Extraction process of pepper pigment

The pepper pigment is a red-orange natural food colorant extracted from peppers using a high carotenoid system. The pigment belongs to the anthraquinone pigment. The product is a viscous liquid, and it can also be powdered after drying. It is insoluble in water and has good thermal stability, acid and alkali resistance, lightfastness, and emulsifying and dispersing properties. The solution of pepper pigment can present dark red, orange, yellow, light yellow and other colors due to different concentrations; because it contains carotene, β-carotene and various vitamins, it has rich nutritional value, therefore, the color of pepper can be It is widely used in the coloring of industrial products such as food, medicine and cosmetics. The extraction of pepper pigments was first carried out using oil-soluble and solvent methods. Oil-dissolving method, that is, the use of animal and vegetable oils (such as fish oil, cottonseed oil, soybean oil, vegetable oil, coconut oil, corn oil, etc.) soaking chili skin or chili powder, and then separating the pigment dissolved in oil, the disadvantages of this method It is difficult to separate the oil from the pigment and it is difficult to obtain a thick pigment. Solvent method can be divided into impregnation method, percolation method, reflux extraction method and Soxhlet extraction method according to the operation mode, that is, the pigment is extracted with alkyl ketone or hydrocarbon. The pigment obtained by this method is unstable in quality, poor in purity, low in concentration, or difficult to remove spicy taste; it can also first destroy the pungent element to remove the pungent taste and then extract it into a non-spicy pigment, which is extracted from the residue of this method. A considerable amount of red pigment still remains, and the resulting crude product has a high impurity content, is expensive to purify, and has poor usability of the residue, making it difficult for large-scale production. First, the aqueous alkali solution treatment - solvent extraction - steam distillation method In order to eliminate the drawbacks of the above extraction method, the researchers conducted a comprehensive experimental study on the domestic and foreign pepper pigment extraction methods, that the use of alkaline solution - Solvent Extraction - Steam distillation produces excellent chili pigments with good color, high purity and good stability. The specific methods are described as follows: 1. Process flow: peppers → extraction → distillation → capsicum oleoresin → hydrolysis → filtration → solids → soaking → vacuum filtration → extracts → vacuum distillation → pigments → steam distillation → concentration Refined Pigment→Drying→Powdered Pepper Pigment 2、Extraction Method (1) Extraction of capsicum oleoresin. After the mature pepper fruit is dried and crushed, it is put into an extraction tank and continuously extracted with an organic solvent (such as ethanol, acetone, 2-propanol, trichloroethylene, ethane, etc.) from the extract at room temperature. Distill the organic solvent, and then extract the pepper oleoresin with a lower aliphatic alcohol solvent (such as methanol, ethanol, propanol, isopropanol, etc.), the amount of which is about 10 times that of the pepper oleoresin, and the temperature is room temperature to the alcohol. The boiling point, stirring time 1-10 hours. After that, it is left to stand still, and decantation or liquid-liquid centrifugation is used to separate out the pigment phase containing the pepper; then, steam distillation is performed under normal pressure or vacuum, and residual alcohol is distilled off to obtain a resin containing pepper pigment. (2) Aqueous alkali treatment. After the distillation, the pigment containing the pepper pigment was added and treated with an aqueous alkali solution. The concentration of the aqueous alkali solution is about 45%, and the addition amount is equivalent to 3 to 5 times the weight of the distilled resin, the temperature is 80° C., and the stirring time is 3 to 10 hours. The pH is then adjusted between 4-6.5 to convert the fatty acids contained in the chilli pigment resin from the water-soluble basic salt form to free fatty acids; the pH adjusting agent is a common inorganic or organic acid. After the acid is adjusted, the precipitant is gradually added to convert the free fatty acids into insoluble or insoluble salts to form precipitates; the precipitant includes cesium hydroxide, magnesium hydroxide, calcium hydroxide, and the like. 2-8 times the weight of chili oil resin. After precipitation, soap-like solids are obtained by centrifugation or filtration. (3) extraction. The soap-like solids were placed in an extraction tank and organic solvents were added for continuous extraction. The organic solvents were petroleum ether such as acetone, butanone, methyl acetate, methanol, ethanol, propanol, pentane, benzene, toluene, and diethyl ether. class. The amount of organic solvent added is equivalent to 1-15 times the weight of solids, the temperature is controlled at room temperature, and the extraction time is about 1-15 hours depending on the choice of solvent. (4) Distillation. The extract (removal of the residue) was distilled under constant pressure or vacuum, and the organic solvent was distilled off to obtain a colorant with a color value of 30-650000. If the obtained pigment still has the peculiar smell of pepper, the pigment is depressurized at about 26.7 kPa, and the steam is distilled for 4 hours to remove the odor. The water is filtered off and then dried in a vacuum desiccator to obtain a concentrated and purified pigment. Alternatively, it can be dried at a low temperature to obtain a powdered chilli pigment. Second, CO2 supercritical extraction In addition to the above methods, the current world is also popular with supercritical extraction. Compared with the traditional method, using CO2 supercritical extraction method avoids the use of organic solvents, eliminating the need for distillation and other operating steps, is a very promising extraction method. The extraction process of the method is: chili powder → extraction tank → separation tank → coarse pigment → extraction tank → separation tank → pigment The specific operations are as follows: The pepper is dried and crushed and placed in an extraction tank, and the flow rate is 5 L/min. At a pressure of 12 mPa CO2, the extraction tank temperature was 40°C, the above CO2 pressure was maintained for 60 min, CO2 was introduced into the separation tank, and the pressure was reduced to atmospheric pressure to obtain a spicy extract having a pigment content of about 8%. The extract was then placed in an extraction tank and CO2 at a pressure of 45 mPa was fed at a flow rate of 5 L/min. The tank temperature was 40° C. and the extraction time was 40 min. Then the separation tank was introduced and the pressure was reduced to atmospheric pressure to obtain a non-spicy taste. Chili pepper pigments. Third, the separation of pepper pigments Pepper pigment with different concentrations can be a variety of colors, such as: Edible ethanol dissolved in 1:15, the amount of 1/5000 when the red, 1/8000 orange, 1/12000 It is yellow. In recent years, column chromatography has also been used to directly separate the pepper pigments into single pigments such as black, yellow, red, orange, etc. These single pigments have good thermal stability. After heating for several hours at 100° C., the residual rate of pigments is About 95%, and have good lightfastness. The specific method is as follows: In a glass column filled with silica gel, add the concentrated pepper pigment, the ratio of the additive of silica gel and pepper pigment is 5:1, then elute with n-hexane, n-hexane is distilled from the eluate. First, melanin can be obtained; then eluted with 5% isopropyl ether and 95% n-hexane, the solvent is distilled off in the eluent to obtain a yellow pigment; then eluted with 25% isopropyl ether and 75% n-hexane, The solvent was distilled off in the eluent to obtain the red pigment, and finally eluted with acetone. After the acetone was distilled off, the orange pigment was obtained.

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