CN101210113A - Preparation method of oil-soluble citrus yellow pigment - Google Patents

Abstract

The invention discloses a preparation method of oil-soluble citrus yellow pigment. The oil-soluble citrus yellow pigment is obtained through acid hydrolysis, enzymatic hydrolysis and leaching by using orange peel dry powder as a raw material. The preparation method adopts an enzymatic hydrolysis method to first enzymatically hydrolyze the citrus pectin, and then extract the yellow pigment, which can greatly save the loss of the extraction agent and significantly reduce the cost. The product is a natural pigment, non-toxic and pollution-free, suitable for use as a colorant for oily foods, replacing artificial pigments.

Description

Preparation method of oil-soluble citrus yellow pigment

technical field

The invention relates to a preparation method of yellow pigment, in particular to a preparation method of oil-soluble citrus yellow pigment which can be directly dissolved in edible oil.

Background technique

Food coloring is an indispensable additive in food industry, pharmaceutical industry and daily chemical industry. In recent years, due to safety issues, some synthetic pigments are no longer suitable for the food industry. Therefore, the development of natural pigments has attracted increasing attention.

Invention patent No. 01131293.9 "a pectin oligosaccharide, its preparation process and application of plant disease prevention and control" introduced the method of pectinase degradation to prepare pectin oligosaccharides with a polymerization degree of 2-20. Gum oligosaccharides can be used to prevent and control plant diseases such as vegetables and fruit melons by spraying or soaking roots. The method for preparing pectin oligosaccharides by enzymatic hydrolysis with pectinase greatly shortens the reaction time and improves the production efficiency.

Patent No. 03812467.X's invention patent "Oil-Soluble Pigment Synthesis" introduces a method for preparing an oily solution of carotenoids. This method prepares a solid carotenoid-containing composition and a carotenoid-containing The solution with organic solvent can be better dissolved in oily mixture. This kind of pigment has low color price, high loss of reagents, high cost, and is a synthetic product, which is restricted in the food field.

The invention patent No. 87101355 "method of extracting pigment and volatile oil from turmeric" introduces that the Chinese herbal medicine turmeric is used as the starting material, and after pretreatment, the volatile oil of turmeric is first collected by distillation, then extracted with a solvent, and refined to obtain a powder Turmeric. This coloring may contain a pungent taste.

Patent No. 200310111453.3, "A Preparation Method of Gardenia Yellow Pigment", discloses that the dried gardenia fruit is air-dried, crushed, added with petroleum ether, ultrasonically extracted, then ultrasonically extracted with ethanol, filtered, and passed through two columns Chromatographic separation, resulting in gardenia yellow pigment. The technological process of this method is more loaded down with trivial details, and cost is high.

The invention patent No. 92110381.6 "Method for Simultaneously Extracting Natural Yellow Pigment, Orange Oil and Pectin from Citrus Peel" discloses all physical methods and non-toxic reagent petroleum ether for extraction, which has high yellow quality. , Preserving the original natural ingredients in the orange peel. Hydrolyzate is a high-quality dietary fiber. However, this method does not enzymatically hydrolyze the pectin before extracting the pigment, which leads to the problem of high viscosity of the solution during the extraction process and the problem of excessive adsorption of residual solvent in the residue, which leads to more loss of reagents and high cost.

These pigments have defects such as high production cost and inconvenient practical application.

Contents of the invention

The purpose of the present invention is to explore the preparation method of extracting oil-soluble citrus yellow pigment by pectinase hydrolysis, so as to overcome the high cost in the process of preparing citrus yellow pigment, the high viscosity of the solution in the extraction process, and the low added value of resource utilization. defect.

The preparation method of oil-soluble citrus yellow pigment of the present invention comprises the following steps:

1, with 50～200 order orange peel dry powders with a moisture content of 5～10% as raw material, mix the two by the method that every milliliter of dilute hydrochloric acid mixes with 3～12 grams of orange peel dry powders, the pH of described dilute hydrochloric acid Value 3~6; acid hydrolyze at 20~30°C for 10~150min, then filter, collect the filter residue after acid hydrolysis, dry at 40~60°C to obtain dry filter residue for later use, and recover the filtrate for other use;

2, get the dry filter residue of step 1 and add pectinase, and its addition is that every gram of dry filter residue adds 0.005～0.02 gram of pectinase; Get the hydrochloric acid of pH3.5～5.0 as extraction solution, add the above-mentioned pectinase and filter residue For enzymolysis in the mixture, the amount added is 6-12 ml of extract per gram of dry filter residue, the enzymolysis time is 10-90 minutes, and the enzymolysis temperature is 30°C-70°C; Dry at ~60°C to obtain a dry filter residue, and recover the filtrate for other uses;

3. Take the dry filter residue after enzymolysis in step 2 and add petroleum ether or diethyl ether for leaching. The amount added is 7-15 ml of petroleum ether or diethyl ether per gram of dry filter residue; the leaching time is 1.5-8.5 hours, and the leaching temperature is 15 ~30°C, to obtain petroleum ether solution of oil-soluble citrus yellow pigment or ether solution of oil-soluble citrus yellow pigment;

4. Distill the petroleum ether solution of the oil-soluble citrus yellow pigment or the ether solution of the oil-soluble citrus yellow pigment in step 3, and discard the evaporated matter to obtain the oil-soluble citrus yellow pigment.

In the preparation method of the oil-soluble citrus yellow pigment of the present invention, the citrus pectin is firstly enzymolyzed by an enzymatic hydrolysis method, and then the yellow pigment is extracted, which can greatly save the loss of the extraction agent and significantly reduce the cost. The product is a natural pigment, non-toxic and pollution-free, and can be used as a yellow coloring agent for food, directly soluble in edible oil and fat-containing food. When used as a food coloring agent, its dosage depends on the variety of food to be colored and the hue and intensity of the required color. It shows absorption in the ultraviolet-visible spectrum, and the maximum absorption wavelength of its oil solution is 330nm. Changing the pH of the solution will not change the hue of the pigment. The pigment has fairly good light and heat stability, and is relatively stable under the action of metal ions aluminum and calcium, and magnesium ions have a color-protecting effect on the oil-soluble orange peel yellow pigment of the invention.

The oil-soluble citrus yellow pigment prepared by the method of the invention is a natural pigment and can be used in various oily foods in combination with other food colorants. For example, cakes, ice cream, marinated products, meat products, pastries, fried, puffed, edible oil, dairy products and other foods. It can replace artificial synthetic pigments.

Detailed ways

In order to fully disclose the oil-soluble citrus yellow pigment of the present invention and its preparation method, the following examples will be used to illustrate.

Embodiment 1: A kind of preparation method of oil-soluble citrus yellow pigment

Add 2 tons of dried orange peel powder with a moisture content of 7% to 20,000L of dilute hydrochloric acid solution with pH 3.5, bathe in 25°C for 2.0 hours, filter, collect the filter residue, and dry at 40°C; take 1 ton of dry filter residue and mix with 10 kg of pectinase Mix well, add 10000L of dilute hydrochloric acid solution with pH4.0, stir well, heat enzymolysis in 50℃ water bath for 80min, collect filter residue, and dry; take 0.5 tons of dry filter residue after enzymolysis, add 6000L petroleum ether at 25℃, fully Extract for 7 hours, repeat the extraction for 3 times, collect the extract, concentrate under reduced pressure to obtain oil-soluble citrus yellow pigment.

Embodiment 2: A kind of preparation method of oil-soluble citrus yellow pigment

Add 20 grams of orange peel dry powder with a moisture content of 7% to 250 ml of a dilute hydrochloric acid solution at pH 4.0, bathe in water at 25°C for 1.5 hours, filter, collect the filter residue, and dry at 40°C; take 10 grams of dry filter residue and mix it with 0.15 gram of pectinase Mix well, add 150ml of dilute hydrochloric acid solution with pH 4.5, stir well, heat enzymolysis in 55°C water bath for 70min, collect filter residue, and dry; take 5g of dry filter residue after enzymolysis, add 55ml of ether at room temperature, fully extract for 5 hours , repeated leaching 3 times, collecting the extract, concentrating under reduced pressure to obtain oil-soluble citrus yellow pigment.

Claims (3)

1. a preparation method of oil-soluble citrus yellow pigment, is characterized in that comprising the following steps: (1) With 50～200 order orange peel dry powders with a moisture content of 5～10% as raw material, the mixed acidolysis of the two is carried out by the method that every milliliter of dilute hydrochloric acid mixes with 3～12 grams of orange peel dry powders, the amount of said dilute hydrochloric acid pH value 3-6; acid hydrolysis at 20-30°C for 10-150 minutes, then filter, collect acid-hydrolyzed filter residue, dry at 40-60°C to obtain dry filter residue for later use, and recover filtrate for other use; (2) Get the dry filter residue of step 1 and add pectinase, the amount of which is to add 0.005 to 0.02 gram of pectinase per gram of dry filter residue; take hydrochloric acid of pH 3.5 to 5.0 as the extract, add the above pectinase and filter residue Enzymolysis in the mixture, the addition amount is to add 6-12 ml of extract per gram of dry filter residue, the enzymolysis time is 10-90min, and the enzymolysis temperature is 30°C-70°C; then filter, collect the filter residue after enzymolysis, and put it in Dry at 40-60°C to obtain dry filter residue, and recover the filtrate for other uses; (3) Get the dry filter residue after enzymolysis in step 2 and add sherwood oil or diethyl ether for leaching, and its addition is to add 7 to 15 milliliters of sherwood oil or diethyl ether per gram of dry filter residue; leaching time 1.5 to 8.5 hours, leaching temperature 15-30°C, to obtain petroleum ether solution of oil-soluble citrus yellow pigment or ether solution of oil-soluble citrus yellow pigment; (4) distilling the petroleum ether solution of the oil-soluble citrus yellow pigment or the ether solution of the oil-soluble citrus yellow pigment in step 3, and discarding the evaporated matter to obtain the oil-soluble citrus yellow pigment. 2. the preparation method of a kind of oil-soluble citrus yellow pigment according to claim 1 is characterized in that the preparation method is as follows: 2 tons of dry powder of orange peel with a moisture content of 7% is added in the dilute hydrochloric acid solution of 20000L pH3.5, Water bath at 25°C for 2.0 hours, filter, collect filter residue, and dry at 40°C; take 1 ton of dry filter residue, mix with 10 kg of pectinase, add 10,000L of dilute hydrochloric acid solution with pH 4.0, stir well, and heat enzymatic hydrolysis in a 50°C water bath After 80 minutes, collect the filter residue and dry it; take 0.5 tons of the dry filter residue after enzymolysis, add 6000L petroleum ether at 25°C, fully extract for 7 hours, repeat the extraction for 3 times, collect the extract, and concentrate under reduced pressure. 3. the preparation method of a kind of oil-soluble citrus yellow pigment according to claim 1 is characterized in that the preparation method is as follows: 20 grams of dry powder of orange peel with a water content of 7% is added in the dilute hydrochloric acid solution of 250mlpH4.0, 25 ℃ water bath for 1.5 hours, filter, collect filter residue, and dry at 40°C; take 10 g of dry filter residue, mix with 0.15 g of pectinase, add 150 ml of dilute hydrochloric acid solution with pH 4.5, stir well, heat enzymolysis in 55°C water bath for 70 minutes, Collect the filter residue and dry; take 5 grams of the dried filter residue after enzymolysis, add 55ml of ether at room temperature, fully extract for 5 hours, repeat the extraction for 3 times, collect the extract, and concentrate under reduced pressure.