CN108676381A - The extraction preparation method of Bauhinia blakeana carthamin - Google Patents
The extraction preparation method of Bauhinia blakeana carthamin Download PDFInfo
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- CN108676381A CN108676381A CN201810767462.4A CN201810767462A CN108676381A CN 108676381 A CN108676381 A CN 108676381A CN 201810767462 A CN201810767462 A CN 201810767462A CN 108676381 A CN108676381 A CN 108676381A
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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
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Abstract
The invention discloses a kind of extraction preparation methods of Bauhinia blakeana carthamin, include the following steps：1) it is 1 by solid-to-liquid ratio by Bauhinia blakeana pollen end and distilled water:15~1:20 (g/mL) are mixed, and with ultrasonic wave extraction, extracting solution is filtered, obtains filtrate；Or it is 1 that solid-to-liquid ratio is pressed at Bauhinia blakeana pollen end and distilled water:10~1:20 (g/mL) are mixed, and with Microwave Extraction, gained extracting solution are filtered, filtrate is obtained；Or solid-to-liquid ratio 1 is pressed at Bauhinia blakeana pollen end and distilled water:20~1:40 (g/mL) are mixed, and gained extracting solution is filtered, obtains filtrate by mechanical agitation extraction；2) above-mentioned pigment filtrate decompression is concentrated, and activated D101 macroreticular resins is packed into chromatographic column, with distilled water flushing balance resin column until interlaminar resin does not have apparent bubble；Filtrate after concentration is packed into chromatographic column, until after pigment is all adsorbed on resin, is eluted, be eluted to efflux it is colourless until, eluent is collected in concentration, and eluent is concentrated under reduced pressure and obtains lotion, then lotion is dried to obtain Bauhinia blakeana carthamin.
Description
Technical field
The present invention relates to technical field of pigment extraction, it particularly relates to a kind of extraction of Bauhinia blakeana carthamin
Preparation method.
Background technology
Bauhinia blakeana (Bauhinia blakeana Dunn) alias Chinese redbud, pulse family Caesalpinoidea Bauhinia, extensively
General distribution in south China, the ground such as Yunnan.In south China, Bauhinia blakeana is planted extensively as a kind of green plants, flower
Phase is long, flower amount is big, pigment content is high.Studies have shown that the pigment of Bauhinia blakeana flower has significant antioxidant activity, inhibits thin
The bioactivity such as bacterium have inhibition, also, safflower sheep hoof to Escherichia coli, staphylococcus aureus, bacillus subtilis etc.
For a kind of anthocyanidin, there is soluble easily in water, dilute alcohol, dilute acid soln, the characteristic for being practically insoluble in the organic solvents such as acetone, ether,
It is in beautiful red in an acidic solution, aqueous solution has the characteristic of heat-resisting, fast light, resistance to sugar, salt tolerant.Researcher is by safety
Experiment, by the way that mouse feeding and observation, safety is higher, growth and development, and Physiology and biochemistry, histology and morphology structure are not found
What has influence, and nontoxic long-pending phenomenon occurs, and is a kind of food color, additive of ideal green natural.Therefore, for
The meaning for preparing own profound of Bauhinia blakeana haematochrome.
In the prior art, mainly there are microwave loss mechanisms, ultrasonic wave for the extracting method of Bauhinia blakeana carthamin
Extraction method, solvent extraction method, extractant is mostly acid-water, acid-ethyl alcohol or alcohol-water, extractant acid adding pair in the prior art
Extraction equipment is more demanding, and environmental pollution is also larger, and production cost is increased with ethanol-water solution, also not friendly to environment
It is good.I.e. there are production cost height for extractant used in the prior art, the deficiencies of causing serious pollution to the environment.And it is further not right
Product carries out separation and concentration, and the product obtained contains a large amount of non-pigmented ingredients such as polysaccharide, contains more impurity in product, in turn
Lead to the unstable quality of product so that the stability of product is not poor, easy to maintain, and gained pigment product purity is relatively low, also increases
Production cost is added.
Invention content
In place of overcoming the shortcomings of the prior art, defect of the existing technology is carried out comprehensive
Close evaluation on the basis of analysis, the present invention provide it is a kind of ensure it is simple for process it is easy to operate, extraction efficiency is high under the premise of, use
Distilled water the technologies such as detaches with macroporous resin column chromatography and combines and remove the impurity such as a large amount of polysaccharide as Extraction solvent, is promoted
The purity of product, and then reduce the production cost of Bauhinia blakeana carthamin and the pollution to environment, it is ensured that the quality of product
Stability, the natural food colour for making acquisition be easy long-term preservation extract preparation method.
To achieve the above object, the technical solution taken：
A kind of extraction preparation method of Bauhinia blakeana carthamin, includes the following steps：
1) it is 1 by solid-to-liquid ratio by Bauhinia blakeana pollen end and distilled water:15~1:20 (g/mL) are mixed, and are carried with ultrasonic wave
It takes, gained extracting solution is filtered, filtrate is obtained；
Or it is 1 that solid-to-liquid ratio is pressed at Bauhinia blakeana pollen end and distilled water:10~1:20 (g/mL) are mixed, and are carried with microwave
It takes, gained extracting solution is filtered, filtrate is obtained；
Or solid-to-liquid ratio 1 is pressed at Bauhinia blakeana pollen end and distilled water:20~1:40 (g/mL) are mixed, and mechanical agitation carries
It takes, gained extracting solution is filtered, filtrate is obtained；
2) above-mentioned pigment filtrate decompression is concentrated, activated D101 macroreticular resins is packed into chromatographic column, are rushed with distilled water
Balance resin column is washed until interlaminar resin does not have apparent bubble；Filtrate after concentration is packed into chromatographic column, until pigment is all adsorbed on
After on resin, eluted, be eluted to efflux it is colourless until, concentration collect eluent, by eluent be concentrated under reduced pressure obtain it is red
Flower mountain ebony carthamin lotion, then Bauhinia blakeana carthamin lotion is dried to obtain Bauhinia blakeana carthamin.
Preferably, it uses ultrasonic wave at 60~70 DEG C in the step 1), extracts 40~50min, and extract 2~3 times.
Preferably, the use microwave in the step 1) is that 400~600W is carried under the conditions of temperature is 50~70 DEG C in power
15~25min is taken, and is extracted 2~4 times, obtained extracting solution filtering obtains filtrate.
Preferably, under the conditions of low whipping speed is 20~30r/s in the step 1), mechanical agitation is extracted 2~3 times, will
Gained extracting solution, filtering, obtains filtrate.
Preferably, in the step 2) by above-mentioned pigment filtrate bath temperature be 50~70 DEG C, vacuum degree 0.09Mpa
It is concentrated under reduced pressure into 0.3~0.7 times of remaining extracting liquid volume, waits for upper prop.
Preferably, the filtrate after concentration is packed into chromatographic column by the step 2), and coutroi velocity is 0.3~0.8mL/s.
Preferably, after the step 2) pigment is all adsorbed on resin, first with distillation water elution, flow velocity be 1.0~
1.5mL/s, be eluted to efflux be it is colourless until, then with 60~80% ethanol-water solutions elution by the color of macroporous resin adsorption
Element, flow velocity be 0.8~1.5mL/s, be eluted to efflux it is colourless until.
Preferably, the D101 macroreticular resins activation in the step 2) is small with 0.01mol/L Hcl solution immersion resin 4
When, it is eluted with water and is washed till eluate and is in neutrality；It uses 0.01mol/L NaOH solutions to impregnate resin 2h again, is finally eluted with water to washing
Go out liquid to be in neutrality, for use.
Preferably, the chromatographic column selects normal pressure glass chromatography column, draw ratio 40:1~46.5:1.
Preferably, described 3~4 times of column volumes of distillation water consumption；60~80% ethanol-water solution dosages are 1.0~1.5 times
Column volume.
Advantageous effect：
Under the premise of extraction process is simple to operation, extraction efficiency is high of the Bauhinia blakeana carthamin of the present invention, is used
Distilled water the technologies such as detaches with macroporous resin column chromatography and combines and remove the impurity such as a large amount of polysaccharide as Extraction solvent, is promoted
The purity of product, and then reduce the production cost of Bauhinia blakeana carthamin and the pollution to environment, it is ensured that the quality of product
Stability obtains the natural food colour extraction preparation method for being easy long-term preservation.
Specific implementation mode
Below in conjunction with specific embodiment, the invention will be further described.It should be understood that following embodiment is merely to illustrate this
Invention is not for restriction the scope of the present invention.Therefore all Method And Principles according to described in present patent application range done it is equivalent
Variation or modification, are included within the scope of present patent application.
The invention discloses a kind of extraction preparation methods of Bauhinia blakeana carthamin, include the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 40
6~7h is dried in~50 DEG C of baking oven or is dried in the shade naturally, and 80 mesh sieve is then crushed.
2) pigment extracts：It is 1 that solid-to-liquid ratio is pressed at Bauhinia blakeana pollen end and distilled water:15~1:20 (g/mL) are mixed,
With ultrasonic wave 60~70 DEG C, power be 60~80W under the conditions of, extract 40~50min, extract 2~3 times, obtained extracting solution
With 80 mesh filtered through gauze, then with filtered on buchner funnel, filtrate is obtained；
Or it is 1 that solid-to-liquid ratio is pressed at Bauhinia blakeana pollen end and distilled water:10~1:20 (g/mL), with microwave in power
For 400~600W, under the conditions of temperature is 50~70 DEG C, 15~25min is extracted, and extract 2~4 times, obtained extracting solution is with 80
Mesh filtered through gauze, then with filtered on buchner funnel, obtain filtrate；
Or solid-to-liquid ratio 1 is pressed at Bauhinia blakeana pollen end and distilled water:20~1:40 (g/mL), 50~60 DEG C, stir
20~30r/s of speed is mixed, mechanical agitation extracts 60~120min, extracts 2~3 times, by gained extracting solution, with 80 mesh gauze mistakes
Filter, then with filtered on buchner funnel, obtain filtrate.
3) pigment separated is enriched with：By above-mentioned pigment filtrate bath temperature be 50~70 DEG C, vacuum degree be 0.09Mpa decompression
It is concentrated into 0.3~0.7 times of remaining extracting liquid volume, waits for upper prop；Activated D101 macroreticular resins are packed into chromatographic column, with distillation
Water rinses balance resin column until interlaminar resin does not have apparent bubble.Filtrate after concentration is packed into chromatographic column, coutroi velocity 0.3
~0.8mL/s, until after pigment is all adsorbed on resin, first with distillation water elution, flow velocity is 1.0~1.5mL/s, is eluted to stream
Go out until liquid is colourless, then with the elution of 60~80% ethanol-water solutions by the pigment of macroporous resin adsorption, flow velocity for 0.8~
1.5mL/s, be eluted to efflux it is colourless until, concentrate the alcohol-water eluent of collection, by eluent bath temperature be 60~
70 DEG C, vacuum degree is that 0.09Mpa is concentrated under reduced pressure and obtains Bauhinia blakeana carthamin lotion, then by Bauhinia blakeana carthamin
Lotion dry 6~8h in 40~60 DEG C of baking oven, obtains Bauhinia blakeana carthamin.
The separation material of the present invention selects D101 macroreticular resins, D101 macroreticular resins activation molten with 0.01mol/L HCL
Liquid impregnates resin 4 hours, is eluted with water and is washed till eluate and is in neutrality；0.01mol/L NaOH solutions are used to impregnate resin 2h again, most
After be eluted with water to eluate and be in neutrality, for use.
Above-mentioned chromatographic column selects normal pressure glass chromatography column, draw ratio 40:1~46.5:1.
Above-mentioned resin demand is：Bauhinia blakeana spends sample size：Column volume=1 of resin:16~1:19, g/cm3。
Above-mentioned step 3) distills 3~4 times of column volumes of water consumption；Alcohol-water eluent dosage is 1.0~1.5 times of cylinders
Product.
Embodiment 1
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 40
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 40g is weighed, distilled water 600mL (solid-to-liquid ratios 1 are added:15, g/mL),
40min is extracted under the conditions of temperature 70 C, power 80W with ultrasonic wave, is extracted 2 times, 80 mesh filtered through gauze, merging filtrate.
3) pigment separated is enriched with：By above-mentioned steps 2) in filtrate bath temperature be 65 DEG C, vacuum degree subtracts for 0.09Mpa
Pressure is concentrated into 0.3 times of remaining extracting liquid volume, and it is 46.5 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1
Normal pressure glass chromatography column, resin column volume are 760cm3(Bauhinia blakeana spends sample size：The column volume of resin is 1:18g/cm3),
After there is no apparent bubble with distilled water flushing to interlaminar resin, by above-mentioned concentrate upper prop, coutroi velocity 0.3mL/s, until color
Element be all adsorbed on resin after, first with distillation water elution, flow velocity 1.0mL/s, be eluted to efflux be it is colourless until (water consumption
For 4 times of column volumes), then eluted by the pigment of macroporous resin adsorption for 60% ethanol-water solution with volume fraction of ethanol, flow velocity is
1.0mL/s, be eluted to efflux it is colourless until (eluting agent be 1.5 times of column volumes), concentrate the alcohol-water elution of collection
Liquid, by eluent bath temperature be 70 DEG C, vacuum degree be 0.09Mpa be concentrated under reduced pressure obtain Bauhinia blakeana carthamin cream
Body, then Bauhinia blakeana carthamin lotion is dried into 7h in 60 DEG C of baking oven, Bauhinia blakeana carthamin product is obtained,
Pigment quality is 2.42g, and the pigment yield of the present embodiment is 6.0%.
Embodiment 2
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 6h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 20g is weighed, distilled water 360mL (solid-to-liquid ratios 1 are added:18, g/mL),
With ultrasonic wave under the conditions of temperature 60 C, power 70W, extraction time 50min is extracted 3 times, 80 mesh filtered through gauze, merging filtrate.
3) pigment separated is enriched with：Filtrate is 60 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extraction
0.5 times of liquid product.It is 40 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, resin
Column volume is 348cm3(extraction sample size：Column volume=1 of resin:18g/cm3) unapparent to interlaminar resin with distilled water flushing
Bubble after, by above-mentioned concentrate upper prop, coutroi velocity 0.3mL/s first uses distilled water until after pigment is all adsorbed on resin
Elution, flow velocity 1.0mL/s are eluted to efflux and stop (3.7 times of column volumes of water consumption) to be colourless, then be with volume fraction of ethanol
The elution of 70% ethanol-water solution is by the pigment of macroporous resin adsorption, flow velocity 1.2mL/s, be eluted to efflux it is colourless until (wash
De- agent dosage is 1.3 times of column volumes), the alcohol-water eluent of collection is concentrated, in bath temperature is 60 DEG C by eluent, vacuum
Degree is 0.09Mpa reduced pressure acquisition Bauhinia blakeana carthamin lotions, then by Bauhinia blakeana carthamin lotion 60
DEG C baking oven in dry 6h, obtain Bauhinia blakeana carthamin product, pigment quality is 1.20g, pigment yield 6.0%.
Embodiment 3
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 6h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 20g is weighed, distilled water 400mL (solid-to-liquid ratios 1 are added:20, g/mL),
With ultrasonic wave under the conditions of 65 DEG C of temperature, power 60W, extraction time 45min is extracted 3 times, 80 mesh filtered through gauze, merging filtrate.
3) pigment separated is enriched with：Filtrate is 65 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extraction
0.3 times of liquid product.It is 40 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, resin
Column volume is 348cm3(extraction sample size：Column volume=1 of resin:18g/cm3) unapparent to interlaminar resin with distilled water flushing
Bubble after, by above-mentioned concentrate upper prop, coutroi velocity 0.3mL/s first uses distilled water until after pigment is all adsorbed on resin
Elution, flow velocity 1.0mL/s are eluted to efflux and stop (3.7 times of column volumes of water consumption) to be colourless, then be with volume fraction of ethanol
The elution of 70% ethanol-water solution is by the pigment of macroporous resin adsorption, flow velocity 1.2mL/s, be eluted to efflux it is colourless until (wash
De- agent dosage is 1.3 times of column volumes), the alcohol-water eluent of collection is concentrated, in bath temperature is 60 DEG C by eluent, vacuum
Degree is 0.09Mpa reduced pressure acquisition Bauhinia blakeana carthamin lotions, then by Bauhinia blakeana carthamin lotion 60
DEG C baking oven in dry 6h, obtain Bauhinia blakeana carthamin product, pigment quality is 1.20g, pigment yield 6.0%.
Embodiment 4
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 45
DEG C baking oven in dry 6.5h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 20g is weighed, distilled water 400mL (solid-to-liquid ratios 1 are added:20, g/mL),
With microwave in temperature 50 C, power 400W, extraction time 15min is extracted 2 times, filtered on buchner funnel again after 80 mesh filtered through gauze,
Merging filtrate.
3) pigment separated is enriched with：Filtrate is 50 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extracting solution
0.5 times.It is 46.5 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, resin column
Product is 383cm3(extraction sample size：Column volume=1 of resin:19g/cm3), it is not apparent to interlaminar resin with distilled water flushing
After bubble, by above-mentioned concentrate upper prop, coutroi velocity 0.8mL/s is first washed with distillation until after pigment is all adsorbed on resin
It is de-, flow velocity 1.0mL/s, be eluted to efflux be it is colourless only (3 times of column volumes of water consumption), then with volume fraction of ethanol be 60%
Ethanol-water solution elution is by the pigment of macroporous resin adsorption, flow velocity 1.5mL/s, be eluted to efflux it is colourless until (eluant, eluent
Dosage is 1.0 times of column volumes), the alcohol-water eluent of collection is concentrated, in bath temperature is 65 DEG C by eluent, vacuum degree is
0.09Mpa, which is concentrated under reduced pressure, obtains Bauhinia blakeana carthamin lotion, then by Bauhinia blakeana carthamin lotion at 50 DEG C
Dry 7h in baking oven, obtains Bauhinia blakeana carthamin product, and pigment quality is 1.37g, pigment yield 6.8%.
Embodiment 5
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 20g is weighed, distilled water 200mL (solid-to-liquid ratios 1 are added:10, g/mL),
15min is extracted under the conditions of temperature 60 C, power 600W with microwave, is extracted 3 times in total, Buchner funnel again after 80 mesh filtered through gauze
Filtering, merging filtrate.
3) pigment separated is enriched with：Filtrate is 60 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extraction
0.7 times of liquid product.It is 46.5 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, tree
Fat column volume is 349cm3(extraction sample size：Column volume=1 of resin:17.5g/cm3), do not have with distilled water flushing to interlaminar resin
After having apparent bubble, by above-mentioned concentrate upper prop, coutroi velocity 0.8mL/s is first used until after pigment is all adsorbed on resin
Distill water elution, flow velocity 1.5mL/s, be eluted to efflux be it is colourless until (3.8 times of column volumes of water consumption), then with volume point
Number is that 60% ethanol-water solution is eluted by the pigment of macroporous resin adsorption, flow velocity 1.0mL/s, and it is colourless only to be eluted to efflux
(eluting agent be 1.1 times of column volumes), concentrates the alcohol-water eluent of collection, in bath temperature is 60 DEG C by eluent, very
Reciprocal of duty cycle is that acquisition Bauhinia blakeana carthamin lotion is concentrated under reduced pressure in 0.09Mpa, then Bauhinia blakeana carthamin lotion is existed
Dry 6.5h in 60 DEG C of baking oven, obtains Bauhinia blakeana carthamin product, and pigment quality is 1.44g, pigment yield
7.2%.
Embodiment 6
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 20g is weighed, distilled water 300mL (solid-to-liquid ratios 1 are added:15, g/mL),
With microwave under the conditions of temperature 60 C, power 400W, 25min is extracted, is extracted 3 times altogether, then with Bu Shi again after 80 mesh filtered through gauze
Funnel filters, merging filtrate.
3) pigment separated is enriched with：Filtrate after above-mentioned merging is 60 DEG C in bath temperature, and it is dense that vacuum degree is that 0.09Mpa is depressurized
It is reduced to 0.4 times of remaining extracting liquid volume.It is 45 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass
Chromatographic column, resin column volume are 349cm3(extraction sample size：Column volume=1 of resin:17.5g/cm3), extremely with distilled water flushing
After interlaminar resin does not have apparent bubble, by above-mentioned concentrate upper prop, coutroi velocity 0.5mL/s, until pigment is all adsorbed on resin
After upper, first with distillation water elution, flow velocity 1.0mL/s, be eluted to efflux be it is colourless until (water consumption is 3.7 times of cylinders
Product), then eluted by the pigment of macroporous resin adsorption, flow velocity 0.8mL/s for 80% ethanol-water solution with volume fraction of ethanol,
Be eluted to outflow solution it is colourless until (eluting agent be 1.1 times of column volumes), concentrate the alcohol-water eluent of collection, will wash
De- liquid is 60 DEG C in bath temperature, and vacuum degree is 0.09Mpa reduced pressure acquisition Bauhinia blakeana carthamin lotions, then will be red
Flower mountain ebony carthamin lotion dry 7h in 50 DEG C of baking oven, obtains Bauhinia blakeana carthamin product, pigment quality
For 1.32g, pigment yield 6.6%.
Embodiment 7
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：Bauhinia blakeana pollen end 40g is weighed, distilled water 400mL (solid-to-liquid ratios 1 are added:10, g/mL),
With microwave under the conditions of temperature 70 C, power 500W, 20min is extracted, extracts Bu Shi leakages again after 4 times, then 80 mesh filtered through gauze altogether
Bucket filtering, merging filtrate.
3) pigment separated is enriched with：Filtrate is 65 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extracting solution
0.5 times of volume.Activated D101 macroporous absorbent resins are packed into long through than being 46.5:1 normal pressure glass chromatography column, resin
Column volume is 696cm3(extraction sample size：Column volume=1 of resin:18g/cm3), it is not bright to interlaminar resin with distilled water flushing
After aobvious bubble, by above-mentioned concentrate upper prop, coutroi velocity 0.6mL/s first uses distillation until after pigment is all adsorbed on resin
Water elution, flow velocity 1.0mL/s, be eluted to efflux be it is colourless until (4.0 times of column volumes of water consumption), then with ethyl alcohol volume divide
Number is the elution of 80% ethanol-water solution by the pigment of macroporous resin adsorption, flow velocity 1.0mL/s, is eluted to that efflux is colourless to be
Only (eluting agent be 1.1 times of column volumes), the alcohol-water eluent of collection is concentrated, in bath temperature is 65 DEG C by eluent,
Vacuum degree is that 0.09Mpa is concentrated under reduced pressure and obtains Bauhinia blakeana carthamin lotion, then by Bauhinia blakeana carthamin lotion
The dry 8h in 60 DEG C of baking oven, obtains Bauhinia blakeana carthamin product, and pigment quality is 2.82g, pigment yield
7.0%.
Embodiment 8
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：100.65g mountain ebony dried flower powder is weighed, 2.0L distilled water (solid-liquid ratios 1 are added:20(g/
ML), heating water bath, at 60 DEG C, mechanical agitation extracts 1h, mixing speed 25r/s, and gauze is filtered.Extraction twice, merges
Filtrate twice.
3) pigment separated is enriched with：Filtrate is 70 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extracting solution
0.3 times of volume.Activated D101 macroporous absorbent resins are packed into long through than being 46.5:1 normal pressure glass chromatography column, resin
Column volume is 1800cm3(extraction sample size：Column volume=1 of resin:18g/cm3), do not have with distilled water flushing to interlaminar resin
After apparent bubble, by above-mentioned concentrate upper prop, coutroi velocity 0.8mL/s is first used and is steamed until after pigment is all adsorbed on resin
Distilled water elutes, flow velocity 1.2mL/s, be eluted to efflux be it is colourless until (water consumption is 4.0 times of column volumes), then with ethyl alcohol body
Fraction is that 60% ethanol-water solution is eluted by the pigment of macroporous resin adsorption, flow velocity 1.3mL/s, be eluted to efflux without
Until color (eluting agent is 1.5 times of column volumes), the alcohol-water eluent of collection is concentrated, is in bath temperature by eluent
60 DEG C, vacuum degree is that 0.09Mpa is concentrated under reduced pressure and obtains Bauhinia blakeana carthamin lotion, then by Bauhinia blakeana carthamin
Lotion dry 8h in 40 DEG C of baking oven, obtains Bauhinia blakeana carthamin product, and pigment quality is 6.96g, pigment yield
It is 6.9%.
Embodiment 9
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：360g Bauhinia blakeanas pollen end is weighed, is extracted 2 times using mechanical agitation：Extraction adds for the first time
Enter 9.0L distilled water, solid-to-liquid ratio 1:25, Extracting temperature is 50 DEG C, and mechanical agitation extracts 2h, mixing speed 20r/s, gauze mistake
Filter, filter residue add 7.2L distilled water, solid-to-liquid ratio 1:20, mechanical agitation extract 1.5h, mixing speed 20r/s, filtered through gauze,
Merge 2 filtrates.
3) pigment separated is enriched with：Filtrate is 60 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extracting solution
0.5 times of mL of volume.It is 40 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, resin
Column volume is 6480cm3(1:16g/cm3), it, will be on above-mentioned concentrate after there is no apparent bubble with distilled water flushing to interlaminar resin
Column, coutroi velocity 0.8mL/s, until after pigment is all adsorbed on resin, first with distillation water elution, flow velocity 1.0mL/s, elution
To efflux be it is colourless until (water consumption be 4.0 times of column volumes), then with volume fraction of ethanol be 60% ethanol-water solution elution
By the pigment of macroporous resin adsorption, flow velocity 1.3mL/s, be eluted to efflux it is colourless until (eluting agent is 1.5 times of cylinders
Product), concentrate the alcohol-water eluent of collection, by eluent bath temperature be 60 DEG C, vacuum degree be 0.09Mpa reduced pressure
Bauhinia blakeana carthamin lotion is obtained, then Bauhinia blakeana carthamin lotion is dried into 6h in 60 DEG C of baking oven, is obtained
To Bauhinia blakeana carthamin product, pigment quality is 23.4g, and pigment yield is 6.5%.
Embodiment 10
A kind of extraction preparation method of Bauhinia blakeana carthamin of the present embodiment, includes the following steps：
1) pretreatment of raw material：It selects without rotten, fresh Bauhinia blakeana flower petal, after washing with water totally, 50
DEG C baking oven in dry 7h, then crushed 80 mesh sieve.
2) pigment extracts：300g Bauhinia blakeanas pollen end is weighed, is extracted 3 times using mechanical agitation：Extraction is added 12L and steams
Distilled water, solid-to-liquid ratio 1:40, Extracting temperature is 55 DEG C, and mechanical agitation extracts 2h, mixing speed 22r/s, and filtered through gauze merges 3
Secondary filtrate.
3) pigment separated is enriched with：Filtrate is 60 DEG C in bath temperature, and vacuum degree is that 0.09Mpa is concentrated under reduced pressure into remaining extracting solution
0.5 times of mL of volume.It is 40 that activated D101 macroporous absorbent resins, which are packed into draw ratio,:1 normal pressure glass chromatography column, resin
Column volume is 6480cm3(1:16g/cm3), it, will be on above-mentioned concentrate after there is no apparent bubble with distilled water flushing to interlaminar resin
Column, coutroi velocity 0.8mL/s, until after pigment is all adsorbed on resin, first with distillation water elution, flow velocity 1.5mL/s, elution
To efflux be it is colourless until (water consumption be 4.0 times of column volumes), then with volume fraction of ethanol be 60% ethanol-water solution elution
By the pigment of macroporous resin adsorption, flow velocity 1.3mL/s, be eluted to efflux it is colourless until (eluting agent is 1.5 times of cylinders
Product), concentrate the alcohol-water eluent of collection, by eluent bath temperature be 70 DEG C, vacuum degree be 0.09Mpa reduced pressure
Bauhinia blakeana carthamin lotion is obtained, then Bauhinia blakeana carthamin lotion is dried into 6h in 60 DEG C of baking oven, is obtained
To Bauhinia blakeana carthamin product, pigment quality is 19.2g, and pigment yield is 6.5%.
Comparative example 1
In this comparative example 1 in pigment extraction process, extractant uses hydrochloric acid-water extractant (pH 3)
In addition to extractant is different, the pretreatment of raw material and the extraction step of pigment are same as Example 3.
Comparative example 2
In this comparative example 2 in pigment extraction process, extractant use pH for 3 sour -ol (75% ethyl alcohol：Hydrochloric acid is molten
Liquid) extractant.
In addition to extractant is different, the pretreatment of raw material and the extraction step of pigment are same as Example 3.
Comparative example 3
In this comparative example 3 in pigment extraction process, extractant use pH for 3 75% ethyl alcohol, by again to pigment
Add the citric acid tune pH of isoconcentration in filtrate after extraction.
In addition to extractant is different, the pretreatment of raw material and the extraction step of pigment are same as Example 3.
Effect experiment
13mim (4000r/ are centrifuged using the filtrate after the pigment separated of embodiment 3 and comparative example 1 to 3
min).Take filtrate 1mL that distilled water is added to be diluted to 5mL after centrifugation, the full wavelength scanner between 400~800nm detects maximum absorption wave
It is long.The results are shown in Table 1 for it：
The maximum absorption wavelength and absorbance of extracting solution obtained by 1 different solvents of table
As shown in Table 1, it extracts Bauhinia blakeana haematochrome with acidic extraction agent and extracts the pigment institute with neutral extractant
The maximum absorption wavelength for obtaining extracting solution is consistent, illustrates that the pigment extracted is identical substance；And neutral extractant extraction gained
Extracting solution absorbance under same concentrations is higher than acidic extraction agent, and aqueous extract higher, therefore steaming also than alcohol extract
Distilled water is the optimum extraction solvent of the pigment.
Bauhinia blakeana carthamin properties of product：The maximum absorption wave of Bauhinia blakeana carthamin prepared by the present invention
It is long：524~530nm (hydrochloric acid-water of pH=3 is solvent), is dark red powder, there is the faint scent of distinctive Bauhinia blakeana flower.
The pigment shows the typical color and luster variation characteristic of anthocyanin, i.e., with the change of pH：Acidity is aubergine, acid stronger, face
Color is deeper；Alkalinity is yellow green.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent substitution, improvement and etc. done should be included within the scope of protection of the invention god.
Claims (10)
1. a kind of extraction preparation method of Bauhinia blakeana carthamin, which is characterized in that include the following steps：
1) it is 1 by solid-to-liquid ratio by Bauhinia blakeana pollen end and distilled water:15~1:20 (g/mL) are mixed, with ultrasonic wave extraction,
Gained extracting solution is filtered, filtrate is obtained；
Or it is 1 that solid-to-liquid ratio is pressed at Bauhinia blakeana pollen end and distilled water:10~1:20 (g/mL) are mixed, with Microwave Extraction,
Gained extracting solution is filtered, filtrate is obtained；
Or solid-to-liquid ratio 1 is pressed at Bauhinia blakeana pollen end and distilled water:20~1:40 (g/mL) are mixed, mechanical agitation extraction,
Gained extracting solution is filtered, filtrate is obtained；
2) above-mentioned pigment filtrate decompression is concentrated, activated D101 macroreticular resins is packed into chromatographic column, it is flat with distilled water flushing
Weighing apparatus resin column is not until interlaminar resin has apparent bubble；Filtrate after concentration is packed into chromatographic column, until pigment is all adsorbed on resin
After upper, eluted, be eluted to efflux it is colourless until, eluent is collected in concentration, and eluent is concentrated under reduced pressure and obtains safflower sheep
Hoof nail carthamin lotion, then Bauhinia blakeana carthamin lotion is dried to obtain Bauhinia blakeana carthamin.
2. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
1) it uses ultrasonic wave at 60~70 DEG C in, extracts 40~50min, and extract 2~3 times.
3. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
1) in microwave power be 400~600W, temperature be 50~70 DEG C under the conditions of, extract 15~25min, and extract 2~4
Extracting solution filtering that is secondary, obtaining, obtains filtrate.
4. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
1) under the conditions of low whipping speed is 20~30r/s in, mechanical agitation extracts 60~120min, extracts 2~3 times, gained is extracted
Liquid filters, and obtains filtrate.
5. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
2) in by above-mentioned pigment filtrate bath temperature be 50~70 DEG C, vacuum degree be 0.09Mpa be concentrated under reduced pressure into remaining extracting liquid volume
0.3~0.7 times, wait for upper prop.
6. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
2) filtrate after concentration is packed into chromatographic column, coutroi velocity is 0.3~0.8mL/s.
7. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
2) after pigment is all adsorbed on resin, first with distillation water elution, flow velocity is 1.0~1.5mL/s, and to be eluted to efflux, which be colourless, is
Only, then with the elution of 60~80% ethanol-water solutions by the pigment of macroporous resin adsorption, flow velocity is 0.8~1.5mL/s, is eluted to
Until efflux is colourless.
8. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the step
2) activation of D101 macroreticular resins impregnates resin 4 hours with 0.01mol/L Hcl solution in, is eluted with water and is washed till during eluate is in
Property；It uses 0.01mol/L NaOH solutions to impregnate resin 2h again, is finally eluted with water to eluate and is in neutrality, for use.
9. the extraction preparation method of Bauhinia blakeana carthamin according to claim 1, which is characterized in that the layer
It analyses column and selects normal pressure glass chromatography column, draw ratio 40:1~46.5:1.
10. the extraction preparation method of Bauhinia blakeana carthamin according to claim 7, which is characterized in that the steaming
3~4 times of column volumes of distilled water dosage；60~80% ethanol-water solution dosages are 1.0~1.5 times of column volumes.
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