CN106590020A - Method of separating water soluble monascus pigment by the use of macroreticular resin and application thereof - Google Patents
Method of separating water soluble monascus pigment by the use of macroreticular resin and application thereof Download PDFInfo
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- CN106590020A CN106590020A CN201610943653.2A CN201610943653A CN106590020A CN 106590020 A CN106590020 A CN 106590020A CN 201610943653 A CN201610943653 A CN 201610943653A CN 106590020 A CN106590020 A CN 106590020A
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- absorbent resin
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Abstract
The invention discloses a method of separating water soluble monascus pigment by the use of macroreticular resin and application thereof. The method comprises the steps of conducting solid-liquid separation on fermented monascus fungi fermentation primary liquid in a liquid fermentation medium, taking liquid to obtain extracellular water soluble monascus pigment fermentation solution, then adding the macroreticular resin after pretreatment to conduct absorbing, then using ethyl alcohol to conduct elution, removing eluent from obtained eluant and conducting frozen vacuum drying on the eluant, and finally obtaining the water soluble monascus pigment. According to the method of separating the water soluble monascus pigment by the use of the macroreticular resin and application thereof, the problems of unstable water soluble monascus pigment and massive impurities in the fermentation solution are solved by utilizing the macroreticular resin to conduct separation and purification on the monascus pigment; meanwhile efficient separation of the extracellular water soluble monascus pigment is achieved by removing impurities of polysaccharide, inorganic salt and the like in the monascus pigment fermentation solution, and a good application prospect and market value are provided.
Description
Technical field
The present invention relates to the separation method of monascorubin, more particularly to a kind of water-soluble red using macroporous absorbent resin separation
The method of bent pigment and its application.
Background technology
Monascorubin is a kind of natural colouring matter, by Monascus fermenting and producing, is proposed from the red yeast rice of Fermentation Condition of Monascus spp
Pigment is mainly para chrome, and these pigments are soluble in the larger organic solution of ethanol, acetone isopolarity, are all non-water-soluble
Pigment, is subject to certain restrictions in terms of food applications.With going deep into that monascorubin is studied, in recent years with liquid fermentation production
Monascorubin then have good water solubility.The heat endurance of water-soluble monascus pigment, light shine, antioxidant and resistance to reduction
The performance of agent is good, and its developmental research has broad prospects and great economic benefit.But at present to water-soluble in Monas cuspurpureus Went fermentation liquid
Property pigment isolate and purify research report it is relatively fewer, it is less efficient.Such as have been reported that spent ion exchange resin (D380,
D301R, 110H etc.) monascorubin is separated, there are problems that being difficult to wash-out or eluting rate not (Lian Xi armies etc., food industry section
Skill, 2003,24 (8):81-83)；Have been reported that and separate water-soluble monascus pigment with anion exchange resin D301, obtain purity very
High monascorubin, there is a problem of all reclaiming pigment (bear He Jian etc., Southwestern University's journal natural science edition,
2009,31(9):20-24)；Have been reported that with macroporous absorbent resin (X-5, AB-8, D14、D16Deng) monascorubin is separated, exist back
The problems such as yield is low (Tong Qunyi, Sichuan Light Chemical Engineering College's journal, 1999,12 (4):9-12)；Have been reported that and use macroreticular resin NKA
Deng processing monascorubin waste liquid, there is a problem of adsorption rate and eluting rate it is all low (hold gorgeous skin of bamboo etc., Food Additives Used in China,
2012,01:154-157)。
Generally increase the generation that soluble protein, peptide, amino acid promote water-soluble monascus pigment in the medium,
Hassan Hajjaj etc. (International Journal of Food Science and Technology, 2015,50:
1731-1736) extracellular monascorubin is increased by the carbon nitrogen source ratio and fermentation condition in optimization red koji fermentation culture medium,
But cause fermentation broth contents to become more complicated, red, orange, yellow three classes pigment and protein, polypeptide, amino acid, Glucosamine
The various derivatives of generation are combined Deng material.In addition, Chen gong etc. (BMC Biotechnology, 2015,15 (1):72-80)
High density fermentation is carried out so that the substantial increase of monascus liquid fermentation extracellular uranidin by single carbon source (glucose) of adding, but
In the Monas cuspurpureus Went fermentation liquid for finally giving residual sugar be higher than 25g/L, increase later stage water-soluble monascus pigment product separate and purify
Difficulty, therefore, need a kind of method for efficiently separating water-soluble monascus pigment badly.
The content of the invention
The primary and foremost purpose of the present invention is the shortcoming and deficiency for overcoming prior art, there is provided one kind utilizes macroporous absorbent resin
The method for separating water-soluble monascus pigment.
Another object of the present invention is to providing the utilization macroporous absorbent resin separates water-soluble monascus pigment method
Using.
The purpose of the present invention is achieved through the following technical solutions：One kind separates water-soluble monascus color using macroporous absorbent resin
The method of element, comprises the steps：
(1) pretreatment of zymotic fluid：The good monascus ruber fermenation raw liquid of liquid state fermentation is carried out into separation of solid and liquid, liquid is taken,
Obtain extracellular water-soluble monascus pigment zymotic fluid；
(2) pretreatment of resin：Macroporous absorbent resin is pre-processed, wet resin is obtained；
(3) adsorb：The wet resin obtained in step (2) is added in step (1) the extracellular water-soluble monascus color for obtaining
Adsorbed in plain zymotic fluid, separation of solid and liquid takes solid, obtains filter cake；
(4) desorb：The filter cake obtained in step (3) is eluted with ethanol, separation of solid and liquid, collected liquid, washed
De- liquid；
(5) eluant, eluent is removed：The eluent obtained in step (4) is removed into eluant, eluent, concentrate is obtained；
(6) it is vacuum dried：The concentrate obtained in step (5) is carried out into vacuum freezedrying, water-soluble monascus color is obtained
Element.
The culture medium of the liquid state fermentation described in step (1) is preferably：In per 100mL liquid state fermentation culture mediums, containing grape
Sugar 10～30g, (NH4)2SO4 0.5g、KH2PO4 0.5g、MgSO4·7H2O 0.05g、FeSO4·7H2O 1.0mg、ZnSO4·
7H2O 1.0mg、MnSO4·H2O 3.0mg, with water 100ml, pH natures are settled to.
Described water is distilled water or deionized water.
Monascus ruber described in step (1) is preferably the monascus ruber that deposit number is CGMCC No.10910
(Monascus ruber)。
The colour value of the extracellular water-soluble monascus pigment zymotic fluid described in step (1) is 40～250AU350/ mL, preferably
99.13～135.88AU350/mL。
The method of the separation of solid and liquid described in step (1), (3) and (4) is preferably suction filtration.
Macroporous absorbent resin described in step (2) is preferably macroporous absorbent resin DA201, more preferably macroporous absorption tree
Fat DA201-B or DA201-C.
The method for being pre-processed macroporous absorbent resin described in step (2) is preferably achieved by the steps of：
A () soaks macroporous absorbent resin with ethanol, then with alcohol flushing, be washed till the ethanol of outflow without muddiness, Ran Houyong
It is washed to without alcohol taste；
B () is then soaked with HCl solution, wash with water to neutrality, then is soaked with NaOH solution, is washed with water to neutrality, is obtained
Macroporous absorbent resin (wet resin) after process；
C () terminates to this；Or repeat step (b) 2～3 times.
The concentration of the ethanol described in step (a) is preferably percent by volume 95%.
The time soaked with ethanol described in step (a) is 8～24h, preferably 12h.
Water described in step (a) and step (b) is preferably distilled water or deionized water.
The concentration of the HCl solution described in step (b) is preferably percent by volume 2～8%, and preferably 4%.
The time soaked with HCl solution described in step (b) is preferably 2～8h, preferably 4h.
The concentration of the NaOH solution described in step (b) is preferably percent by volume 2～8%, and preferably 4%.
The time soaked with NaOH solution described in step (b) is preferably 2～8h, preferably 4h.
The macroporous absorbent resin after the process for obtaining described in step (b) is preserved in a wet process.
Macroporous absorbent resin addition described in step (3) is by the extracellular water-soluble monascus pigment zymotic fluid proportionings of every mL
0.2～0.5g macroporous absorbent resins are calculated, preferably by the extracellular water-soluble monascus pigment zymotic fluid 0.43～0.5g of proportioning of every mL
Macroporous absorbent resin is calculated.
Absorption described in step (3) is included carrying out Static Adsorption by standing mode and is inhaled by way of vibration
It is attached.
The time of described absorption is 0.15～2.5h, preferably 0.25～0.5h.
Wash-out described in step (4) is static wash-out or dynamic gradient wash-out.
The method of described static wash-out is preferably achieved by the steps of：The filter cake for obtaining is fitted in container, is added
Ethanol, standing is eluted.
Described container is preferably glass container, more preferably beaker.
The concentration of described ethanol is preferably percent by volume 95%.
The method of described dynamic gradient wash-out is preferably achieved by the steps of：The filter cake for obtaining is loaded into normal pressure chromatography
Post, with the ethanol of the variable concentrations of 2 times of column volumes gradient elution is carried out.
The concentration of described ethanol is percent by volume 25%, 50%, 75% and 100%.
The speed of described gradient elution is preferably 1～10BV/h；Preferably 5BV/h.
The time of described wash-out is 0.15～2.5h, preferably 0.25～0.5h.
The method of the removal eluant, eluent described in step (5) is preferably removed by reduction vaporization mode, while recyclable wash
De- agent, resource is reused.
Described reduction vaporization is carried out under the conditions of 45 DEG C of water-baths, vacuum≤- 0.085Mpa.
Described utilization macroporous absorbent resin separates the method for water-soluble monascus pigment in water-soluble monascus pigment is separated
Application.
The present invention has the following advantages and effect relative to prior art：
1st, the method that the present invention separates water-soluble monascus pigment using macroporous absorbent resin, can obtain under Dynamic Adsorption wash-out
It is real to high-recovery (more than 95%) and desalination (more than 95%), the extracellular water-soluble monascus pigment of desugar (more than 98%)
Isolating and purifying for water-soluble monascorubin is showed, while the macroreticular resin DA201 that the present invention is used is to water-soluble monascus color
Rapid 0.25h～the 0.5h of adsorption-desorption process of element substantially can reach adsorption-desorption balance, and this has wide to industrial production
Application prospect.
2nd, the present invention is according to inorganic salts, polysaccharide, protein etc. between water-soluble monascus pigment and in Monas cuspurpureus Went fermentation liquid
The difference of each component molecules size in impurity, purification ＆ isolation is carried out using macroporous absorbent resin by monascorubin, is solved water-soluble
Pigment is unstable and zymotic fluid in problem more than impurity；It is simultaneously miscellaneous by removing monascorubin polysaccharide of fermentation broth, inorganic salts etc.
Matter, realizes that extracellular monascorubin is efficiently separated, with good application prospect and market value.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1 separates water-soluble monascus pigment using macroporous absorbent resin DA201-C
(1) pretreatment of zymotic fluid：By the monascus ruber Monascusruber fermented in liquid state fermentation culture medium
(CGMCC No.10910) zymotic fluid carries out suction filtration, takes filtrate, obtains extracellular water-soluble monascus pigment zymotic fluid, determines extracellular water
The colour value of soluble red rice red pigment is 99.13AU350/ mL (determines the extinction at characteristic wavelength 350nm with ultraviolet specrophotometer
Degree), salinity 2.15ms/cm (electrical conductivity), residual sugar content 30g/L (DNS methods), wherein, the composition of liquid state fermentation culture medium is as follows：
Glucose 7.5g, (NH4)2SO40.25g, KH2PO40.25g, MgSO4·7H2O 0.025g, KCl 0.025g, FeSO4·
7H2O 0.5mg, ZnSO4·7H2O 0.5mg, MnSO4·H2O 1.5mg, with distilled water 50mL, pH natures are settled to.
(2) pretreatment of resin：The DA201-C macroreticular resins (Zhengzhou Qin Shi Science and Technology Ltd.s) of purchase are used into 95%
(v/v) alcohol solution dipping 12h, first with 95% (v/v) alcohol flushing, washes the ethanol for flowing out without muddiness, then uses distilled water
It is washed till without alcohol taste；Then 4h is soaked with 4% (v/v) HCl solution, with distillation neutrality is washed to, then with 4% (v/v) NaOH solution
Immersion 4h, with distillation neutrality is washed to, and is repeated 2 times, and wet method is saved backup.
(3) adsorb：Take treated in extracellular water-soluble monascus pigment addition step (2) that 5mL steps (1) are obtained
DA201-C wet resin 2.5g, stir, and standing adsorption 0.25h, suction filtration obtains filter cake, while the colour value for determining filtrate is
3.37AU350/mL。
(4) desorb：The filter cake that step (3) is obtained is placed in beaker, the static wash-out of 95% (v/v) ethanol solution is added
0.25h, suction filtration, collect eluent, determine its salinity for 0.25ms/cm (electrical conductivity), residual sugar amount 3.37g/L (DNS methods) and
Colour value is 76.24AU350/ mL (determines the absorbance at characteristic wavelength 350nm) with ultraviolet specrophotometer.
(5) eluant, eluent is reclaimed：The eluent that step (4) is obtained adopts reduction vaporization mode (45 DEG C of bath temperature, vacuum
Degree≤- 0.085MPa) reclaim eluant, eluent, the concentrate of the eluant, eluent that is removed.
(6) it is vacuum dried：The concentrate that step (5) is obtained is carried out into vacuum freezedrying (- 20 DEG C of cryogenic temperature, vacuum
≤ -0.037Mpa), obtain water-soluble monascus pigment product.
As a result：To the adsorption rate of water-soluble monascus pigment in zymotic fluid up to 96.60%, pigment is returned DA201-C macroreticular resins
Yield is 76.91%, and salt clearance is 88.37%, and sugared clearance is 88.77%.Show using macroporous absorbent resin DA201-C
The high-purity water soluble red rice red pigment of desalination, desugar can be obtained.
Embodiment 2 separates water-soluble monascus pigment using macroporous absorbent resin DA201-B
(1) pretreatment of zymotic fluid：With step (1) in embodiment 1.
(2) pretreatment of resin：It is identical with the step of embodiment 1 (2) in sheet, differ only in the present embodiment and adopt DA201-
B (Zhengzhou Qin Shi Science and Technology Ltd.s) macroreticular resin instead of DA201-C macroreticular resins in embodiment 1.
(3) adsorb：Take treated in extracellular water-soluble monascus pigment addition step (2) that 5mL steps (1) are obtained
DA201-B wet resin 2.5g, stir, and standing adsorption 30min, suction filtration obtains filter cake, while the colour value for determining filtrate is
0.88AU350/mL。
(4) desorb：The filter cake that step (3) is obtained is placed in beaker, the static wash-out of 95% (v/v) ethanol solution is added
0.5h, suction filtration collects eluent, determines its salinity for 0.35ms/cm (electrical conductivity), residual sugar amount 4.30g/L (DNS methods) and color
Valency is 75.21AU350/ mL (determines the absorbance at characteristic wavelength 350nm) with ultraviolet specrophotometer.
(5) eluant, eluent is reclaimed：With the step of embodiment 1 (5).
(6) it is vacuum dried：With the step of embodiment 1 (6).
As a result：DA201-B macroreticular resins can reach to the adsorption rate of water-soluble monascus pigment in zymotic fluid after 0.5h
99.11%, pigment recovery rate is 75.87%, and salt clearance is 83.72%, and sugared clearance is 85.67%.Show to utilize macropore
Polymeric adsorbent DA201-B can obtain the water-soluble monascus pigment of desalination desugar.
Embodiment 3 separates water-soluble monascus pigment using macroporous absorbent resin DA201-C
(1) pretreatment of zymotic fluid：By the monascus ruber Monascusruber fermented in liquid state fermentation culture medium
(CGMCC No.10910) zymotic fluid carries out suction filtration, takes supernatant, obtains extracellular water-soluble monascus pigment zymotic fluid, determines extracellular
The colour value of water-soluble monascus pigment is 135.88AU350/ mL (determines the extinction at characteristic wavelength 350nm with ultraviolet specrophotometer
Degree), salinity 2.37ms/cm (electrical conductivity), residual sugar content 137.01g/L (DNS methods), wherein, the composition of liquid state fermentation culture medium
It is as follows：Glucose 15g, (NH4)2SO40.25g, KH2PO40.25g, MgSO4·7H2O 0.025g, KCl 0.025g,
FeSO4·7H2O0.5mg, ZnSO4·7H2O 0.5mg, MnSO4·H2O 1.5mg, with distilled water 50mL, pH natures are settled to.
(2) pretreatment of resin：With the step of embodiment 1 (2).
(3) adsorb：Treated DA201-C wet resins in 25g steps (2) are taken, the born of the same parents for adding 58mL steps (1) to obtain
Outer water-soluble monascus pigment, with 180rpm speed oscillations 0.25h is adsorbed, and suction filtration is washed to the clarification of water of outflow, obtains filter cake,
Colour value (the 1.43AU of filtrate is determined simultaneously350/mL)。
(4) desorb：The filter cake that step (3) is obtained loads normal pressure chromatography glass column (Φ 15mm × 305mm), respectively with 2
Times column volume different concentration ethanol (25%, 50%, 75%, 100%, v/v), totally 8 times of column volume eluant, eluents (are used successively
25%th, 50%, 75%, 100% ethanol elution) gradient elution is carried out, gradient elution speed is 5BV/h.Eluent is collected, is surveyed
Fixed its salinity is 0.1ms/cm (electrical conductivity), residual sugar amount (DNS methods) 2.36g/L and colour value 129.55AU350/ mL is (with ultraviolet point
Absorbance at light photometric determination characteristic wavelength 350nm).
(5) eluant, eluent is reclaimed：With the step of embodiment 1 (5).
(6) it is vacuum dried：With the step of embodiment 1 (6).
As a result：To the adsorption rate of water-soluble monascus pigment in zymotic fluid up to 98.95%, pigment is returned DA201-C macroreticular resins
Yield is 95.34%, and salt clearance is 95.78%, and sugared clearance is 98.28%, is shown using macroporous absorbent resin DA201-C
The high-purity water soluble red rice red pigment product of desalination, desugar can be obtained.
Comparative example 1 separates water-soluble monascus pigment using macroporous absorbent resin D150
(1) pretreatment of zymotic fluid：With step (1) in embodiment 1.
(2) pretreatment of resin：It is identical with the step of embodiment 1 (2) in sheet, differ only in the present embodiment and adopt D150
(Zhengzhou Qin Shi Science and Technology Ltd.s) macroreticular resin instead of DA201-C macroreticular resins in embodiment 1.
(3) adsorb：Take treated in extracellular water-soluble monascus pigment addition step (2) that 5mL steps (1) are obtained
D150 wet resin 2.5g, stir, and standing adsorption 30min, suction filtration obtains filter cake, while the colour value for determining filtrate is
38.30AU350/mL。
(4) desorb：The filter cake that step (3) is obtained is placed in beaker, the static wash-out of 95% (v/v) ethanol solution is added
0.5h, suction filtration collects eluent, determines its salinity for 0.42ms/cm (electrical conductivity), residual sugar amount 9.31g/L (DNS methods) and color
Valency is 11.01AU350/ mL (determines the absorbance at characteristic wavelength 350nm) with ultraviolet specrophotometer.
(5) eluant, eluent is reclaimed：With the step of embodiment 1 (5).
(6) it is vacuum dried：With the step of embodiment 1 (6).
As a result：D150 macroreticular resins can reach to the adsorption rate of water-soluble monascus pigment in zymotic fluid after 0.5h
61.36%, pigment recovery rate is 11.11%, and salt clearance is 80.47%, and sugared clearance is 68.97%.Show to utilize macropore
Polymeric adsorbent D150 separates water-soluble monascus pigment, although can reach certain desalting effect, but obtain it is water-soluble red
Bent pigment recovery rate is extremely low.
Comparative example 2 separates water-soluble monascus pigment using macroporous absorbent resin LX-38
(1) pretreatment of zymotic fluid：With step (1) in embodiment 1.
(2) pretreatment of resin：It is identical with the step of embodiment 1 (2) in sheet, differ only in the present embodiment and adopt LX-38
(Zhengzhou Qin Shi Science and Technology Ltd.s) macroreticular resin instead of DA201-C macroreticular resins in embodiment 1.
(3) adsorb：Take treated in extracellular water-soluble monascus pigment addition step (2) that 5mL steps (1) are obtained
LX-38 wet resin 2.5g, stir, and standing adsorption 30min, suction filtration obtains filter cake, while the colour value for determining filtrate is
8.61AU350/mL。
(4) desorb：The filter cake that step (3) is obtained is placed in beaker, the static wash-out of 95% (v/v) ethanol solution is added
0.5h, suction filtration collects eluent, determines its salinity for 0.72ms/cm (electrical conductivity), residual sugar amount 6.64g/L (DNS methods) and color
Valency is 59.79AU350/ mL (determines the absorbance at characteristic wavelength 350nm) with ultraviolet specrophotometer.
(5) eluant, eluent is reclaimed：With the step of embodiment 1 (5).
(6) it is vacuum dried：With the step of embodiment 1 (6).
As a result：LX-38 macroreticular resins can reach to the adsorption rate of water-soluble monascus pigment in zymotic fluid after 0.5h
91.31%, pigment recovery rate is 60.31%, and salt clearance is 66.51%, and sugared clearance is 77.87%.Show to utilize macropore
Separation of the polymeric adsorbent LX-38 to water-soluble monascus pigment, can obtain the water-soluble monascus pigment of certain desugar, but reclaim
Rate and salt rejection rate be not high.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of method that utilization macroporous absorbent resin separates water-soluble monascus pigment, it is characterised in that comprise the steps：
(1) pretreatment of zymotic fluid：The good monascus ruber fermenation raw liquid of liquid state fermentation is carried out into separation of solid and liquid, liquid is taken, is obtained
Extracellular water-soluble monascus pigment zymotic fluid；
(2) pretreatment of resin：Macroporous absorbent resin is pre-processed, wet resin is obtained；
(3) adsorb：The wet resin obtained in step (2) is added to the extracellular water-soluble monascus pigment obtained in step (1) to send out
Adsorbed in zymotic fluid, separation of solid and liquid takes solid, obtains filter cake；
(4) desorb：The filter cake obtained in step (3) is eluted with ethanol, separation of solid and liquid, collected liquid, obtained eluent；
(5) eluant, eluent is removed：The eluent obtained in step (4) is removed into eluant, eluent, concentrate is obtained；
(6) it is vacuum dried：The concentrate obtained in step (5) is carried out into vacuum freezedrying, water-soluble monascus pigment is obtained.
2. the method that utilization macroporous absorbent resin according to claim 1 separates water-soluble monascus pigment, it is characterised in that：
Macroporous absorbent resin described in step (2) is macroporous absorbent resin DA201.
3. the method that utilization macroporous absorbent resin according to claim 1 separates water-soluble monascus pigment, it is characterised in that：
Absorption described in step (3) is included carrying out Static Adsorption by standing mode and is adsorbed by way of vibration；
Wash-out described in step (4) is static wash-out or dynamic gradient wash-out.
4. the method that utilization macroporous absorbent resin according to claim 3 separates water-soluble monascus pigment, it is characterised in that：
The method of described static wash-out is achieved by the steps of：The filter cake for obtaining is fitted in container, ethanol is added, is stood
Eluted；
The method of described dynamic gradient wash-out is achieved by the steps of：The filter cake for obtaining is loaded into normal pressure chromatographic column, with 2 times
The ethanol of the variable concentrations of column volume carries out gradient elution.
5. the method that utilization macroporous absorbent resin according to claim 3 separates water-soluble monascus pigment, it is characterised in that：
The time of described absorption is 0.15～2.5h；
The time of described wash-out is 0.15～2.5h.
6. the method that utilization macroporous absorbent resin according to claim 1 separates water-soluble monascus pigment, it is characterised in that：
The method for being pre-processed macroporous absorbent resin described in step (2) is achieved by the steps of：
A () soaks macroporous absorbent resin with ethanol, then with alcohol flushing, be washed till the ethanol of outflow without muddiness, then washes with water
To without alcohol taste；
B () is then soaked with HCl solution, wash with water to neutrality, then is soaked with NaOH solution, is washed with water to neutrality, is processed
Macroporous absorbent resin afterwards；
C () terminates to this；Or repeat step (b) 2～3 times.
7. the method that utilization macroporous absorbent resin according to claim 6 separates water-soluble monascus pigment, it is characterised in that：
The concentration of the ethanol described in step (a) is percent by volume 95%；
The time soaked with ethanol described in step (a) is 8～24h；
Water described in step (a) and step (b) is distilled water or deionized water；
The concentration of the HCl solution described in step (b) is percent by volume 2～8%；
The time soaked with HCl solution described in step (b) is 2～8h；
The concentration of the NaOH solution described in step (b) is percent by volume 2～8%；
The time soaked with NaOH solution described in step (b) is 2～8h.
8. the method that utilization macroporous absorbent resin according to claim 1 separates water-soluble monascus pigment, it is characterised in that：
Macroporous absorbent resin addition described in step (3) be by the extracellular water-soluble monascus pigment zymotic fluid proportionings 0.2 of every mL～
0.5g macroporous absorbent resins are calculated.
9. the method that utilization macroporous absorbent resin according to claim 1 separates water-soluble monascus pigment, it is characterised in that：
Monascus ruber described in step (1) is the monascus ruber (Monascus that deposit number is CGMCC No.10910
ruber)；
The composition of the culture medium of the liquid state fermentation described in step (1) is as follows：In per 100mL liquid state fermentation culture mediums, containing grape
Sugar 10～30g, (NH4)2SO4 0.5g、KH2PO4 0.5g、MgSO4·7H2O 0.05g、FeSO4·7H2O 1.0mg、ZnSO4·
7H2O 1.0mg、MnSO4·H2O 3.0mg, with water 100ml, pH natures are settled to.
10. the utilization macroporous absorbent resin described in any one of claim 1～9 separates the method for water-soluble monascus pigment in separation
Application in water-soluble monascus pigment.
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| CN201610943653.2A CN106590020B (en) | 2016-11-02 | 2016-11-02 | Utilize the method and its application of macroporous absorbent resin separation water-soluble monascus pigment |
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| CN201610943653.2A CN106590020B (en) | 2016-11-02 | 2016-11-02 | Utilize the method and its application of macroporous absorbent resin separation water-soluble monascus pigment |
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| CN106590020A true CN106590020A (en) | 2017-04-26 |
| CN106590020B CN106590020B (en) | 2019-05-14 |
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| CN201610943653.2A Active CN106590020B (en) | 2016-11-02 | 2016-11-02 | Utilize the method and its application of macroporous absorbent resin separation water-soluble monascus pigment |
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| CN107189490A (en) * | 2017-07-07 | 2017-09-22 | 福建正味生物科技有限公司 | A kind of preparation method of water-soluble High color values monascorubin |
| CN108047345A (en) * | 2017-12-21 | 2018-05-18 | 嘉兴学院 | The method of enriching and purifying black nightshade polysaccharide and the black nightshade polysaccharide obtained using this method |
| CN110437644A (en) * | 2019-08-19 | 2019-11-12 | 长江大学 | A kind of isolation and purification method of red yeast rice citraurin |
| CN111748585A (en) * | 2019-03-26 | 2020-10-09 | 长江大学 | Method for increasing yield of liquid fermentation monascus pigment |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189490A (en) * | 2017-07-07 | 2017-09-22 | 福建正味生物科技有限公司 | A kind of preparation method of water-soluble High color values monascorubin |
| CN107189490B (en) * | 2017-07-07 | 2019-06-14 | 福建正味生物科技有限公司 | A kind of preparation method of high water solubility color value monascorubin |
| CN108047345A (en) * | 2017-12-21 | 2018-05-18 | 嘉兴学院 | The method of enriching and purifying black nightshade polysaccharide and the black nightshade polysaccharide obtained using this method |
| CN111748585A (en) * | 2019-03-26 | 2020-10-09 | 长江大学 | Method for increasing yield of liquid fermentation monascus pigment |
| CN110437644A (en) * | 2019-08-19 | 2019-11-12 | 长江大学 | A kind of isolation and purification method of red yeast rice citraurin |
| CN110437644B (en) * | 2019-08-19 | 2020-08-07 | 长江大学 | Separation and purification method of monascus orange pigment |
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