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, and the product is in a viscous liquid state and can also be powdered after drying. It is insoluble in water and has good thermal stability, acid and alkali resistance, spin-rotation resistance and emulsification dispersion. The solution of pepper pigments can present dark red, orange, yellow, pale yellow and other colors due to different concentrations; because it contains carotene, B-carotene and various vitamins, it has a rich nutritional value, so the pepper pigment 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.) soaked in the skin of chili peppers or paprika, after which the pigments dissolved in the oil are separately produced. It is difficult for oil and pigment to obtain dense pigments.

Solvent method, according to the operation method can be divided into impregnation method, osmotic method, reflux extraction method and Soxhlet extraction method, that is extracted with alkyl ketone or hydrocarbon pigment. The quality of the pigment obtained by this method is not consolidating, poor in purity, low in concentration, or difficult to remove spicy taste; it may also firstly damage the element to remove the spicy taste, and thereafter extract the non-spicy pigment, which is extracted from the residue after 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 to achieve a wide range of production.

A solution of alkaline solution - solvent extraction - steam distillation

In order to eliminate the drawbacks of the above extraction methods, researchers have conducted comprehensive experimental studies on the extraction methods of pepper pigments at home and abroad for many years. They believe that the use of aqueous alkali solution-solvent extraction-steam distillation method can produce excellent color and high purity. Consolidate good chili pigments. The specific method is described as follows:

1. Process flow: Pepper extract Distillation Pepper oleoresin Hydrolysis Filtration Solids soaking Vacuum filtration extract Vacuum distillation Pigment steam distillation Concentrate Refined pigment Dry powdered chili pepper pigment

2, extraction method

(1) Extract pepper oleoresin. After the mature pepper fruit is dried and crushed, it is put into an extraction tank and continued to be extracted with organic solvents (such as ethanol, acetone, 2-propanol, trichloroethylene, and 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, mixing time 1-10 hours. After that, put it stillly, and adopt decantation or liquid-liquid centrifugation to separate out the pigment phase containing the pepper; thereafter, steam distillation is performed under normal pressure or vacuum, and residual alcohol is distilled off to obtain a resin containing pepper pigment.

(2) Alkaline solution solution. After distilling, the resin containing pepper pigment was added and the solution of alkali solution was added. The concentration of the aqueous alkali solution is about 45%, and the addition amount is 3 to 5 times the weight of the distilled resin, the temperature is 80° C., and the stirring time is 3 to 10 hours. Afterwards, the pH is adjusted between 4 and 6.5 so that the fatty acids contained in the pepper pigment resin are converted from free-radical alkali salts to free fatty acids; the pH adjusting agent is a commonly used inorganic or organic acid. After the acid is adjusted, the accumulating agent is added slowly so that the free fatty acids are converted into insoluble or insoluble salts to produce a deposit; the depressant includes barium hydroxide, magnesium hydroxide, calcium hydroxide, and the like. 2-8 times the weight of chili oil resin. After the accumulation, a soap-like solid is obtained by centrifugation or filtration.

(3) extraction. The soap and alkali solids are placed in an extraction tank and organic solvents are added for continuous extraction. The organic solvents include petroleum ether such as acetone, methyl ethyl ketone, 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 conditions, and the organic solvent was distilled off to obtain a colorant of 380,000 to 650,000 red pepper pigments. 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. After the water is filtered out, it is monotonous in a vacuum monotonator to obtain a concentrated and refined pigment; or it can be dried at a low temperature to obtain a powdered chilli pigment.

Second, CO2 supercritical extraction method

In addition to the above methods, there is currently a supercritical extraction method in the world. 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 this method is:

Paprika extraction tanks separate rough pigment extraction tanks respectively

The specific operation is as follows: the pepper is dried and crushed and placed in an extraction tank, CO2 with a pressure of 12 mPa is fed at a flow rate of 5 L/min, the extraction tank temperature is 40° C., the above-mentioned CO2 pressure is maintained for 60 min, CO2 is introduced into the respective tanks, and The pressure was reduced to atmospheric pressure to obtain a spicy extract with a pigment content of about 8%. The extract was then placed in an extraction tank, and a CO2 pressure of 45 mPa was introduced at a flow rate of 5 L/min. The tank temperature was 40° C., and the extraction time was 40 min. Then, the extract was placed in a separate tank and depressurized to atmospheric pressure to obtain no spicy food. Flavored chili pigments.

Third, the difference of pepper pigment

The color of pepper can be varied in color with different concentrations. For example, when edible alcohol dissolves at 1:15, it is red when added at 1/5000, orange when it is 1/8000, and yellow when it is 1/12000. In recent years, the use of column chromatography to directly separate the pepper pigments into single pigments such as black, yellow, red, and orange, these single pigments have good thermal constancy. After heating at 100°C for several hours, the residual rate of pigments is About 95%, and there is a good spin-rotation.

The specific method is as follows: In a glass column filled with silica gel, a concentrated pepper pigment is added, and the ratio of silica gel and pepper pigment addition is 5:1, after which it is eluted with n-hexane, and n-hexane is distilled from the eluent. 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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2022-12-29

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