CN104130591A - Method for extracting and purifying beet red pigment from garden beet concentrated juice - Google Patents
Method for extracting and purifying beet red pigment from garden beet concentrated juice Download PDFInfo
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- CN104130591A CN104130591A CN201410406932.6A CN201410406932A CN104130591A CN 104130591 A CN104130591 A CN 104130591A CN 201410406932 A CN201410406932 A CN 201410406932A CN 104130591 A CN104130591 A CN 104130591A
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Abstract
The invention discloses a method for extracting and purifying a beet red pigment from garden beet concentrated juice. The method comprises the following steps: (1) diluting the garden beet concentrated juice by using citric acid water of pH3-pH5 until the brix is 4-6 degrees, so that diluent of the garden beet concentrated juice is obtained; (2) putting the diluent of the garden beet concentrated juice on a mixed resin column, and carrying out elution, separation and purification on the diluent, so that beet red eluent is obtained; and (3) concentrating the beet red eluent on a water bath single-effect concentrator until the brix is 20-30 degrees, and carrying out spray drying on the obtained product, so that beet red powder is obtained. According to the method disclosed by the invention, sugar in garden beet concentrated juice is removed, and other impurities such as inorganic salts and the like are also removed, thereby improving the production efficiency; and the water bath single-effect concentrator is adopted for carrying out low-temperature vacuum concentration, so that the degradation of raw materials is reduced, and beet red products with a relatively high color value can be obtained.
Description
Technical field
The invention belongs to the extracting and purifying method of beet red pigment, particularly a kind of method of extracting purifying beet red from red beet inspissated juice.
Background technology
Beet red (Beet red) is a kind of water-soluble nitrogenous pigment, because being found in beet tails and gaining the name the earliest, it is pyridine derivate, basic chromophoric group is 1,7-bis-azo methines in heptan, be the general name of colored compound all in red beet, comprise Betacyanins (betacyanin) and 2 kinds of forms of betaxanthin (betaxanthin).Beet red pigment is extensively present in the various plants such as Chenopodiaceae, Amaranthaceae, Cactaceae, Phytolaccaceae, also accumulates betanidin in part higher fungi.Betanidin is generally present in flower, fruit and the part vegetative propagation organ of plant.The main component of beet red is betanin (Betanine), accounts for 75%～95% of haematochrome, and all the other still have different betanin, front betanin and different front betanin; Betaxanthin comprises betaxanthin I and betaxanthin II.
Beet red solid is red-purple powder, soluble in water, is slightly soluble in ethanol, is insoluble to dehydrated alcohol, and it is red in red-violet colour that the aqueous solution is, and lovely luster has maximum absorption band near wavelength 535nm.Ph3.0～7.0 are o'clock more stable, and PH3.0～5.0 stability is best; In the next yellow that is of alkaline condition; Dying property is good, poor heat resistance.Its degradation speed increases sharply with temperature rise, and when PH5.0, the half life of pigment is 1150 ± 100min(25 DEG C), 310 ± 30min(50 DEG C), 90 ± 100min(75 DEG C) and 14.5 ± 2min(100 DEG C).Light and oxygen also can promote degraded.The impact of metal ion is generally less, but as Fe3+, when Cu2+ content is high, brown stain can occur.Very sensitive to heat, oxygen and light because of beet red, it is restricted in application, be generally usually used in ice cream, solidifying state Yogurt, be dry mixed in the food such as food and candy.The 31st meeting of JECFA in 1987 determines that it allows daily intake (ADI) without regulation.
Red beet, claim again filiale, beet tails, red vegetables, developed by a kind of wild plant that is named as sea beet root that is grown in Mediterranean, originate in European western part and Southern Coast, being transplanted to Spain from Sweden, is a main sugar source beyond tropical sugarcane.Red beet root prominence is as fire, and flame dish is otherwise known as.Red beet root has long history as food, and its contained mineral compound and plant compound are that beet tails is distinctive, and these compounds can be anti-infective, increases cell oxygen level, treatment hemopathy, hepatopathy and immune system dysfunction.Red beet inspissated juice had both extracted the root from red beet.The red beet root of general every 100 grams contains the pigment up to 200 milligrams, is good pigment source.200,000 tons of above beet tails of the annual approximately output in West Europe, wherein nearly 10 ﹪ systems are used for processing as pigment purposes.
Haplo-effect concentrator is a kind of vacuum concentrator, adopt external heat natural circulation and negative pressure of vacuum to evaporate the mode combining to reach the object of concentrated liquid, heating medium is generally steam, but because beet red is to thermo-responsive, poor heat resistance, therefore transform heating medium as circulating hot water by the steam of high temperature, i.e. water-bath haplo-effect concentrator.
At present, beet red extracts purifying multiple patents, and what Chinese patent CN 102093747B, CN 102675910A, CN 101429347A purifying beet red used is macroporous resin, and they use single resin, in beet red, Impurity removal is not thorough, makes Dry Sack valency on the low side.
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Summary of the invention
The object of the invention is to overcome deficiency of the prior art, a kind of method of extracting purifying beet red pigment from beet inspissated juice is provided.
Technical scheme of the present invention is summarized as follows:
A method of extracting purifying beet red pigment from beet inspissated juice, comprises the steps:
(1) by red beet inspissated juice, be diluted to 4 ° of Bx～6 ° Bx of Brix with the citric acid water of PH3.0～PH5.0, obtain red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant; Described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin;
(3) by beet red elutriant 60 DEG C～80 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 20 ° of Bx～30 ° Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.
Described red beet inspissated juice is look valency 3～10, the red beet inspissated juice of 50 ° of Bx～75 ° Bx of Brix.
Described citric acid water is the citric acid water of PH3.0～PH5.0.
The bath temperature of described water-bath haplo-effect concentrator is 60 DEG C～80 DEG C.
Described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin, and mixing quality ratio is 5～95:5～95.
Described ion exchange resin is Zeo-karb, and model is: 001 × 7; 7320; CD-180 or D151.
Described macroporous resin, model is: D101; O3K7; DM21; XDA200B; SP207 or SP825L.
Advantage of the present invention is:
1, use hybrid resin purifying beet red, make a large amount of sugars, inorganic salt, heavy metal etc. impurity is disposable to be removed, improved production efficiency, reduced the foreign matter content in finished product, make gained beet red finished product look valency higher;
2, use water-bath haplo-effect concentrator cryogenic vacuum concentrated, reduced the degraded loss of beet red when concentrated, reduced production cost.
Embodiment
Below by a kind of method of extracting purifying beet red pigment from beet inspissated juice of specific embodiment explanation the present invention, description is below only in order to make those skilled in the art understand better the present invention, but does not limit the present invention in any way.
Use in the present invention hybrid resin as separating medium, in improving the red valency of beet, removed sugar, inorganic salt, the inorganic and organic impurity such as heavy metal, wherein hybrid resin is selected from the mixing of ion exchange resin, two kinds of resins of macroporous resin.
Embodiment 1
A method of extracting purifying beet red pigment from beet inspissated juice, comprises the steps:
(1) by red beet inspissated juice, red beet inspissated juice is look valency 3, and the red beet inspissated juice of 50 ° of Bx of Brix is diluted to 4 ° of Bx of Brix with the citric acid water of PH3.0, obtains red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, hybrid resin is that 5:95 is that Zeo-karb 001 × 7 and macroporous resin DM21 form by mass ratio, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant;
(3) by beet red elutriant 60 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 20 ° of Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.Look valency is 215.
Embodiment 2
A method of extracting purifying beet red pigment from beet inspissated juice, comprises the steps:
(1) by red beet inspissated juice, red beet inspissated juice is look valency 5, and the red beet inspissated juice of 65 ° of Bx of Brix is diluted to 5 ° of Bx of Brix with the citric acid water of PH4.0, obtains red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, hybrid resin is that 50:50 is that Zeo-karb 7320 and macroporous resin O3K7 form by mass ratio, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant;
(3) by beet red elutriant 70 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 25 ° of Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.Look valency is 220.
Embodiment 3
A method of extracting purifying beet red pigment from beet inspissated juice, comprises the steps:
(1) by red beet inspissated juice, red beet inspissated juice is look valency 10, and the red beet inspissated juice of 75 ° of Bx of Brix is diluted to 6 ° of Bx of Brix with the citric acid water of PH5.0, obtains red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, hybrid resin is that 95:5 is that Zeo-karb CD-180 and macroporous resin SP207 form by mass ratio, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant;
(3) by beet red elutriant 80 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 30 ° of Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.Look valency is 231.
Embodiment 4
A method of extracting purifying beet red pigment from beet inspissated juice, comprises the steps:
(1) by red beet inspissated juice, red beet inspissated juice is look valency 6.5, and the red beet inspissated juice of 62 ° of Bx of Brix is diluted to 5.5 ° of Bx of Brix with the citric acid water of PH3.5, obtains red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, hybrid resin is that 25:75 is that Zeo-karb D151 and macroporous resin XDA200B form by mass ratio, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant;
(3) by beet red elutriant 65 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 23 ° of Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.Look valency is 219.
Claims (7)
1. a method of extracting purifying beet red pigment from red beet inspissated juice, is characterized in that comprising the steps:
(1) by red beet inspissated juice, be diluted to 4 ° of Bx～6 ° Bx of Brix with the citric acid water of PH3.0～PH5.0, obtain red beet inspissated juice diluent;
(2) by hybrid resin post on described red beet inspissated juice diluent, be that 70% aqueous ethanolic solution carries out wash-out by the concentration expressed in percentage by volume that the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume is 30% aqueous ethanolic solution, 1.5 times of column volumes respectively, collect 70% ethanol eluate, both obtained beet red elutriant; Described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin;
(3) by beet red elutriant 60 DEG C～80 DEG C of bath temperatures, concentrated on the water-bath haplo-effect concentrator of vacuum tightness≤-0.085MPa, be reduced to 20 ° of Bx～30 ° Bx of Brix, obtain beet red concentrated solution, be spray dried to beet red powder.
2. a kind of method of extracting purifying beet red pigment from red beet inspissated juice according to claim 1, is characterized in that described red beet inspissated juice is look valency 3～10, the red beet inspissated juice of 50 ° of Bx～75 ° Bx of Brix.
3. a kind of method of extracting purifying beet red pigment from red beet inspissated juice according to claim 1, the citric acid water that the water that it is characterized in that described dilution red beet inspissated juice is PH3.0～PH5.0.
4. a kind of method of extracting purifying beet red pigment from red beet inspissated juice according to claim 1, the bath temperature that it is characterized in that described water-bath haplo-effect concentrator is 60 DEG C～80 DEG C.
5. a kind of method of extracting purifying beet red pigment from red beet inspissated juice according to claim 1, is characterized in that described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin, and mixing quality ratio is 5～95:5～95.
6. according to a kind of method of extracting purifying beet red pigment from red beet inspissated juice described in claim 1 or 5, it is characterized in that described ion exchange resin is Zeo-karb, model is: 001 × 7; 7320; CD-180 or D151.
7. according to a kind of method of extracting purifying beet red pigment from beet inspissated juice described in claim 1 or 5, it is characterized in that described macroporous resin model is: D101; O3K7; DM21; XDA200B; SP207 or SP825L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112011192A (en) * | 2020-09-09 | 2020-12-01 | 江西丹霞生物科技股份有限公司 | Preparation process of deodorized beet red and product thereof |
| CN112142695A (en) * | 2020-09-10 | 2020-12-29 | 万华化学集团股份有限公司 | Red-heart pitaya pulp extract and extraction method thereof |
| CN112656018A (en) * | 2019-10-16 | 2021-04-16 | 姜志斌 | Safe concentration technical equipment for VLT vacuum low-temperature aqueous medium paste without gelatinization |
| CN112662198A (en) * | 2021-01-21 | 2021-04-16 | 云南通海杨氏天然产物有限公司 | Method for efficiently preparing high-quality beet red pigment |
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| JPS5811555A (en) * | 1981-07-14 | 1983-01-22 | San Ei Chem Ind Ltd | Betacyanin pigment preparation |
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| CN101429347A (en) * | 2008-12-12 | 2009-05-13 | 东北林业大学 | Process for producing beet red pigment |
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Patent Citations (8)
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| JPS5811555A (en) * | 1981-07-14 | 1983-01-22 | San Ei Chem Ind Ltd | Betacyanin pigment preparation |
| CN1191877A (en) * | 1997-02-27 | 1998-09-02 | 吉林省农业科学院原子能利用研究所 | Preparation of betanin pigment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112656018A (en) * | 2019-10-16 | 2021-04-16 | 姜志斌 | Safe concentration technical equipment for VLT vacuum low-temperature aqueous medium paste without gelatinization |
| CN112011192A (en) * | 2020-09-09 | 2020-12-01 | 江西丹霞生物科技股份有限公司 | Preparation process of deodorized beet red and product thereof |
| CN112142695A (en) * | 2020-09-10 | 2020-12-29 | 万华化学集团股份有限公司 | Red-heart pitaya pulp extract and extraction method thereof |
| CN112662198A (en) * | 2021-01-21 | 2021-04-16 | 云南通海杨氏天然产物有限公司 | Method for efficiently preparing high-quality beet red pigment |
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