Preparation method of capsanthin

Abstract

The invention relates to the technical field of natural pigment extraction, in particular to a preparation method of capsanthin. According to the preparation method of the capsanthin provided by the invention, an organic solvent is not used, a relatively high capsanthin extraction yield can be realized, the prepared capsanthin is relatively high in color value and free of solvent residues and can be applied to scenes such as food and cosmetics, and the safety and the application value of a capsanthin product are improved; and the method has the advantages of simple operation, high efficiency, environmental protection and the like, and provides a new method for industrial production of the capsanthin.

Description

Technical Field

[0001] The present invention relates to the technical field of natural pigment extraction, and particularly to a method for preparing capsanthin. Background Art

[0002] Capsanthin (also known as "chili red") is a natural pigment that is widely used in industries such as food and cosmetics due to its bright color, good stability, and non-toxic side effects. The preparation process of capsanthin directly affects the quality and application effect of the pigment. Traditional methods for preparing capsanthin often use organic solvents for extraction, which not only have complex operations and poor environmental protection, but also have the problem of solvent residues, affecting the safety of the pigment. Therefore, it is of great significance to develop a method for preparing capsanthin without solvent residues and with high efficiency and environmental protection.

[0003] Chinese Patent Application CN117264436A extracts capsanthin by enzymatic hydrolysis combined with subcritical countercurrent extraction. Although it has a high extraction rate, it requires the use of butane as an extraction agent in the subcritical extraction step, and involves complex processes and high costs. Chinese Patent Application CN110396305A uses organic solvents such as tetrahydrofuran for Soxhlet extraction, which has the risk of solvent residues and environmental pollution. Summary of the Invention

[0004] The present invention provides a method for preparing capsanthin.

[0005] In view of the problem that the existing methods for extracting capsanthin generally rely on organic solvent extraction and thus have solvent residues, the present invention has developed a method for preparing capsanthin without organic solvents. This method does not rely on organic solvent extraction, but uses a water extraction method, thereby achieving no solvent residues and greatly improving the safety of the prepared pigment. During the research and development process, the present invention found that the extraction yield is relatively low when water and chili powder are simply mixed and then stirred for extraction under certain temperature conditions, and unexpectedly found that the mixing step of water and chili powder has a great influence on the extraction yield of capsanthin. After continuous attempts, it was determined that the chili powder and water are mixed multiple times under different temperature conditions in sequence, and combined with high-speed shear extraction, the yield and color value of capsanthin can be significantly improved. In addition, the present invention also found that after water extraction using the above method, further controlling the pH of the obtained capsanthin mixture can further improve the yield and color value of capsanthin.

[0006] Specifically, the present invention provides the following technical solutions.

[0007] The present invention provides a method for preparing capsanthin, the method comprising: mixing chili powder and water and then performing extraction to obtain an extract, adjusting the pH of the extract to 5 - 7; then separating and collecting the supernatant to obtain a capsanthin extract; Among them, mixing chili powder with water includes a first stirring and mixing treatment, a second stirring and mixing treatment, and a third stirring and mixing treatment. The temperature of the first stirring and mixing treatment is 25 - 35°C, the temperature of the second stirring and mixing treatment is 40 - 45°C, and the temperature of the third stirring and mixing treatment is 50 - 55°C.

[0008] Due to the oil-soluble property of capsanthin, using water as the extraction solvent will seriously affect its extraction effect. Through a large number of practices, the present invention proves that mixing chili powder with water through the above mixing procedure can effectively promote the release of capsanthin from the cell structure, and combined with high-shear extraction, it overcomes the problem of low solubility of capsanthin in the aqueous phase, significantly improving the extraction yield. Compared with directly mixing chili powder and water in one step or through other temperature gradient mixing treatments, using the above mixing procedure can effectively improve the extraction yield of capsanthin and the color value of the extraction product.

[0009] Preferably, the temperature of the first stirring and mixing treatment is 25 - 30°C, the temperature of the second stirring and mixing treatment is 40 - 45°C, and the temperature of the third stirring and mixing treatment is 50 - 55°C.

[0010] The above-described method for preparing capsanthin does not use organic solvents.

[0011] The present invention extracts capsanthin with water and does not use organic solvents during the extraction process, which can avoid the residue of organic solvents in the extraction product and improve the safety of the prepared capsanthin. The above organic solvents include but are not limited to ethanol, acetone, tetrahydrofuran, butane, etc. commonly used in the extraction of capsanthin.

[0012] In the above method, in the mixing of chili powder and water, the material-liquid ratio of chili powder to water is 1 g:1 - 6 mL. Preferably, it is 1 g:3 - 5 mL.

[0013] Preferably, the time for each mixing treatment is 0.5 - 2 h. The stirring speed for each mixing treatment is 200 - 500 r / min.

[0014] Preferably, the stirring speed of the first stirring and mixing treatment is 200 - 250 r / min; the stirring speed of the second stirring and mixing treatment is 300 - 350 r / min; the stirring speed of the third stirring and mixing treatment is 400 - 450 r / min.

[0015] Preferably, the time of the first stirring and mixing treatment is 0.5 - 1 h, the time of the second stirring and mixing treatment is 0.5 - 1 h, and the time of the third stirring and mixing treatment is 1.5 - 2 h.

[0016] In some embodiments of the present invention, chili powder is mixed with water at a material-liquid ratio of 1 g: 1-6 mL. The mixing is carried out by three stirring and mixing processes in sequence. Among them, the temperature of the first stirring and mixing process is 25-35 °C, the stirring speed is 200-250 r / min, the time is 0.5-1 h, the temperature of the second stirring and mixing process is 40-45 °C, the stirring speed is 300-350 r / min, the time is 0.5-1 h, the temperature of the third stirring and mixing process is 50-55 °C, the stirring speed is 400-450 r / min, and the time is 1.5-2 h.

[0017] In the above method, after mixing chili powder and water, an extraction operation is carried out. After the extraction is completed, the pH of the extract is adjusted to 5-7.

[0018] After the extraction is completed, the pH of the capsanthin mixture is generally 7.2-9. The present invention finds that adjusting the pH of the extract to 5-7 after the extraction is completed can inhibit the oxidation reaction. If the pH of the extract is higher or lower than the above range, it will cause the decomposition of capsanthin, thereby reducing the color value and yield of the capsanthin obtained.

[0019] Preferably, an acidic pH regulator is used to adjust the pH of the extract to 5-7. The acidic pH regulator can be selected from one of vitamin C or its aqueous solution, citric acid or its aqueous solution, acetic acid or its aqueous solution, hydrochloric acid or its aqueous solution.

[0020] Preferably, the extraction is carried out under high-speed shearing conditions.

[0021] The above high-speed shearing conditions can be achieved by using a high-shear homogenizer or a grinder, that is, the extraction can be carried out by using a high-shear homogenizer or a grinder.

[0022] Preferably, the temperature of the extraction is 40-60 °C (more preferably 50-60 °C). The time of the extraction is 2-6 h (more preferably 4-5 h).

[0023] The number of times of the above extraction can be one or more, for example, it can be 1-5 times, preferably 1-3 times.

[0024] For the chili powder raw material, preferably the water content of the chili powder is 8%-12%.

[0025] The present invention finds that compared with using chili powder raw materials with other water contents, controlling the water content of the chili powder raw material at 8%-12% is more conducive to improving the extraction yield of capsanthin.

[0026] Preferably, the color value of the chili powder raw material is not less than E8.0. Preferably it is E8.0-E20.0.

[0027] In the above method, the supernatant is separated and collected by centrifugation. The purpose of separation is to remove the incompletely extracted capsicum components and impurities. The preferred centrifugation conditions are 3500 - 4500 r / min and the centrifugation time is 0.5 - 1 h.

[0028] The above method further includes the step of concentrating the capsanthin extract to obtain capsanthin.

[0029] For the concentration method, the present invention has no special limitation, and common concentration methods such as rotary evaporation concentration can be used.

[0030] The beneficial effects of the present invention at least include: The capsanthin preparation method provided by the present invention does not use organic solvents, can achieve a high extraction rate of capsanthin, the color value of the obtained capsanthin is high, there is no solvent residue, and it can be applied to scenarios such as food and cosmetics, improving the safety and application value of capsanthin products; and this method has advantages such as simple operation, high efficiency and environmental protection, providing a new method for the industrial production of capsanthin. Detailed Embodiments

[0031] To make the objectives, technical solutions and advantages of the present invention clearer, the technical solutions in the present invention will be clearly and completely described below. Obviously, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0032] In the following embodiments, the calculation formula for the extraction rate of capsanthin is: Extraction rate of capsanthin = (Color value of capsanthin × Weight of capsanthin) / (Color value of pepper particles × Weight of pepper particles).

[0033] Example 1 (1) Place 100 g of chili powder with a color value of E15.0 and a water content of 10% in an extraction container; (2) Add 500 mL of water to the extraction container and perform the first stirring and mixing at 30°C with a stirring speed of 250 r / min and a stirring and mixing time of 0.5 h; then raise the temperature to 40°C for the second stirring and mixing with a stirring speed of 350 r / min and a stirring and mixing time of 1 h; finally raise the temperature to 50°C for the third stirring and mixing with a stirring speed of 400 r / min and a stirring and mixing time of 1.5 h to obtain a chili powder mixture sample; (3) Extract 600 g of the chili powder mixture sample prepared in step (2) with a high-shear homogenizer at 50°C for 4 h, and then adjust the pH of the extract to 6 with an aqueous VC solution to obtain a capsanthin mixture sample; (4)Centrifuge 600 g of the capsanthin mixed sample prepared in step (3) (at 4000 r / min for 30 min) to remove incompletely extracted capsicum components and impurities, and collect the supernatant as the capsanthin extract; (5)Concentrate 207 g of the capsanthin extract to obtain 7 g of solvent-free residual capsanthin, with a color value E180 and a extraction yield of 84%.

[0034] Example 2: (1)Place 200 g of chili powder with a color value E13.0 and a water content of 11% in an extraction container; (2)Add 600 mL of water to the extraction container and conduct the first stirring and mixing at 25 °C, with a stirring speed of 200 r / min and a stirring and mixing time of 1 h; then raise the temperature to 45 °C for the second stirring and mixing, with a stirring speed of 300 r / min and a stirring and mixing time of 0.5 h; finally raise the temperature to 55 °C for the third stirring and mixing, with a stirring speed of 450 r / min and a stirring and mixing time of 2 h to obtain a chili powder mixed sample; (3)Extract 800 g of the chili powder mixed sample prepared in step (2) with a high-shear homogenizer at 60 °C for 5 h, and then adjust the pH of the extract to 7.0 with an acetic acid aqueous solution to obtain a capsanthin mixed sample; (4)Centrifuge 800 g of the capsanthin mixed sample prepared in step (3) (at 4000 r / min for 1 h) to remove incompletely extracted capsicum components and impurities, and collect the supernatant as the capsanthin extract; (5)Concentrate 310 g of the capsanthin extract to obtain 10 g of solvent-free residual capsanthin, with a color value E220 and a extraction yield of 85%.

[0035] Comparative Example 1 (1)Place 200 g of chili powder with a color value E13.0 and a water content of 11% in an extraction container; (2)Add 600 mL of water to the extraction container and stir and mix at 40 °C for 3.5 h, with a stirring speed of 450 r / min to obtain a chili powder mixed sample; (3)Extract 800 g of the chili powder mixed sample prepared in step (2) with a high-shear homogenizer at 60 °C for 5 h, and then adjust the pH of the extract to 7.0 with an acetic acid aqueous solution to obtain a capsanthin mixed sample; (4)Centrifuge 800 g of the capsanthin mixed sample prepared in step (3) (at 4000 r / min for 1 h) to remove incompletely extracted capsicum components and impurities, and collect the supernatant as the capsanthin extract; (5)Concentrate 110 g of the capsanthin extract to obtain 5 g of solvent-free residual capsanthin, with a color value E150 and a extraction yield of 29%.

[0036] Comparative Example 2 (1) Place 200 g of chili powder with a color value of E13.0 and a water content of 11% in an extraction container; (2) Add 600 mL of water to the extraction container and conduct the first stirring and mixing at 20°C with a stirring speed of 200 r / min and a stirring and mixing time of 1 h; then raise the temperature to 55°C for the second stirring and mixing with a stirring speed of 300 r / min and a stirring and mixing time of 0.5 h; finally raise the temperature to 65°C for the third stirring and mixing with a stirring speed of 450 r / min and a stirring and mixing time of 2 h to obtain a chili powder mixture sample; (3) Extract 800 g of the chili powder mixture sample prepared in step (2) with a high-shear homogenizer at 60°C for 5 h, and then adjust the pH of the extract to 7.0 with an acetic acid aqueous solution to obtain a capsanthin mixture sample; (4) Centrifuge 800 g of the capsanthin mixture sample prepared in step (3) (4000 r / min, centrifugation time 1 h) to remove the incompletely extracted chili components and impurities, and collect the supernatant as the capsanthin extract; (5) Concentrate 180 g of the capsanthin extract to obtain 15.9 g of solvent-free residual capsanthin with a color value of E80 and a extraction yield of 49%.

[0037] Comparative Example 3 (1) Place 200 g of chili powder with a color value of E13.0 and a water content of 11% in an extraction container; (2) Add 600 mL of water to the extraction container and conduct the first stirring and mixing at 65°C with a stirring speed of 200 r / min and a stirring and mixing time of 1 h; then lower the temperature to 35°C for the second stirring and mixing with a stirring speed of 300 r / min and a stirring and mixing time of 0.5 h; finally lower the temperature to 15°C for the third stirring and mixing with a stirring speed of 450 r / min and a stirring and mixing time of 2 h to obtain a chili powder mixture sample; (3) Extract 800 g of the chili powder mixture sample prepared in step (2) with a high-shear homogenizer at 60°C for 5 h, and then adjust the pH of the extract to 7.0 with an acetic acid aqueous solution to obtain a capsanthin mixture sample; (4) Centrifuge 800 g of the capsanthin mixture sample prepared in step (3) (4000 r / min, centrifugation time 1 h) to remove the incompletely extracted chili components and impurities, and collect the supernatant as the capsanthin extract; (5) Concentrate 160 g of the capsanthin extract to obtain 15.25 g of solvent-free residual capsanthin with a color value of E75 and a extraction yield of 44%.

[0038] Comparative Example 4 (1) Place 200 g of chili powder with a color value of E13.0 and a water content of 11% in an extraction container; (2) Add 600 mL of water to the extraction container and conduct the first stirring and mixing at 25°C, with a stirring speed of 200 r / min and a stirring and mixing time of 1 h; then raise the temperature to 45°C for the second stirring and mixing, with a stirring speed of 300 r / min and a stirring and mixing time of 0.5 h; finally, raise the temperature to 55°C for the third stirring and mixing, with a stirring speed of 450 r / min and a stirring and mixing time of 2 h to obtain a chili powder mixture sample; (3) Use a high-shear homogenizer to extract 800 g of the chili powder mixture sample prepared in step (2) at 60°C for 5 h to obtain a capsanthin mixture sample with a pH of 8.3; (4) Centrifuge 800 g of the capsanthin mixture sample prepared in step (3) (4000 r / min, centrifugation time 1 h) to remove incompletely extracted chili components and impurities, and collect the supernatant as the capsanthin extract; (5) Concentrate 200 g of the capsanthin extract to obtain 20.8 g of solvent-free residual capsanthin, with a color value of E60 and an extraction yield of 48%.

[0039] Comparative Example 5 (1) Place 200 g of chili powder with a color value of E13.0 and a water content of 11% in an extraction container; (2) Add 600 mL of water to the extraction container and conduct the first stirring and mixing at 25°C, with a stirring speed of 200 r / min and a stirring and mixing time of 1 h; then raise the temperature to 45°C for the second stirring and mixing, with a stirring speed of 300 r / min and a stirring and mixing time of 0.5 h; finally, raise the temperature to 55°C for the third stirring and mixing, with a stirring speed of 450 r / min and a stirring and mixing time of 2 h to obtain a chili powder mixture sample; (3) Use a high-shear homogenizer to extract 800 g of the chili powder mixture sample prepared in step (2) at 60°C for 5 h, and then adjust the pH of the extract to 10.0 with an aqueous sodium hydroxide solution to obtain a capsanthin mixture sample; (4) Centrifuge 800 g of the capsanthin mixture sample prepared in step (3) to remove incompletely extracted chili components and impurities, and collect the supernatant as the capsanthin extract; (5) Concentrate 150 g of the capsanthin extract to obtain 13.43 g of solvent-free residual capsanthin, with a color value of E60 and an extraction yield of 31%.

[0040] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the various embodiments of the present invention.

Claims

1. A method for preparing capsanthin, characterized in that, The method includes: mixing chili powder with water and then performing extraction to obtain an extract, and adjusting the pH of the extract to 5 - 7; then separating and collecting the supernatant to obtain a capsanthin extract solution; Among them, mixing chili powder with water includes a first stirring and mixing treatment, a second stirring and mixing treatment, and a third stirring and mixing treatment. The temperature of the first stirring and mixing treatment is 25 - 35°C, the temperature of the second stirring and mixing treatment is 40 - 45°C, and the temperature of the third stirring and mixing treatment is 50 - 55°C.

2. The preparation method according to claim 1, characterized in that, The method does not use organic solvents.

3. The preparation method of capsanthin according to claim 1 or 2, characterized in that, In the mixing of chili powder and water, the material - liquid ratio of chili powder to water is 1g:1 - 6mL.

4. The preparation method of capsanthin according to any one of claims 1 to 3, characterized in that The time for each mixing treatment is 0.5 - 2h, and / or the stirring speed for each mixing treatment is 200 - 500r / min.

5. The preparation method of capsanthin according to claim 4, characterized in that, The stirring speed of the first stirring and mixing treatment is 200 - 250r / min; the stirring speed of the second stirring and mixing treatment is 300 - 350r / min; the stirring speed of the third stirring and mixing treatment is 400 - 450r / min; and / or, the time of the first stirring and mixing treatment is 0.5 - 1h, the time of the second stirring and mixing treatment is 0.5 - 1h, and the time of the third stirring and mixing treatment is 1.5 - 2h.

6. The preparation method of capsanthin according to any one of claims 1 to 5, characterized in that, The extraction is carried out under high - speed shearing conditions.

7. The preparation method of capsanthin according to claim 6, characterized in that, The temperature of the extraction is 40 - 60°C.

8. The method for preparing capsanthin according to claim 6 or 7, characterized in that, The time of the extraction is 2 - 6h.

9. The preparation method of capsanthin according to any one of claims 1 to 8, characterized in that, The water content of the chili powder is 8% - 12%.

10. The preparation method of capsanthin according to any one of claims 1 to 9, characterized in that, The method further includes the step of concentrating the capsanthin extract solution to obtain capsanthin.