CN104130591B - A kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice - Google Patents
A kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice Download PDFInfo
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Abstract
The invention discloses a kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice, the method comprises the steps: that (1) is by Herba Gynurae bicoloris concentrated juice, it is diluted to 4 �� of Bx��6 �� Bx of Brix Scale with the citric acid water of PH3��PH5, obtains Herba Gynurae bicoloris concentrated juice diluent; (2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, and carry out eluting separation purification, obtain beet red eluent; (3) beet red eluent being concentrated into 20 �� of Bx��30 �� Bx of Brix Scale on water-bath haplo-effect concentrator, spray drying obtains beet red powder. While the method for present invention sugar in removing red beet juice, also eliminate other impurity such as inorganic salt therein, improve production efficiency; And adopt water-bath haplo-effect concentrator cryogenic vacuum to concentrate, decrease the degraded of raw material, it is possible to obtain the beet red product of relatively High color values.
Description
Technical field
The invention belongs to the method for extraction and purification of beet red pigment, particularly to a kind of method of extraction purification beet red from Herba Gynurae bicoloris concentrated juice.
Background technology
Beet red (Beetred) is a kind of nitrogenous pigment of water solublity, gain the name because being found in beet root the earliest, it it is pyridine derivate, basic chromophore is 1,7-bis-azo methine in heptan, it is the general name of all of colored compound in Herba Gynurae bicoloris, including Betacyanins (betacyanin) and 2 kinds of forms of betaxanthin (betaxanthin). Beet red pigment is widely present in the various plants such as Chenopodiaceae, Amaranthaceae, Cactaceae, Phytolaccaceae, also accumulates betanidin in part higher fungus. Betanidin is generally present in the flower of plant, fruit and part asexual propagation organ. Beet red be mainly composed of betanin (Betanine), account for the 75%��95% of red pigment, all the other still have different betanin, front betanin and different front betanin; Betaxanthin includes betaxanthin I and betaxanthin II.
Beet red solid is aubergine powder, soluble in water, is slightly soluble in ethanol, and insoluble in dehydrated alcohol, aqueous solution is red in reddish violet, bright in colour, has maximum absorption band near wavelength 535nm. During Ph3.0��7.0 more stable, PH3.0��5.0 stability is best; In the basic conditions then in yellow; Dieing activity is good, poor heat resistance. Its degradation speed with temperature rise and increase sharply, during 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 typically small, but during such as Fe3+, Cu2+ content height, brown stain can occur. Because beet red is very sensitive to heat, oxygen and light so that it is be restricted in application, generally it is usually used in the food such as ice cream, solidifying state Yogurt, dry-mix food and confection. The 31st meeting of JECFA in 1987 determines that it allows daily intake (ADI) without regulation.
Herba Gynurae bicoloris, also known as filiale, beet root, red vegetables, a kind of wild plant being named as sea beet root being grown in Mediterranean develop, originate in western European and Southern Coast, it is transplanted to Spain from Sweden, is a main sugar source beyond the Caulis Sacchari sinensis of the torrid zone. Herba Gynurae bicoloris root prominence such as fire, be otherwise known as flame dish. Herba Gynurae bicoloris root has long history as food, and mineral compound contained by it and plant compound are that beet root is distinctive, these compound energy infection, increases cell oxygen content, treats hematopathy, hepatopathy and immune system dysfunction. Herba Gynurae bicoloris concentrated juice had both extracted from the root of Herba Gynurae bicoloris. Generally the Herba Gynurae bicoloris root of every 100 grams contains the pigment of up to 200 milligrams, is good pigment source. The beet root of West Europe about output more than 200,000 tons every year, wherein nearly 10 is for processing as pigment purposes.
Haplo-effect concentrator is a kind of vacuum concentrator, the mode that external heat Natural Circulation combines with negative pressure of vacuum evaporation is adopted to reach the purpose of concentrated liquid, add thermal medium and be generally steam, yet with beet red to thermo-responsive, poor heat resistance, therefore it is transform as circulating hot water by adding thermal medium by the steam of high temperature, i.e. water-bath haplo-effect concentrator.
At present, beet red extraction purification has had multiple patent, and Chinese patent CN102093747B, CN102675910A, CN101429347A purification beet red uses macroporous resin, and they use single resin, in beet red, Impurity removal is not thorough so that color valency is on the low side.
Summary of the invention
It is an object of the invention to overcome deficiency of the prior art, it is provided that a kind of method of extraction purification beet red pigment from Radix Betae concentrated juice.
Technical scheme is summarized as follows:
A kind of method of extraction purification beet red pigment from Radix Betae concentrated juice, comprises the steps:
(1) by Herba Gynurae bicoloris concentrated juice, it is diluted to 4 �� of Bx��6 �� Bx of Brix Scale with the citric acid water of PH3.0��PH5.0, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent; Described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin;
(3) by beet red eluent bath temperature 60 DEG C��80 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa concentrates, is reduced to 20 �� of Bx��30 �� Bx of Brix Scale, obtains beet red concentrated solution, be spray dried to beet red powder.
Described Herba Gynurae bicoloris concentrated juice is color valency 3��10, the Herba Gynurae bicoloris concentrated juice of 50 �� of Bx��75 �� Bx of Brix Scale.
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 cation exchange resin, and model is: 001 �� 7; 7320; CD-180 or D151.
Described macroporous resin, model is: D101; O3K7; DM21; XDA200B; SP207 or SP825L.
The invention have the advantage that
1, hybrid resin purification beet red is used so that impurity is disposable is removed for substantial amounts of sugar, inorganic salt, heavy metal etc., improves production efficiency, reduces the impurity content in finished product so that gained beet red finished product color valency is higher;
2, use the concentration of water-bath haplo-effect concentrator cryogenic vacuum, decrease the beet red degraded loss when concentration, reduce production cost.
Detailed description of the invention
Below by specific embodiment, a kind of method of extraction purification beet red pigment from Radix Betae concentrated juice of the present invention being described, as explained below is merely to make those skilled in the art be more fully understood that the present invention, but does not limit the present invention in any way.
Using hybrid resin as separating medium in the present invention, while improving Radix Betae redness valency, eliminate the inorganic and organic impuritiess such as sugar, inorganic salt, heavy metal, wherein hybrid resin is selected from the mixing of ion exchange resin, two kinds of resins of macroporous resin.
Embodiment 1
A kind of method of extraction purification beet red pigment from Radix Betae concentrated juice, comprises the steps:
(1) by Herba Gynurae bicoloris concentrated juice, Herba Gynurae bicoloris concentrated juice is color valency 3, the Herba Gynurae bicoloris concentrated juice of 50 �� of Bx of Brix Scale, is diluted to 4 �� of Bx of Brix Scale with the citric acid water of PH3.0, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, hybrid resin is made up of mass ratio to be 5:95 be cation exchange resin 001 �� 7 and macroporous resin DM21, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent;
(3) beet red eluent is concentrated on bath temperature 60 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa, be reduced to 20 �� of Bx of Brix Scale, obtain beet red concentrated solution, be spray dried to beet red powder. Color valency is 215.
Embodiment 2
A kind of method of extraction purification beet red pigment from Radix Betae concentrated juice, comprises the steps:
(1) by Herba Gynurae bicoloris concentrated juice, Herba Gynurae bicoloris concentrated juice is color valency 5, the Herba Gynurae bicoloris concentrated juice of 65 �� of Bx of Brix Scale, is diluted to 5 �� of Bx of Brix Scale with the citric acid water of PH4.0, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, hybrid resin is made up of mass ratio to be 50:50 be cation exchange resin 7320 and macroporous resin O3K7, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent;
(3) beet red eluent is concentrated on bath temperature 70 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa, be reduced to 25 �� of Bx of Brix Scale, obtain beet red concentrated solution, be spray dried to beet red powder. Color valency is 220.
Embodiment 3
A kind of method of extraction purification beet red pigment from Radix Betae concentrated juice, comprises the steps:
(1) by Herba Gynurae bicoloris concentrated juice, Herba Gynurae bicoloris concentrated juice is color valency 10, the Herba Gynurae bicoloris concentrated juice of 75 �� of Bx of Brix Scale, is diluted to 6 �� of Bx of Brix Scale with the citric acid water of PH5.0, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, hybrid resin is 95:5 by mass ratio is that cation exchange resin CD-180 and macroporous resin SP207 forms, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent;
(3) beet red eluent is concentrated on bath temperature 80 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa, be reduced to 30 �� of Bx of Brix Scale, obtain beet red concentrated solution, be spray dried to beet red powder. Color valency is 231.
Embodiment 4
A kind of method of extraction purification beet red pigment from Radix Betae concentrated juice, comprises the steps:
(1) by Herba Gynurae bicoloris concentrated juice, Herba Gynurae bicoloris concentrated juice is color valency 6.5, the Herba Gynurae bicoloris concentrated juice of 62 �� of Bx of Brix Scale, is diluted to 5.5 �� of Bx of Brix Scale with the citric acid water of PH3.5, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, hybrid resin is 25:75 by mass ratio is that cation exchange resin D151 and macroporous resin XDA200B forms, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent;
(3) beet red eluent is concentrated on bath temperature 65 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa, be reduced to 23 �� of Bx of Brix Scale, obtain beet red concentrated solution, be spray dried to beet red powder. Color valency is 219.
Claims (5)
1. a method for extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice, is characterized in that comprising the steps:
(1) by Herba Gynurae bicoloris concentrated juice, it is diluted to 4 �� of Bx��6 �� Bx of Brix Scale with the citric acid water of pH3.0��pH5.0, obtains Herba Gynurae bicoloris concentrated juice diluent;
(2) by hybrid resin post on described Herba Gynurae bicoloris concentrated juice diluent, respectively with the concentration expressed in percentage by volume of 1 times of column volume deionized water, 1 times of column volume be 30% ethanol water, 1.5 times of column volumes concentration expressed in percentage by volume be that 70% ethanol water carries out eluting, collect 70% ethanol elution, both obtain beet red eluent; Described hybrid resin is the mixing of ion exchange resin, two kinds of resins of macroporous resin;
(3) by beet red eluent bath temperature 60 DEG C��80 DEG C, the water-bath haplo-effect concentrator of vacuum��-0.085MPa concentrates, is reduced to 20 �� of Bx��30 �� Bx of Brix Scale, obtains beet red concentrated solution, be spray dried to beet red powder.
2. a kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice according to claim 1, it is characterised in that described Herba Gynurae bicoloris concentrated juice is color valency 3��10, the Herba Gynurae bicoloris concentrated juice of 50 �� of Bx��75 �� Bx of Brix Scale.
3. a kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice according to claim 1, it is characterised 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.
4. a kind of method of extraction purification beet red pigment from Herba Gynurae bicoloris concentrated juice according to claim 1 or 3, it is characterised in that described ion exchange resin is cation exchange resin, and model is: 001 �� 7;7320; CD-180 or D151.
5. a kind of method of extraction purification beet red pigment from Radix Betae concentrated juice according to claim 1 or 3, it is characterised in that described macroporous resin model is: D101; O3K7; DM21; XDA200B; SP207 or SP825L.
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| 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 |
| CN112142695B (en) * | 2020-09-10 | 2023-05-30 | 万华化学集团股份有限公司 | Red-heart dragon fruit 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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| 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 |
| CN101429347A (en) * | 2008-12-12 | 2009-05-13 | 东北林业大学 | Process for producing beet red pigment |
| CN101735648A (en) * | 2010-01-25 | 2010-06-16 | 青岛鹏远天然色素研究所 | Method for separating and purifying beet red pigment by two aqueous phase extraction system |
| CN102093747A (en) * | 2010-12-22 | 2011-06-15 | 晨光生物科技集团股份有限公司 | Process for producing high color value betalain by utilizing macroporous resin |
| CN102660140A (en) * | 2012-05-18 | 2012-09-12 | 江西国亿生物科技有限公司 | Preparation method of multi-tone beet red pigment |
| CN102675910A (en) * | 2012-03-26 | 2012-09-19 | 安徽尚善生物科技有限公司 | Preparation method of high-color-value beet root red color |
| CN102993769A (en) * | 2012-12-24 | 2013-03-27 | 晨光生物科技集团股份有限公司 | Method for improving color tone of beet red pigment |
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- 2014-08-19 CN CN201410406932.6A patent/CN104130591B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101429347A (en) * | 2008-12-12 | 2009-05-13 | 东北林业大学 | Process for producing beet red pigment |
| CN101735648A (en) * | 2010-01-25 | 2010-06-16 | 青岛鹏远天然色素研究所 | Method for separating and purifying beet red pigment by two aqueous phase extraction system |
| CN102093747A (en) * | 2010-12-22 | 2011-06-15 | 晨光生物科技集团股份有限公司 | Process for producing high color value betalain by utilizing macroporous resin |
| CN102675910A (en) * | 2012-03-26 | 2012-09-19 | 安徽尚善生物科技有限公司 | Preparation method of high-color-value beet root red color |
| CN102660140A (en) * | 2012-05-18 | 2012-09-12 | 江西国亿生物科技有限公司 | Preparation method of multi-tone beet red pigment |
| CN102993769A (en) * | 2012-12-24 | 2013-03-27 | 晨光生物科技集团股份有限公司 | Method for improving color tone of beet red pigment |
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