CN104448918B - A kind of method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying - Google Patents
A kind of method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying Download PDFInfo
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- CN104448918B CN104448918B CN201410809380.3A CN201410809380A CN104448918B CN 104448918 B CN104448918 B CN 104448918B CN 201410809380 A CN201410809380 A CN 201410809380A CN 104448918 B CN104448918 B CN 104448918B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
- B01J2220/60—Use in several different columns
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Abstract
The invention discloses a kind of method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying, comprise the following steps: the 1) preparation of the red wooden carthamin concentrate that continues: first from the red wooden pollen end of continuing, lixiviate goes out the red wooden carthamin extract that continues, again the red wooden carthamin extract that continues is concentrated, prepare the red wooden carthamin concentrate that continues; 2) purifying of the red wooden carthamin that continues: using aluminium oxide and calcium carbonate as compound adsorbent, carry out after upper prop absorption continue wooden carthamin concentrate red, carry out wash-out with eluant, eluent, obtain the red wooden carthamin chromatographic solution that continues after purifying. It is that the activation neutral alumina of 2:1 and calcium carbonate are as compound adsorbent, to the good separating effect of the red wooden carthamin that continues that the present invention adopts mass ratio; The activation neutral alumina adopting and calcium carbonate are as compound adsorbent, and price is the most cheap, with short production cycle, do not need complex apparatus, thereby production cost are low simultaneously, and production efficiency is high, and equipment investment is little.
Description
Technical field
The present invention relates to a kind of purification process of natural colouring matter, relate in particular to one and utilize aluminium oxide-calcium carbonate compound adsorbent purifyingThe method of the red wooden carthamin that continues.
Background technology
Pigment, according to the difference in source, can be divided into natural colouring matter and synthetic dyestuff. Along with much research shows some synthetic dyestuff pairHuman body, except general toxicity, also has other illeffects such as mutagenesis and carcinogenicity, in view of synthetic dyestuff is to the existing danger of human bodyEvil property, increasing people pays close attention to the development and utilization of natural colouring matter. Natural colouring matter is safe and reliable, color and luster nature not only, andWhat have also has nutrition and pharmacological action concurrently, thereby extremely people's favor, especially in recent years along with pollution-free food and natural cosmeticsPopularization day by day and large-scale application, development and utilization natural colouring matter has become the focus of whole world food service industry and cosmetic industry,It has been trend of the times that the natural colouring matter of application safety Nantural non-toxic replaces synthetic dyestuff.
The red wood that continues, has another name called the safflower wood that continues, and calls red fetters wood, the red flower that continues, and for Hamamelidaceae evergreen shrubs or dungarunga, mainly dividesBe distributed in middle and lower reach of Yangtze River areas to the south and north India. The red wooden premium that continues, Ye Hong, root are red, mainly do at present greening and view and admire, quiltGardening circle is called all-round greening fancy breed, considerable leaf, sees flower, reward shape, spends time in full bloom of dazzling beautyly, can repeatedly open in 1 yearFlower, adaptability, germination are strong, are common horticultural gardening plants. The red wood flower that continues all contains abundant natural red colouring matter with leaf, isWell natural pigment resource, especially to spend middle haematochrome content maximum, the red wooden haematochrome that continues belongs to anthocyanidin, flowerForm mainly with anthocyanin under blue or green plain nature exists.
In the red branch that continues of bibliographical information, contain tannin, in seed, containing multiple aliphatic acid, in spending, contain isoquercitrin and haematochrome, Ye ZhongContaining tannin, reduced sugar, glycoside, flavonoids, aldehydes matter and organic acid, the red wood flower that continues, root, Ye Junke are used for medicinal purpose, and haveAnti-inflammation, hemostasis are invigorated blood circulation, antipyretic analgesic, the multiple efficacies such as anti-oxidant, and the western Hunan is among the people also the red wooden medicinal folk prescription that continues. At presentResearch shown that the red wooden haematochrome that continues has the stronger effect such as antibacterial and anti-oxidant, except can be used for developing antibiosis anti-inflammatory drug beyond the region of objective existence,Also can be used as antibiotic antiseptic and the toner of food, the raw material of the cosmetics such as nail polish and lipstick and the additive of other products,Have bibliographical information to show the red haematochrome nontoxicity that continues wooden through small white mouse toxicity test, the red wooden haematochrome that continues is not only nontoxic to be done without mutagenesisWith, and there is treatment characteristic, the red wooden haematochrome that continues is the good raw material of natural colouring matter, has wide development and utilization prospect,Therefore the red wooden carthamin that continues of reasonable development, to ensureing consumer health, promotes the development of food industry and cosmetics industry, splitsSending out utilizes the research of natural colouring matter significant.
In the time developing natural colouring matter, in order to obtain the product that purity is higher, need to carry out pigment semifinished product further pureChange. The purification process of natural colouring matter is broadly divided into solvent extraction, Amberlyst process, ion-exchange-resin process, alumina methodWith silica gel method etc. These technical methods are with single technical method or the fixing pigment separated that carries out mutually of single adsorption substantially at presentPurifying, thereby there is the shortcomings such as pigment product purity is low, also need to carry out further separation and purification with other technical method techniqueComplexity, the production cycle is long, and cost is high.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provides one to utilize aluminium oxide-calcium carbonate composite adsorptionThe method of the red wooden carthamin that continues of agent purifying.
The technical scheme that the present invention proposes is:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying, comprises the following steps:
1) preparation of the red wooden carthamin concentrate that continues: first lixiviate goes out the red wooden carthamin extract that continues from the red wooden pollen end of continuing,Again the described red wooden carthamin extract that continues is concentrated, prepare the red wooden carthamin concentrate that continues;
2) purifying of the red wooden carthamin that continues: using aluminium oxide and calcium carbonate as compound adsorbent, to the described red wooden premium look that continuesElement concentrate carries out after upper prop absorption, carries out wash-out with eluant, eluent, obtains the red wooden carthamin chromatographic solution that continues after purifying.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, aluminium oxide is activation neutral alumina;The mass ratio of described activation neutral alumina and calcium carbonate is 2:1.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, compound adsorbent is divided into 2 layers, underLayer is calcium carbonate, and upper strata is activation neutral alumina; The upper prop process of compound adsorbent is: first calcium carbonate dry method dress post is placed inChromatographic column bottom, then will activate after neutral alumina and 70% ethanolic solution stirring immersion 10min, wet method dress post is in chromatographic columnCalcium carbonate on.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, the activation of activation neutral aluminaJourney is neutral alumina to be placed in to 150～160 DEG C process 4h and complete activation.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, every gram of red continuing of Composite Adsorbent AbsorbingThe volume of wood carthamin concentrate is 0.667ml～1.333ml; Flow velocity when the red wooden carthamin concentrate that continues is adsorbedBe 10～70/min.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, the absorption of every gram of activation neutral aluminaThe volume of the red wooden carthamin concentrate that continues is 1.333ml; Flow velocity when the red wooden carthamin concentrate that continues is adsorbed is 10Drip/min.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, eluant, eluent is ethanolic solution; DescribedThe concentration of ethanolic solution is that 30%～90%, PH is 2～8.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, flow velocity when eluant, eluent wash-out is 10～70/min.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 2) in, eluant, eluent is that concentration is 50% secondAlcoholic solution, PH=6; Flow velocity when eluant, eluent wash-out is 30/min, and the volume of eluant, eluent is 5 times of resin bed volumes.
The method of the red wooden carthamin that continues of above-mentioned purifying, preferred, described step 1) in, the red wooden carthamin extract that continuesPreparation process is: first take the red wooden pollen end of continuing, then the amount that is 1g:10ml by the red solid-liquid ratio that continues wooden pollen end and 40% acetic acid,The red wooden pollen end of continuing is immersed in to 20min in 40% acetic acid, then Microwave Extraction 2 times, extract 1min at every turn, prepare red continuingWood carthamin extract; In the red wooden carthamin concentrate that continues, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The neutral alumina that the present invention uses is porous loose structure, the fine sand shape that is white in color, and granularity, between 100～300 orders, is changedPurity is high, at 150～160 DEG C of activation processing 4h, the absorption of pigment is belonged to physical absorption before upper prop, also have necessarily simultaneously fromThe character of sub-exchanger, the adsorption capacity difference of aluminium oxide to opposed polarity material. Aluminium oxide, than the high adsorption capacity of silica gel, is livedProperty high, solution transmission rates is fast, chromatography is effective, regeneration easily, the advantages such as long service life; Neutral alumina be applicable to aldehyde,Quinone, ketone and some glycosides, can also be used to separate weak organic bronsted lowry acids and bases bronsted lowry etc., the red wooden carthamin that continues can be dissolved in acid solution andHighly stable, illustrate that it is a kind of weak alkali or organic acid, thereby neutral alumina is applicable to the separation and purification of the red wooden carthamin that continues.In addition, the suction-operated of calcium carbonate is mainly determined by two factors: first is formed by the calcium ion that is wrapped in particle surfaceThere is chosen anion exchange layer; Second is the good dispersion degree of new system calcium carbonate. Thereby the adsorbable a large amount of look of calcium carbonateElement class coloring matter, and be reversible to the absorption of coloring matter.
Compared with prior art, the invention has the advantages that:
1) to adopt mass ratio be that the activation neutral alumina of 2:1 and calcium carbonate are as compound adsorbent, to the red wooden premium that continues in the present inventionThe good separating effect of pigment;
2) the activation neutral alumina that the present invention adopts and calcium carbonate are as compound adsorbent, and price is the most cheap, with short production cycle,Do not need complex apparatus, thereby production cost is low, production efficiency is high simultaneously, and equipment investment is little;
3) the invention provides a kind of environmental protection, low cost, highly purified separating and purifying technology, is the red wooden carthamin that continuesResearch and development new separation and purification optimum process condition is provided, there is positive meaning.
Brief description of the drawings
Fig. 1 is that the adsorbance of the embodiment of the present invention 1 compound adsorbent is on the comparison diagram that affects of adsorption effect.
Fig. 2 is the affect comparison diagrams of the embodiment of the present invention 2 upper prop flow velocities on adsorption effect.
Fig. 3 is the affect comparison diagrams of the embodiment of the present invention 3 eluant, eluent PH on elute effect.
Fig. 4 is the affect comparison diagrams of the embodiment of the present invention 4 eluant strengths on elute effect.
Fig. 5 is the affect comparison diagrams of the embodiment of the present invention 5 eluant, eluent consumptions on elute effect.
Fig. 6 is the affect comparison diagrams of the embodiment of the present invention 6 eluant, eluent flow velocitys on elute effect.
Detailed description of the invention
For the ease of understanding the present invention, below in connection with Figure of description and preferred embodiment to the present invention do more comprehensively, carefulGround is described, but protection scope of the present invention is not limited to following specific embodiment.
Unless otherwise defined, all technical terms of hereinafter using are identical with the implication that those skilled in the art understand conventionally.Technical term used herein, just in order to describe the object of specific embodiment, is not to be intended to limit protection model of the present inventionEnclose.
Embodiment 1:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get respectively red wooden carthamin concentrate 5ml, 10ml, 15ml and the 20ml of continuing, be all diluted to 20ml, then go up respectivelyPost, with the flow velocity of 30/min Dynamic Adsorption 2 times repeatedly, then uses respectively 20ml, PH=6,50% ethanolic solution with 30The flow velocity of/min carries out wash-out, obtains the red wooden carthamin chromatographic solution that continues after purifying.
Get upper prop liquid (when upper prop red in wooden carthamin concentrate) with 30/min flow velocity repeatedly after Dynamic Adsorption 2 timesEfflux, the efflux of measuring every chromatographic column is the absorbance under 520nm at wavelength, its result is as shown in Figure 1.
As shown in Figure 1, the volume of every gram of red wooden carthamin concentrate that continues of Composite Adsorbent Absorbing, at 0.667～1.333ml, is inhaledLuminosity is all smaller, and wherein the volume of every gram of red wooden carthamin concentrate that continues of Composite Adsorbent Absorbing is 0.667ml and 1.333mlTime, absorbance is more or less the same, and considers more polychrom of aluminium oxide-calcium carbonate Composite Adsorbent Absorbing, selects best scheme for everyThe volume of gram red wooden carthamin concentrate that continues of aluminium oxide-calcium carbonate Composite Adsorbent Absorbing is 1.333ml (namely 7.5g oxidationThe best upper column quantity of aluminium-calcium carbonate compound adsorbent is 10ml).
Embodiment 2:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get 4 parts of red wooden carthamin concentrate 10ml that continue, be all diluted to 20ml, then upper prop respectively, respectively with 10,30,The flow velocity of 50 and 70/min Dynamic Adsorption 1 time repeatedly, then use respectively 20ml, PH=6,50% ethanolic solution with 30/minFlow velocity carry out wash-out, obtain the red wooden carthamin chromatographic solution that continues after purifying.
Get the efflux after upper prop liquid adsorbs with different in flow rate, the efflux of measuring every chromatographic column is the suction under 520nm at wavelengthLuminosity, its result as shown in Figure 2.
As can be seen from Figure 2, when upper prop flow velocity is 10/min, absorbance minimum, and absorbance is less, and adsorbent suction is describedAttached effect is better, so best upper prop flow velocity is 10/min.
Embodiment 3:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get 4 parts of red wooden carthamin concentrate 10ml that continue, be all diluted to 20ml, then distinguish upper prop, with the stream of 10/minSpeed Dynamic Adsorption 2 times repeatedly, more respectively with PH be 2,4,6 and 8 50% ethanolic solution (volume is 20ml) withThe flow velocity of 30/min carries out wash-out, obtains the red wooden carthamin chromatographic solution that continues after purifying.
After taking the eluant, eluent wash-out of different PH, obtain the red wooden carthamin chromatographic solution (being eluent) that continues, measure every chromatographic columnThe eluent flowing out is the absorbance under 520nm at wavelength, and its result as shown in Figure 3.
As shown in Figure 3, when PH=6, the light absorption value maximum of eluent, the absorbance of eluent is larger, illustrates that elute effect is moreGood, the separating effect of the red wooden carthamin that continues is better, so best eluant, eluent pH value is 6.
Embodiment 4:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get 4 parts of red wooden carthamin concentrate 10ml that continue, be all diluted to 20ml, then distinguish upper prop, with the stream of 10/minSpeed Dynamic Adsorption 2 times repeatedly, then be that (PH is 6, volume for 30%, 50%, 70% and 90% ethanolic solution by concentration respectivelyBe 20ml) carry out wash-out with the flow velocity of 30/min, obtain the red wooden carthamin chromatographic solution that continues after purifying.
After taking the eluant, eluent wash-out of variable concentrations, obtain the red wooden carthamin chromatographic solution (being eluent) that continues, measure every chromatographic columnThe eluent flowing out is the absorbance under 520nm at wavelength, and its result as shown in Figure 4.
As can be seen from Figure 4, in the time that eluant strength is 50%, the absorbance maximum of eluent, the absorbance of eluent is larger,Illustrate that elute effect is better, the separating effect of the red wooden carthamin that continues is better, so best eluant strength is 50%.
Embodiment 5:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get 4 parts of red wooden carthamin concentrate 10ml that continue, be all diluted to 20ml, then distinguish upper prop, with the stream of 10/minSpeed Dynamic Adsorption 2 times repeatedly, then be that (PH is for 50% ethanolic solution of 10ml, 15ml, 20ml and 25ml with volume respectively6) carry out wash-out with the flow velocity of 30/min, obtain the red wooden carthamin chromatographic solution that continues after purifying.
After taking the eluant, eluent wash-out of different volumes, obtain the red wooden carthamin chromatographic solution (being eluent) that continues, measure every chromatographic columnThe eluent flowing out is the absorbance under 520nm at wavelength, and its result as shown in Figure 5.
As can be seen from Figure 5, the volume of eluant, eluent is 20 and when 25ml, and absorbance is more or less the same, and the absorbance of eluentBe worth greatlyr, illustrate that elute effect is better, the separating effect of the red wooden carthamin that continues is better, thus consider from economic interests,Good eluant, eluent volume is 20ml, i.e. 5 times of resin bed volumes.
Embodiment 6:
A method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying of the present invention, comprises following stepRapid:
First take the red wooden pollen end of continuing, then by red wooden pollen end and the amount that the solid-liquid ratio of 40% acetic acid is 1g:10ml of continuing, continue redWood pollen end is immersed in 20min in 40% acetic acid, and Microwave Extraction 2 times is extracted 1min at every turn, prepares the red wooden premium look that continuesElement extract; Recycling Rotary Evaporators concentrates the red wooden carthamin extract that continues, and makes the red wooden carthamin that continues obtainingIn concentrate, every milliliter of concentrate contains the red wooden pollen 0.291g that continues.
The activation processing of neutral alumina: neutral alumina is placed in to 150～160 DEG C and processes 4h and complete activation process.
First take 4 parts of 2.5g calcium carbonate, dry column-packing is placed in 4 chromatographic column bottoms respectively, then takes 4 parts of 5g and activate neutral oxygenChange aluminium and 70% ethanolic solution and stir after immersion 10min, respectively on the calcium carbonate of wet method dress post in 4 chromatographic columns.
Get 4 parts of red wooden carthamin concentrate 10ml that continue, be all diluted to 20ml, then distinguish upper prop, with the stream of 10/minSpeed Dynamic Adsorption 2 times repeatedly, then use 20ml50% ethanolic solution (PH is 6) respectively with 10,30,50 and 70/minFlow velocity carry out wash-out, obtain the red wooden carthamin chromatographic solution that continues after purifying.
After taking the eluant, eluent wash-out of different in flow rate, obtain the red wooden carthamin chromatographic solution (being eluent) that continues, measure every chromatographic columnThe eluent flowing out is the absorbance under 520nm at wavelength, and its result as shown in Figure 6.
As can be seen from Figure 6, when the flow velocity of eluant, eluent is 30/min, the absorbance maximum of eluent, and eluent is inhaledShading value is larger, illustrates that elute effect is better, and the separating effect of the red wooden carthamin that continues is better, so eluant, eluent optimum flow rateBe 30/min.
Claims (8)
1. a method of utilizing the red wooden carthamin that continues of aluminium oxide-calcium carbonate compound adsorbent purifying, is characterized in that, comprises followingStep:
1) preparation of the red wooden carthamin concentrate that continues: first lixiviate goes out the red wooden carthamin extract that continues from the red wooden pollen end of continuing, more rightThe described red wooden carthamin extract that continues concentrates, and prepares the red wooden carthamin concentrate that continues;
2) purifying of the red wooden carthamin that continues: using aluminium oxide and calcium carbonate as compound adsorbent, dense to the described red wooden carthamin that continuesContracting liquid carries out after upper prop absorption, carries out wash-out with eluant, eluent, obtains the red wooden carthamin chromatographic solution that continues after purifying;
Described aluminium oxide is activation neutral alumina; The mass ratio of described activation neutral alumina and calcium carbonate is 2:1;
Described compound adsorbent is divided into 2 layers, and lower floor is calcium carbonate, and upper strata is activation neutral alumina; The upper prop process of compound adsorbentFor: first calcium carbonate dry method dress post is placed in to chromatographic column bottom, then will activates neutral alumina and 70% ethanolic solution stirring immersionAfter 10min, on the calcium carbonate of wet method dress post in chromatographic column.
2. the method for the red wooden carthamin that continues of purifying as claimed in claim 1, is characterized in that, described step 2) in, in activationThe activation process of property aluminium oxide is neutral alumina to be placed in to 150～160 DEG C process 4h and complete activation.
3. the method for the red wooden carthamin that continues of purifying as claimed in claim 2, is characterized in that, described step 2) in, every gram is multipleThe volume that closes the red wooden carthamin concentrate that continues of adsorbent absorption is 0.667mL～1.333mL; To the red wooden carthamin concentrate that continuesFlow velocity while absorption is 10～70/min.
4. the method for the red wooden carthamin that continues of purifying as claimed in claim 3, is characterized in that, described step 2) in, every gram is multipleThe volume that closes the red wooden carthamin concentrate that continues of adsorbent absorption is 1.333mL; The red wooden carthamin concentrate that continues is adsorbedTime flow velocity be 10/min.
5. the method for the red wooden carthamin that continues of purifying as claimed in claim 4, is characterized in that, described step 2) in, eluant, eluentFor ethanolic solution; The concentration of described ethanolic solution is that 30%～90%, pH is 2～8.
6. the method for the red wooden carthamin that continues of purifying as claimed in claim 5, is characterized in that, described step 2) in, eluant, eluentFlow velocity when wash-out is 10～70/min.
7. the method for the red wooden carthamin that continues of purifying as claimed in claim 6, is characterized in that, described step 2) in, eluant, eluentFor the concentration ethanolic solution that is 50%, pH=6, flow velocity when eluant, eluent wash-out is 30/min, the volume of eluant, eluent is 5 timesResin bed volume.
8. as a method for the red wooden carthamin that continues of purifying as described in claim 1～7 any one, it is characterized in that described step 1)In, the preparation process of the red wooden carthamin extract that continues is: first take the red wooden pollen end of continuing, then by red wooden pollen end and 40% of continuingThe solid-liquid ratio of acetic acid is the amount of 1g:10mL, and the red wooden pollen end of continuing is immersed in to 20min in 40% acetic acid, then Microwave Extraction 2 times,Each 1min that extracts, prepares the red wooden carthamin extract that continues; In the red wooden carthamin concentrate that continues, every milliliter of concentrate containsThere is the red wooden pollen 0.291g that continues.
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