.3.

[0048] 350 g of capsanthin A was taken and prepared according to the method of step (2) of Example 1 to obtain 322.4 g of capsanthin B with a color value of E186.8. 27.6 g of centrifugal heavy phase impurities had a color value of E18.4. The color value yield of this treatment process was 99.12%, and the loss was very low.

[0049] Comparative Example 1 The capsanthin to be purified is directly used in Example 1 (raw material with a color value of E240).

[0050] Comparative Example 2 The capsanthin A is directly prepared according to step (1) of Example 1.

[0051] Comparative Example 3 This comparative example provides a method for refining capsanthin, and the steps are as follows: directly use 350g of the capsanthin to be purified used in Example 1 (raw material with a color value of E240) to carry out step (2) of Example 1, and finally centrifuge to obtain 328.5g of capsanthin B, E249.8, and 21.5g of centrifugal heavy phase impurities, E89.4.

[0052] Comparative Example 4 This comparative example provides a method for refining capsanthin, and the steps are as follows: (1) 1000.0 g of the capsanthin to be purified (capsanthin with a color value of E240) used in Example 1 was put into a 5 L supercritical carbon dioxide extraction kettle. At an extraction temperature of 55° C., an extraction pressure of 27 MPa, a separation pressure of 10 MPa, a separation temperature of 40° C., and a carbon dioxide flow rate of 11 L / h, after 5.0 hours of extraction and separation, the pressure was reduced to obtain 423.7 g of capsanthin A from the separation kettle with a color value of E142.36; 574.8 g of odorless supercritical capsanthin was released from the extraction kettle with a color value of E309.2.

[0053] (2) Take 350g of capsanthin A and put it into a 1000ml glass reactor. Turn on the temperature control system, heat it to 45℃ and stir for 1.0 hour. After the pigment is fully dissolved and the overall color is kept uniformly black and red, start the program cooling. After cooling to 5℃, keep it warm for 1.5 hours, then heat it to 40℃ and keep it warm for 30 minutes, then cool it to 10℃ and keep it warm for 1.0 hour, then heat it to 35℃ and keep it warm for 30 minutes, then cool it to 15℃ and keep it warm for 1.0 hour, then heat it to 25℃ and keep it warm for 1.0 hour. All the program heating and cooling rates are 0.1℃ / min. After that, centrifuge at 4000 rpm for 10 minutes to obtain 284.9g of centrifugal light phase capsanthin B with a color value of E162.2 and 65.1g of centrifugal heavy phase impurities with a color value of E55.2.

[0054] Experimental example This experimental example evaluates the products obtained in each embodiment and comparative example, as follows: Method for determining the coloring stability of capsanthin in powdered food: Use commercially available common edible salt as a carrier, sieve the edible salt, select the 40-60 mesh part (100% through 40 mesh, 100% cannot pass 60 mesh), accurately weigh the capsanthin and edible salt powder, mix them thoroughly, and prepare salt powder with a unit color value of E1.0±0.02. Weigh 15.0±0.1g of the dyed salt powder, put it into a round glass surface dish with a diameter of 10±0.1cm, vibrate to form a uniform plane, put it into a 25℃ light 20000lux, humidity 40% incubator, and conduct stability test. Test once every 5 days. During the test, transfer all the salt powder into a sealed container and mix it again. Then test the color value according to the national standard method, compare it with the initial color value, determine the loss rate, and evaluate the stability. Loss rate = (initial color value-color value after placement) / initial color value × 100%, the results are shown in Table 1.

[0055] Method for determining the low-temperature fluidity of capsanthin: 100.0 g of capsanthin was placed in a 5±1°C constant temperature device for 48 hours, and then the viscosity was tested. The specific method was based on the international standard GB / T10247-2008 for viscosity measurement, and the measurement was performed by the rotation method. The results are shown in Table 2.

[0056] Table 1 Final pigment stability of each embodiment and comparative example Table 2 Low temperature fluidity of capsanthin in various embodiments and comparative examples Although the present invention has been described in detail above with general descriptions and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements may be made thereto based on the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A method for refining capsanthin, characterized in that: include: (1) subjecting the capsanthin to be purified to a first supercritical carbon dioxide extraction, and after the impurities are discharged from the separation kettle, the pressure is increased to conduct a second supercritical carbon dioxide extraction, and the capsanthin A is collected from the separation kettle; The temperature of the first supercritical carbon dioxide extraction and the second supercritical carbon dioxide extraction is 50-55° C.; the pressure of the first supercritical carbon dioxide extraction is 15-20 MPa, and the pressure of the second supercritical carbon dioxide extraction is 25-30 MPa; (2) subjecting the capsanthin A to a temperature rise and fall treatment: First, the capsanthin A is heated to 43±3°C to fully dissolve, then cooled to 5±2°C, and then heated to room temperature; or, after cooling to 5±2°C, the temperature is repeatedly raised and lowered, each time the temperature is lower than the previous temperature, and each time the temperature is lowered, the temperature is finally raised to room temperature; during the temperature raising and lowering treatment, the temperature is kept for 0.5-1.5 hours after each heating and cooling; (3) Separate and remove impurities.

2. The method according to claim 1, characterized in that In step (2), during the temperature rise and fall treatment, the temperature rise and fall rates after sufficient dissolution are 0.09-0.11°C / min; the temperature rise and fall treatment is always carried out under stirring, and the stirring rate is 10-20 rpm.

3. The method according to claim 1 or 2, characterized in that: In step (2), the temperature is repeatedly raised and lowered 1 to 3 times.

4. The method according to any one of claims 1 to 3, characterized in that: During the first supercritical carbon dioxide extraction and the second supercritical carbon dioxide extraction, the mass ratio of the capsanthin to be purified to the flow rate of carbon dioxide is 1: (10-15) kg: L / h; the time of the first supercritical carbon dioxide extraction is 1.0-1.5h, and the time of the second supercritical carbon dioxide extraction is 4-6h.

5. The method according to any one of claims 1 to 4, characterized in that: The separation pressure of the separation kettle is 5-10 MPa, and the separation temperature is 30-40°C.

6. The method according to any one of claims 1 to 5, characterized in that: In step (3), the method of separating and removing impurities is centrifugation or filtration.

7. The method according to any one of claims 1 to 6, characterized in that: In step (2), when the temperature is repeatedly raised and lowered, each heating temperature is 5±1°C lower than the previous heating temperature, and each cooling temperature is 5±1°C higher than the previous cooling temperature.

8. The method according to any one of claims 1 to 7, characterized in that: In step (2), the capsanthin A is first heated to 43±3°C and stirred until fully dissolved, then cooled to 5±2°C at a rate of 0.09-0.11°C / min, stirred for 1.0-1.5h, then heated to 40±2°C at a rate of 0.09-0.11°C / min, stirred for 20-30min, then cooled to 10±2°C at a rate of 0.09-0.11°C / min, stirred for 1.0-1.5h, then heated to 35±2°C at a rate of 0.09-0.11°C / min, stirred for 20-30min, then cooled to 15±2°C at a rate of 0.09-0.11°C / min, stirred for 1.0-1.5h, then heated to 23-25°C at a rate of 0.09-0.11°C / min and stirred for 1.0-1.5h.

9. A capsanthin, characterized in that The method is obtained by refining according to any one of claims 1 to 8.

10. Use of the method according to any one of claims 1 to 8 in improving the stability and / or low-temperature fluidity of capsanthin.

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